CN102382314B - Preparation method and application of modified organic silicon resin - Google Patents
- ️Wed Jan 09 2013
发明内容 Contents of the invention
本发明解决的技术问题是提供一种改性有机硅树脂的制备方法，该方法制备的改性有机硅树脂具有耐热低表面能低和耐酸耐水性能好的优点。The technical problem solved by the present invention is to provide a method for preparing a modified silicone resin. The modified silicone resin prepared by the method has the advantages of low heat resistance, low surface energy and good acid and water resistance.
为解决本发明所述的技术问题，本发明提供的解决方案是：一种改性有机硅树脂的制备方法，该方法由以下步骤组成：In order to solve the technical problems described in the present invention, the solution provided by the present invention is: a preparation method of modified silicone resin, the method is composed of the following steps:
将40～60w％端羧基超支化聚酰胺、1～10w％环氧树脂和30～50w％的有机硅树脂和重量为端氨基超支化聚酰胺用量1～10％的交联催化剂加入反应器中；依次在110～120℃、150～170℃和200～210℃下分别加热1～3小时；最后降至室温，加入有机溶剂调整固含量为60～70％；上述步骤中，Add 40-60w% of carboxyl-terminated hyperbranched polyamide, 1-10w% of epoxy resin, 30-50w% of silicone resin and a cross-linking catalyst whose weight is 1-10% of amino-terminated hyperbranched polyamide into the reactor ; respectively heating at 110-120°C, 150-170°C and 200-210°C for 1-3 hours; finally lowering to room temperature, adding an organic solvent to adjust the solid content to 60-70%; in the above steps,
所述的端羧基超支化聚酰胺的重均分子量为2000～6000，它是将二元胺、三元酸和含氨基烷基羧酸按照物质的量比率为二元胺∶三元酸∶含氨基烷基羧酸＝1∶1～2∶0～0.1进行酰胺化反应得到；其中，所述的二元胺是1，3-丙二胺、1，2-丙二胺、1，4-环己二胺、1，4-丁二胺、异佛尔酮二胺、4，4’-二氨基二苯甲烷、4，4’-二氨基二苯砜和1，6-己二胺其中一种或者两种以上；所述的三元酸是1，2，4-苯三甲酸和1，3，5-苯三甲酸其中一种或者混合物；所述的含氨基烷基羧酸是甘氨酸、3-氨基丙酸和3-氨基-2-甲基丙酸其中一种或者两种以上；The weight-average molecular weight of described carboxyl-terminated hyperbranched polyamide is 2000～6000, and it is that diamine, tribasic acid and amino-containing alkyl carboxylic acid are dibasic amine: tribasic acid: containing Aminoalkylcarboxylic acid=1:1～2:0～0.1 is obtained by amidation reaction; wherein, the diamine is 1,3-propylenediamine, 1,2-propylenediamine, 1,4- Cyclohexanediamine, 1,4-butanediamine, isophoronediamine, 4,4'-diaminodiphenylmethane, 4,4'-diaminodiphenylsulfone and 1,6-hexanediamine One or more than two kinds; the tribasic acid is one or a mixture of 1,2,4-benzenetricarboxylic acid and 1,3,5-benzenetricarboxylic acid; the amino-containing alkyl carboxylic acid is glycine , 3-aminopropionic acid and 3-amino-2-methylpropionic acid, or one or more of them;
所述的环氧树脂是二氧化双环戊二烯、3，4-环氧化环己烷甲酸3’，4’-环氧化环己烷甲酯、双((3，4-环氧环己基)甲基)己二酸酯、双(2，3-环氧环戊基)醚、双酚S环氧树脂和三羟甲基丙烷缩水甘油醚其中一种或者两种以上；Described epoxy resin is dicyclopentadiene dioxide, 3,4-epoxidized cyclohexane carboxylate 3',4'-epoxidized cyclohexane methyl ester, bis((3,4-epoxy ring One or more of hexyl)methyl)adipate, bis(2,3-epoxycyclopentyl)ether, bisphenol S epoxy resin and trimethylolpropane glycidyl ether;
所述的有机硅树脂的重均分子量为800～2000，且含有2.5～15％的甲氧基或乙氧基和3～20％的羟基；The weight average molecular weight of the silicone resin is 800-2000, and contains 2.5-15% methoxyl or ethoxyl and 3-20% hydroxyl;
所述的交联催化剂是钛酸四丁酯、钛酸四异丁酯、二辛氧基锡、二异辛氧基锡、二辛氧基锌和二异辛氧基锌其中一种或者两种以上；The crosslinking catalyst is one or both of tetrabutyl titanate, tetraisobutyl titanate, dioctyltin, diisooctyltin, dioctylzinc and diisooctylzinc more than one species;
所述的有机溶剂为丁醇、异丁醇、丙二醇甲醚、二丙二醇甲醚、二丙二醇丁醚、丙二醇甲醚醋酸酯、二丙二醇甲醚醋酸酯和二丙二醇丁醚醋酸酯其中一种或两种以上。Described organic solvent is one of butanol, isobutanol, propylene glycol methyl ether, dipropylene glycol methyl ether, dipropylene glycol butyl ether, propylene glycol methyl ether acetate, dipropylene glycol methyl ether acetate and dipropylene glycol butyl ether acetate or Two or more.
本发明所述的有机硅树脂可以由一甲基三乙氧基硅烷，二甲基二乙氧基硅烷，一苯基三乙氧基等硅氧烷进行水解缩合反应得到，也可以由一甲基三甲氧基硅烷，二甲基二甲氧基硅烷，一苯基三甲氧基等硅氧烷进行水解缩合反应得到，还可以直接使用下述具体产品中的一种或两种以上的混合物：信越公司的KR211，信越公司的KR212，信越公司的KR214，信越公司的KR216，瓦克公司的IC836，信越公司的KR213，信越公司的KR9218，信越公司的KR217，道康宁公司的233，道康宁公司的249，道康宁公司的Z-6108，道康宁公司的3074，道康宁公司的3037。上述硅氧烷的水解缩合反应是本领域常用的硅氧烷进行水解缩合反应，其工艺和反应条件是本领域技术人员应掌握的常规技术。The organosilicon resin of the present invention can be obtained by hydrolysis and condensation reaction of siloxanes such as monomethyltriethoxysilane, dimethyldiethoxysilane, and monophenyltriethoxy, and can also be obtained by monomethyltriethoxysilane It can be obtained by hydrolysis and condensation reaction of siloxanes such as trimethoxysilane, dimethyldimethoxysilane, and phenyltrimethoxysilane. It is also possible to directly use one or a mixture of two or more of the following specific products: Shin-Etsu KR211, Shin-Etsu KR212, Shin-Etsu KR214, Shin-Etsu KR216, Wacker IC836, Shin-Etsu KR213, Shin-Etsu KR9218, Shin-Etsu KR217, Dow Corning 233, Dow Corning 249 , Dow Corning's Z-6108, Dow Corning's 3074, and Dow Corning's 3037. The above-mentioned hydrolysis and condensation reaction of siloxane is a hydrolysis and condensation reaction of siloxane commonly used in this field, and its process and reaction conditions are conventional techniques that should be mastered by those skilled in the art.
本发明所述的端羧基超支化聚酰胺的重均分子量较佳为3000～4000，它较好是由以下方法制备得到：将三元酸、二元胺和含氨基烷基羧酸按照物质的量比率为二元胺∶三元酸∶含氨基烷基羧酸＝1∶1～1.4∶0.05～0.1加入反应器中；以每小时升温20℃的加热速度，加热至240℃，在0.67～1.33kPa下保温2～4h；冷却到室温；其中，所述的二元胺是1，4-环己二胺、异佛尔酮二胺、4，4’-二氨基二苯甲烷、4，4’-二氨基二苯砜和1，6-己二胺其中一种或者两种以上；所述的三元酸是1，3，5-苯三甲酸和1，2，4-苯三甲酸其中一种或者混合物；所述的含氨基烷基羧酸是3-氨基丙酸和3-氨基-2-甲基丙酸其中一种或者混合物。The carboxyl-terminated hyperbranched polyamide of the present invention preferably has a weight-average molecular weight of 3000 to 4000, and it is preferably prepared by the following method: tribasic acid, diamine and amino-containing alkyl carboxylic acid according to the composition of the substance The volume ratio is diamine: tribasic acid: amino-containing alkyl carboxylic acid = 1: 1 ~ 1.4: 0.05 ~ 0.1. Add in the reactor; heat up to 240 ° C at a heating rate of 20 ° C per hour, at 0.67 ~ Insulate at 1.33kPa for 2 to 4 hours; cool to room temperature; wherein, the diamines are 1,4-cyclohexanediamine, isophoronediamine, 4,4'-diaminodiphenylmethane, 4, One or more of 4'-diaminodiphenylsulfone and 1,6-hexanediamine; the tribasic acid is 1,3,5-benzenetricarboxylic acid and 1,2,4-benzenetricarboxylic acid One or a mixture thereof; the amino-containing alkyl carboxylic acid is one or a mixture of 3-aminopropionic acid and 3-amino-2-methylpropionic acid.
本发明所述的有机硅树脂较好是信越公司的KR211、信越公司的KR212、信越公司的KR214、信越公司的KR216、瓦克公司的IC836、信越公司的KR213、信越公司的KR9218、信越公司的KR217、道康宁公司的233、道康宁公司的249、道康宁公司的Z-6108、道康宁公司的3074和道康宁公司的3037其中一种或者两种以上的混合物。The silicone resin of the present invention is preferably KR211 of Shin-Etsu Corporation, KR212 of Shin-Etsu Corporation, KR214 of Shin-Etsu Corporation, KR216 of Shin-Etsu Corporation, IC836 of Wacker Corporation, KR213 of Shin-Etsu Corporation, KR9218 of Shin-Etsu Corporation, and KR217, Dow Corning 233, Dow Corning 249, Dow Corning Z-6108, Dow Corning 3074 and Dow Corning 3037, or a mixture of two or more.
本发明所述的环氧树脂较佳是二氧化双环戊二烯、3，4-环氧化环己烷甲酸3’，4’-环氧化环己烷甲酯、双((3，4-环氧环己基)甲基)己二酸酯、双(2，3-环氧环戊基)醚、双酚S环氧树脂、三羟甲基丙烷缩水甘油醚其中一种或者两种以上。The epoxy resin described in the present invention is preferably dicyclopentadiene dioxide, 3,4-epoxidized cyclohexanecarboxylic acid 3',4'-epoxidized cyclohexane methyl ester, bis((3,4 -One or more of epoxy cyclohexyl)methyl)adipate, bis(2,3-epoxycyclopentyl)ether, bisphenol S epoxy resin, trimethylol propane glycidyl ether .
本发明所述的交联催化剂较佳是二辛氧基锡、二异辛氧基锡、二辛氧基锌和二异辛氧基锌其中一种或者两种以上。The crosslinking catalyst described in the present invention is preferably one or more of dioctyloxide tin, diisooctyloxide tin, dioctyloxide zinc and diisooctyloxide zinc.
本发明所述的有机溶剂较佳为丙二醇甲醚、二丙二醇甲醚、二丙二醇丁醚、丙二醇甲醚醋酸酯、二丙二醇甲醚醋酸酯和二丙二醇丁醚醋酸酯一种或两种以上。The organic solvent described in the present invention is preferably one or more of propylene glycol methyl ether, dipropylene glycol methyl ether, dipropylene glycol butyl ether, propylene glycol methyl ether acetate, dipropylene glycol methyl ether acetate and dipropylene glycol butyl ether acetate.
本发明所述的改性有机硅树脂的制备方法中，端羧基超支化聚酰胺用量较佳为50～60w％，环氧树脂用量较佳为1～8w％，有机硅树脂用量较佳为35～50w％，交联催化剂用量较佳为端氨基超支化聚酰胺重量1～5％。In the preparation method of the modified silicone resin of the present invention, the amount of carboxyl-terminated hyperbranched polyamide is preferably 50-60w%, the amount of epoxy resin is preferably 1-8w%, and the amount of silicone resin is preferably 35% ~50w%, the dosage of the crosslinking catalyst is preferably 1-5% by weight of the amino-terminated hyperbranched polyamide.
本发明所述的制备方法中发生三种交联反应，第一种是端羧基超支化聚酰胺上的羧基和环氧树脂上的环氧基进行交联反应，第二种是有机硅树脂上的硅醇基和环氧树脂上的环氧基进行缩合反应，第三种是端羧基超支化聚酰胺上的羧基和环氧树脂上的环氧基反应形成的羟基和有机硅树脂上的烷氧基或者硅醇基进行交联反应。如此端羧基超支化聚酰胺、环氧树脂和有机硅树脂进行两两交联反应，形成多重交联互穿孔网络结构，将端羧基超支化聚酰胺、环氧树脂和有机硅树脂的优点结合起来，所获得的改性有机硅树脂具有以下优点：Three kinds of crosslinking reactions take place in the preparation method of the present invention, the first kind is that the carboxyl group on the carboxyl-terminated hyperbranched polyamide and the epoxy group on the epoxy resin carry out crosslinking reaction, and the second kind is the crosslinking reaction on the organosilicon resin. The silanol group on the epoxy resin undergoes a condensation reaction with the epoxy group on the epoxy resin. The third is the hydroxyl group formed by the reaction between the carboxyl group on the carboxyl-terminated hyperbranched polyamide and the epoxy group on the epoxy resin and the alkyl group on the silicone resin. Oxygen or silanol groups undergo crosslinking reactions. In this way, carboxyl-terminated hyperbranched polyamide, epoxy resin and silicone resin are cross-linked in pairs to form a multiple cross-linked interpenetrating network structure, which combines the advantages of carboxyl-terminated hyperbranched polyamide, epoxy resin and silicone resin , the obtained modified silicone resin has the following advantages:
(1)超支化聚合物具有高度支化结构，使得超支化聚合物分子链间缠结较少，赋予本发明制备的超支化聚酰胺改性有机硅树脂具有低粘度和良好的成膜性能的优点。(1) The hyperbranched polymer has a highly branched structure, so that there is less entanglement between the hyperbranched polymer molecular chains, and the hyperbranched polyamide modified silicone resin prepared by the present invention has low viscosity and good film-forming properties. advantage.
(2)聚酰胺具有良好的耐磨性能、耐酸性能和优异的机械性能，赋予本发明所述方法制备的超支化聚酰胺改性有机硅树脂具有良好的机械性能和耐酸性能。(2) polyamide has good wear resistance, acid resistance and excellent mechanical properties, endowing the hyperbranched polyamide modified silicone resin prepared by the method of the present invention with good mechanical properties and acid resistance.
本发明所述的改性有机硅树脂可以应用在制备耐高温低表面能涂料，该涂料具有良好的耐酸性能和耐磨性能。The modified silicone resin of the invention can be used in the preparation of high-temperature-resistant and low-surface-energy coatings, and the coatings have good acid resistance and abrasion resistance.
本发明所述的涂料，该涂料含有60～80w％所述的改性有机硅树脂、10～20w％耐高温颜料填料和5～20w％高沸点溶剂。The coating of the present invention contains 60-80w% of the modified silicone resin, 10-20w% of high temperature resistant pigment filler and 5-20w% of high boiling point solvent.
本发明所述的高沸点溶剂，是指二价酸酯混合物、乙二醇乙醚醋酸酯、二乙二醇丁醚醋酸酯、异丁酸异丁酯、丙酸-3-乙醚乙酯、甲基异戊基酮其中一种或者两种以上。The high boiling point solvent of the present invention refers to dibasic acid ester mixture, ethylene glycol ethyl ether acetate, diethylene glycol butyl ether acetate, isobutyl isobutyrate, 3-ethyl ether ethyl propionate, formaldehyde One or two or more of the base isoamyl ketones.
本发明所述的涂料中，颜料为本领域常用的耐高温颜料，可以是碳黑、铁红等无机耐高温颜料，也可以是酞青蓝等有机耐高温颜料。In the coating of the present invention, the pigment is a high-temperature-resistant pigment commonly used in the field, which can be an inorganic high-temperature-resistant pigment such as carbon black and iron red, or an organic high-temperature-resistant pigment such as phthalocyanine blue.
本发明所述的涂料中，填料为本领域常用的耐高温填料，可以是二氧化钛、二氧化硅和碳化硅。In the coating of the present invention, the filler is a high temperature resistant filler commonly used in the field, which may be titanium dioxide, silicon dioxide and silicon carbide.
本发明所述的涂料还可以含有有机硅助剂。The coating of the present invention may also contain silicone additives.
本发明所述的涂料中，有机硅助剂是本领域常用的有机硅助剂，起到流平、消泡、颜料润湿、粘度调节等作用。本领域的技术人员可以依据要求确定有机硅助剂的种类和用量。本发明所述的有机硅助剂可以有硅油、聚醚改性有机硅助剂等。本发明所述的聚醚改性有机硅助剂是本领域常用的聚醚改性有机硅助剂，可以是迈图高新材料有限公司的CoatOSil系列聚醚改性有机硅助剂。In the coating described in the present invention, the silicone additive is a silicone additive commonly used in the field, which plays the roles of leveling, defoaming, pigment wetting, viscosity adjustment and the like. Those skilled in the art can determine the type and amount of silicone additives according to requirements. The silicone additives described in the present invention may include silicone oil, polyether modified silicone additives and the like. The polyether-modified silicone additives described in the present invention are commonly used polyether-modified silicone additives in the field, and may be CoatOSil series polyether-modified silicone additives from Momentive High-tech Materials Co., Ltd.
本发明所述的涂料中，有机硅助剂的用量为1～5w％。In the paint of the present invention, the amount of the organic silicon additive is 1-5w%.
本发明所述的涂料中，还可以含有流平剂、粘度调节剂和分散剂等其他助剂。In the coating of the present invention, other auxiliary agents such as leveling agent, viscosity modifier and dispersant can also be contained.
本发明所述的涂料的制备方法是本领域常用的制备方法，即将改性有机硅树脂、颜料、填料、有机硅助剂和高沸点溶剂混合得到。The preparation method of the coating in the present invention is a common preparation method in the field, that is, the modified silicone resin, pigments, fillers, silicone additives and high boiling point solvents are mixed.
本发明所述的涂料具有良好的耐热性能、低表面能、良好的耐水耐溶剂性能和良好的金属附着力，可应用金属表面防护，赋予金属耐高温，耐溶剂，易清洁的特点，可以应用于炉具表面、烧烤架、电熨斗、炊具内外壁等五金产品上。The coating of the present invention has good heat resistance, low surface energy, good water and solvent resistance and good metal adhesion, and can be used for metal surface protection, endowing metal with high temperature resistance, solvent resistance, and easy cleaning. Applied to hardware products such as the surface of stoves, grills, electric irons, inner and outer walls of cooking utensils, etc.
本发明相对现有技术，具有以下优点：本发明所述的涂料以改性有机硅树脂作为基础树脂，该树脂制备过程中端羧基超支化聚酰胺、环氧树脂和有机硅树脂进行两两交联反应，形成多重交联改性树脂，将端羧基超支化聚酰胺的附着力好，颜料亲和性高的优点、环氧树脂的机械性能好，耐水和溶剂性能好的优点和有机硅树脂的低表面能，耐热性优异，耐水性能好的优点结合起来，因此本发明所述的涂料具有高耐热性能、良好的金属附着力、低表面能、优异的耐水煮和耐酸性能的优点。Compared with the prior art, the present invention has the following advantages: the coating of the present invention uses modified silicone resin as the base resin, and in the preparation process of the resin, carboxyl-terminated hyperbranched polyamide, epoxy resin and silicone resin are exchanged in pairs. Linkage reaction to form multiple cross-linked modified resins, the carboxyl-terminated hyperbranched polyamide has the advantages of good adhesion, high pigment affinity, good mechanical properties of epoxy resin, good water and solvent resistance and silicone resin Low surface energy, excellent heat resistance, and good water resistance are combined, so the coating of the present invention has the advantages of high heat resistance, good metal adhesion, low surface energy, excellent boiling resistance and acid resistance .
具体实施方式 Detailed ways
以下是本发明所述技术方案的非限制性实施例。The following are non-limiting examples of the technical solution of the present invention.
实施例1：Example 1:
1)端羧基超支化聚酰胺1) Carboxyl-terminated hyperbranched polyamide
a)组成：a) Composition:
三元酸：1，3，5-苯三甲酸105g(0.5mol)；1，2，4-苯三甲酸105g(0.5mol)；Tribasic acid: 1,3,5-benzenetricarboxylic acid 105g (0.5mol); 1,2,4-benzenetricarboxylic acid 105g (0.5mol);
二元胺：1，4-环己二胺57.1g(0.5mol)；二胺基二苯砜99.4g(0.4mol)；1，6-己二胺11.6g(0.1mol)Diamine: 57.1g (0.5mol) of 1,4-cyclohexanediamine; 99.4g (0.4mol) of diaminodiphenylsulfone; 11.6g (0.1mol) of 1,6-hexanediamine
b)合成步骤：b) synthesis steps:
将三元酸和二元胺加入装有加热，冷凝和氮气保护的反应器中，氮气保护下升温到110℃，保温2h；以每小时20℃加热速度加热至240℃，在1.33kPa下保温4h；最后冷却室温，得到344g端羧基超支化聚酰胺。Add tribasic acid and diamine into a reactor equipped with heating, condensation and nitrogen protection, raise the temperature to 110°C under nitrogen protection, and keep it for 2 hours; heat it to 240°C at a heating rate of 20°C per hour, and keep it at 1.33kPa 4h; finally cooled to room temperature to obtain 344g carboxyl-terminated hyperbranched polyamide.
c)端羧基超支化聚酰胺的性能c) Properties of carboxyl-terminated hyperbranched polyamides
端羧基超支化聚酰胺的重均分子量采用凝胶渗透色谱法检测，结果为6002。The weight-average molecular weight of the carboxyl-terminated hyperbranched polyamide was detected by gel permeation chromatography, and the result was 6002.
2)改性有机硅树脂2) Modified silicone resin
a)组成：a) Composition:
端羧基超支化聚酰胺：步骤1制备的端羧基超支化聚酰胺60g；Carboxyl-terminated hyperbranched polyamide: 60 g of carboxyl-terminated hyperbranched polyamide prepared in step 1;
环氧树脂：二氧化双环戊二烯10g；Epoxy resin: dicyclopentadiene dioxide 10g;
有机硅树脂：信越有机硅树脂KR216 30g；Silicone resin: Shin-Etsu silicone resin KR216 30g;
二辛氧基锡：1g。Dioctyltin: 1 g.
b)制备工艺：b) Preparation process:
将步骤1制备的端羧基超支化聚酰胺，环氧树脂和有机硅树脂加入装有加热、冷凝和氮气保护装置的反应器中，加入催化剂，升温到120℃保温2小时，升温到160℃保温2小时，最后冷却到室温，加入丙二醇甲醚醋酸酯调整固含量为70％，得到改性有机硅树脂132g。Add the carboxyl-terminated hyperbranched polyamide prepared in step 1, epoxy resin and silicone resin into a reactor equipped with heating, condensation and nitrogen protection devices, add a catalyst, heat up to 120°C for 2 hours, and heat up to 160°C for heat preservation After 2 hours, it was finally cooled to room temperature, and propylene glycol methyl ether acetate was added to adjust the solid content to 70% to obtain 132 g of modified silicone resin.
c)改性有机硅树脂性能c) Properties of modified silicone resin
改性有机硅树脂的综合性能Comprehensive performance of modified silicone resin
耐热性能：将试片于180℃烘烤2h后，放入电位差计核对的恒温箱式电炉中，按5℃/min升高温度，随炉温到实验要求温度开始计时，试样经过持续高温后，取出，冷至室温(25℃)，用放大镜观察涂层表面状况，如无龟裂、脱落现象，即说明涂层耐热性能良好。Heat resistance performance: After the test piece is baked at 180°C for 2 hours, put it into a thermostatic box-type electric furnace checked by a potentiometer, increase the temperature at 5°C/min, and start timing as the furnace temperature reaches the temperature required by the experiment. After the high temperature continues, take it out, cool to room temperature (25°C), observe the surface condition of the coating with a magnifying glass, if there is no cracking or peeling off, it means that the coating has good heat resistance.
3)涂料3) paint
a)组成a) Composition
改性有机硅树脂：步骤2制备的改性有机硅树脂100g；Modified silicone resin: 100 g of modified silicone resin prepared in step 2;
颜料填料：碳黑40g；二氧化钛20g；Pigment filler: carbon black 40g; titanium dioxide 20g;
有机硅助剂：硅油/350cst 8g；Silicone additives: silicone oil /350cst 8g;
高沸点溶剂：二价酸酯混合物(DBE)5g。High boiling point solvent: 5 g of dibasic ester mixture (DBE).
b)制备工艺b) Preparation process
将颜料填料、改性有机硅树脂、有机硅助剂、高沸点溶剂混合均匀，加入研磨机中研磨到所需要粒径，既得。Mix the pigment filler, modified silicone resin, silicone additives, and high-boiling point solvent evenly, add it to a grinder, and grind it to the required particle size.
c)性能c) Performance
涂料的性能指标The performance index of coating
1*耐水煮性能：将试片于180℃烘烤2h后，冷却到室温，然后将试片放置于100℃的蒸馏水中，加热至漆膜破坏，出现如起泡，失光，变色，龟裂等现象。1*Boiling resistance: Bake the test piece at 180°C for 2 hours, cool to room temperature, then place the test piece in distilled water at 100°C, and heat until the paint film is destroyed, such as blistering, loss of gloss, discoloration, turtle cracking etc.
2*耐热性能：将试片于180℃烘烤2h后，放入电位差计核对的恒温箱式电炉中，按5℃/min升高温度，随炉温到实验要求温度开始计时，试样经过持续高温后，取出，冷至室温(25℃)，用放大镜观察涂层表面状况，如无龟裂、脱落现象，即说明涂层耐热性能良好。2*Heat resistance performance: After baking the test piece at 180°C for 2 hours, put it into a thermostatic box-type electric furnace checked by a potentiometer, increase the temperature at 5°C/min, and start timing as the furnace temperature reaches the temperature required by the experiment. After the sample has been subjected to continuous high temperature, take it out, cool it to room temperature (25°C), and observe the surface condition of the coating with a magnifying glass. If there is no crack or peeling off, it means that the coating has good heat resistance.
3*表面张力：在25℃下，由表面张力测量仪测定。3* Surface tension: Measured by a surface tension meter at 25°C.
实施例2：Example 2:
1)端羧基超支化聚酰胺1) Carboxyl-terminated hyperbranched polyamide
a)组成：a) Composition:
三元酸：1，3，5-苯三甲酸294g(1.4mol)；1，2，4-苯三甲酸126g(0.6mol)；Tribasic acid: 294g (1.4mol) of 1,3,5-benzenetricarboxylic acid; 126g (0.6mol) of 1,2,4-benzenetricarboxylic acid;
二元胺：1，2-丙二胺29.7g(0.4mol)；异佛尔酮二胺68g(0.4mol)；4，4’-二氨基二苯甲烷39.6g(0.2mol)；Diamine: 29.7g (0.4mol) of 1,2-propylenediamine; 68g (0.4mol) of isophoronediamine; 39.6g (0.2mol) of 4,4'-diaminodiphenylmethane;
b)合成步骤：b) synthesis steps:
将三元酸和二元胺加入装有加热，冷凝和氮气保护的反应器中，氮气保护下升温到110℃，保温2h；以每小时20℃加热速度加热至240℃，在0.66kPa下保温2h；最后冷却室温，得到522g端羧基超支化聚酰胺。Add tribasic acid and diamine into a reactor equipped with heating, condensation and nitrogen protection, raise the temperature to 110°C under nitrogen protection, and keep it for 2 hours; heat it to 240°C at a heating rate of 20°C per hour, and keep it at 0.66kPa 2h; finally cooled to room temperature to obtain 522g carboxyl-terminated hyperbranched polyamide.
c)端羧基超支化聚酰胺的性能c) Properties of carboxyl-terminated hyperbranched polyamides
端羧基超支化聚酰胺的重均分子量采用凝胶渗透色谱法检测，结果为1997。The weight-average molecular weight of carboxyl-terminated hyperbranched polyamide was detected by gel permeation chromatography, and the result was 1997.
2)改性有机硅树脂2) Modified silicone resin
a)组成：a) Composition:
端羧基超支化聚酰胺：步骤1制备的端羧基超支化聚酰胺40g；Carboxyl-terminated hyperbranched polyamide: 40 g of carboxyl-terminated hyperbranched polyamide prepared in step 1;
环氧树脂：三羟甲基丙烷缩水甘油醚8g；Epoxy resin: trimethylolpropane glycidyl ether 8g;
有机硅树脂：道康宁3037 52g；Silicone resin: Dow Corning 3037 52g;
催化剂：二辛氧基锡3g。Catalyst: 3 g of dioctyl tin oxide.
b)制备工艺：b) Preparation process:
将步骤1制备的饱和端羧基超支化聚酰胺、环氧树脂和有机硅树脂加入装有加热、冷凝和氮气保护装置的反应器中，加入催化剂，升温到110℃保温3小时，升温到170℃保温1小时，最后冷却到室温，加入丙二醇甲醚醋酸酯调整固含量为60％，得到改性有机硅树脂160g。Add the saturated carboxyl-terminated hyperbranched polyamide, epoxy resin and silicone resin prepared in step 1 into a reactor equipped with heating, condensation and nitrogen protection devices, add a catalyst, raise the temperature to 110°C and keep it for 3 hours, then raise the temperature to 170°C Keep it warm for 1 hour, and finally cool to room temperature, add propylene glycol methyl ether acetate to adjust the solid content to 60%, and obtain 160 g of modified silicone resin.
c)改性有机硅树脂性能c) Properties of modified silicone resin
改性有机硅树脂的综合性能Comprehensive performance of modified silicone resin
3)涂料3) paint
a)组成a) Composition
改性有机硅树脂：步骤2制备的改性有机硅树脂160g；Modified silicone resin: 160g of modified silicone resin prepared in step 2;
颜料填料：碳黑20g；Pigment filler: carbon black 20g;
高沸点溶剂：二价酸酯混合物(DBE)5g；乙二醇乙醚醋酸酯(CAC)：5g。High boiling point solvent: divalent ester mixture (DBE) 5g; ethylene glycol diethyl ether acetate (CAC): 5g.
b)制备工艺b) Preparation process
将颜料填料、改性有机硅树脂、高沸点溶剂混合均匀，加入研磨机中研磨到所需要粒径，既得。Mix the pigment filler, modified silicone resin, and high-boiling point solvent evenly, add it into a grinder, and grind it to the required particle size.
c)性能c) Performance
涂料的性能指标The performance index of coating
实施例3：Example 3:
1)端羧基超支化聚酰胺1) Carboxyl-terminated hyperbranched polyamide
a)组成：a) Composition:
三元酸：1，2，4-苯三甲酸294g(1.4mol)；Tribasic acid: 294g (1.4mol) of 1,2,4-benzenetricarboxylic acid;
二元胺：1，4-丁二胺17.63g(0.2mol)；1，6-己二胺58.1g(0.5mol)；4，4’-二氨基二苯砜74.4g(0.3mol)Diamine: 17.63g (0.2mol) of 1,4-butanediamine; 58.1g (0.5mol) of 1,6-hexanediamine; 74.4g (0.3mol) of 4,4'-diaminodiphenylsulfone
含氨基烷基羧酸：甘氨酸3.75g(0.05mol)；3-氨基丙酸4.45g(0.05mol)Amino-containing alkyl carboxylic acid: glycine 3.75g (0.05mol); 3-aminopropionic acid 4.45g (0.05mol)
b)合成步骤：b) synthesis steps:
将三元酸、二元胺和含氨基烷基羧酸加入装有加热，冷凝和氮气保护的反应器中，氮气保护下升温到110℃，保温2h；以每小时20℃加热速度加热至240℃，在0.78kPa下保温2.5h；最后冷却室温，得到485g端羧基超支化聚酰胺。Add tribasic acid, diamine and amino-containing alkyl carboxylic acid into a reactor equipped with heating, condensation and nitrogen protection, raise the temperature to 110°C under nitrogen protection, and keep it for 2 hours; heat to 240°C at a heating rate of 20°C per hour °C, heat preservation at 0.78kPa for 2.5h; finally cool down to room temperature to obtain 485g carboxyl-terminated hyperbranched polyamide.
c)端羧基超支化聚酰胺的性能c) Properties of carboxyl-terminated hyperbranched polyamides
端羧基超支化聚酰胺的重均分子量采用凝胶渗透色谱法检测，结果为3004。The weight-average molecular weight of the carboxyl-terminated hyperbranched polyamide was detected by gel permeation chromatography, and the result was 3004.
2)有机硅树脂中间体2) Silicone resin intermediate
a)组成a) Composition
一甲基三甲氧基硅烷：42.0g(0.28mol)Monomethyltrimethoxysilane: 42.0g (0.28mol)
二甲基二甲氧基硅烷：18.7g(0.14mol)Dimethyldimethoxysilane: 18.7g (0.14mol)
一苯基三甲氧基硅烷：123.0g(0.58mol)，One-phenyltrimethoxysilane: 123.0g (0.58mol),
b)制备工艺b) Preparation process
在装有冷凝管、温度计、滴液漏斗和搅拌器的反应器中按配比依次加入硅氧烷和4.5mmol盐酸后，开始搅拌并升温，升温到60℃后保持温度恒定，在搅拌下滴加31.7g蒸馏水，滴加完毕后，再恒温反应3h后，开始减压蒸馏，压力控制在0.06MPa，蒸去反应过程中产生的小分子，冷却到室温，调整固含量为60％，得到有机硅树脂中间体290g。After adding siloxane and 4.5mmol hydrochloric acid sequentially according to the ratio in the reactor equipped with a condenser tube, a thermometer, a dropping funnel and a stirrer, start stirring and raise the temperature. 31.7g of distilled water, after the dropwise addition, after constant temperature reaction for 3 hours, start vacuum distillation, control the pressure at 0.06MPa, evaporate small molecules generated during the reaction, cool to room temperature, adjust the solid content to 60%, and obtain organic silicon Resin intermediate 290g.
c)性能c) Performance
有机硅树脂中间体的重均分子量采用凝胶渗透色谱法检测，结果为802；有机硅树脂中间体的羟基含量采用乙酸酐法测定，结果为10.6％；有机硅树脂中间体的甲氧基含量采用高氯酸乙酰法测定，结果为7.4％；R/Si＝1.14；ph/Me＝1.04。The weight-average molecular weight of the silicone resin intermediate was detected by gel permeation chromatography, and the result was 802; the hydroxyl content of the silicone resin intermediate was measured by the acetic anhydride method, and the result was 10.6%; the methoxyl content of the silicone resin intermediate Measured by perchloric acid acetyl method, the result is 7.4%; R/Si=1.14; ph/Me=1.04.
3)改性有机硅树脂3) Modified silicone resin
a)组成a) Composition
端羧基超支化聚酰胺：步骤1制备的端羧基超支化聚酰胺50g；Carboxyl-terminated hyperbranched polyamide: 50 g of carboxyl-terminated hyperbranched polyamide prepared in step 1;
环氧树脂：双((3，4-环氧环己基)甲基)己二酸酯4g；双酚S环氧树脂2g；Epoxy resin: bis((3,4-epoxycyclohexyl) methyl) adipate 4g; Bisphenol S epoxy resin 2g;
有机硅树脂：步骤2制备的固含量60％的有机硅树脂73.3g；Silicone resin: 73.3 g of the silicone resin with a solid content of 60% prepared in step 2;
催化剂：二异辛氧基锡2.7g。Catalyst: 2.7 g of tin diisooctoxide.
b)制备工艺b) Preparation process
将步骤1制备的端羧基超支化聚酰胺，环氧树脂和有机硅树脂加入装有加热、冷凝和氮气保护装置的反应器中，加入催化剂，升温到115℃保温1.5小时，升温到175℃保温1.5小时，最后冷却到室温，加入二丙二醇甲醚醋酸酯和二丙二醇丁醚醋酸酯调整固含量为65％，得到改性有机硅树脂141g。Add the carboxyl-terminated hyperbranched polyamide prepared in step 1, epoxy resin and silicone resin into a reactor equipped with heating, condensation and nitrogen protection devices, add a catalyst, heat up to 115°C for 1.5 hours, and heat up to 175°C for heat preservation After 1.5 hours, it was finally cooled to room temperature, dipropylene glycol methyl ether acetate and dipropylene glycol butyl ether acetate were added to adjust the solid content to 65%, and 141 g of modified silicone resin was obtained.
c)改性有机硅树脂性能c) Properties of modified silicone resin
改性有机硅树脂的综合性能Comprehensive performance of modified silicone resin
4)涂料4) paint
a)组成a) Composition
改性有机硅树脂：步骤3制备的改性有机硅树脂100g；Modified silicone resin: 100 g of modified silicone resin prepared in step 3;
颜料填料：酞青蓝20g；二氧化硅20g；Pigment filler: phthalocyanine blue 20g; silicon dioxide 20g;
有机硅助剂：CoatOSil 7001 4g；硅油
高沸点溶剂：二乙二醇丁醚醋酸酯(DBA)5g；乙二醇乙醚醋酸酯(CAC)5g。High boiling point solvent: diethylene glycol butyl ether acetate (DBA) 5g; ethylene glycol ethyl ether acetate (CAC) 5g.
b)制备工艺b) Preparation process
将颜料填料、改性有机硅树脂、有机硅助剂、高沸点溶剂混合均匀，加入研磨机中研磨到所需要粒径，既得。Mix the pigment filler, modified silicone resin, silicone additives, and high-boiling point solvent evenly, add it to a grinder, and grind it to the required particle size.
c)涂性能c) Coating performance
涂料的性能指标The performance index of coating
实施例4：Example 4:
1)端羧基超支化聚酰胺1) Carboxyl-terminated hyperbranched polyamide
a)组成：a) Composition:
多元醇：1，3，5-苯三甲酸378g(1.8mol)；Polyol: 378g (1.8mol) of 1,3,5-benzenetricarboxylic acid;
二元胺：异佛尔酮二胺34g(0.2mol)；1，6-己二胺58.1g(0.5mol)；4，4’-二氨基二苯砜74.4g(0.3mol)Diamine: 34g (0.2mol) of isophoronediamine; 58.1g (0.5mol) of 1,6-hexanediamine; 74.4g (0.3mol) of 4,4'-diaminodiphenylsulfone
含氨基烷基羧酸：甘氨酸0.75g(0.01mol)；3-氨基丙酸1.78g(0.02mol)；3-氨基-2-甲基丙酸3.63g(0.03mol)；Amino-containing alkyl carboxylic acid: 0.75g (0.01mol) of glycine; 1.78g (0.02mol) of 3-aminopropionic acid; 3.63g (0.03mol) of 3-amino-2-methylpropionic acid;
b)合成步骤：b) synthesis steps:
将三元酸、二元胺和含氨基烷基羧酸加入装有加热，冷凝和氮气保护的反应器中，氮气保护下升温到110℃，保温2h；以每小时20℃加热速度加热至240℃，在0.85kPa下保温3.5h；最后冷却室温，得到390g端羧基超支化聚酰胺。Add tribasic acid, diamine and amino-containing alkyl carboxylic acid into a reactor equipped with heating, condensation and nitrogen protection, raise the temperature to 110°C under nitrogen protection, and keep it for 2 hours; heat to 240°C at a heating rate of 20°C per hour °C, keep warm at 0.85kPa for 3.5h; finally cool down to room temperature to obtain 390g carboxyl-terminated hyperbranched polyamide.
c)端羧基超支化聚酰胺的性能c) Properties of carboxyl-terminated hyperbranched polyamides
端羧基超支化聚酰胺的重均分子量采用凝胶渗透色谱法检测，结果为2245。The weight-average molecular weight of the carboxyl-terminated hyperbranched polyamide was detected by gel permeation chromatography, and the result was 2245.
2)改性有机硅树脂2) Modified silicone resin
a)组成a) Composition
端羧基超支化聚酰胺：步骤1制备的端羧基超支化聚酰胺58g；Carboxyl-terminated hyperbranched polyamide: 58g of carboxyl-terminated hyperbranched polyamide prepared in step 1;
环氧树脂：双(2，3-环氧环戊基)醚4g；3，4-环氧化环己烷甲酸3’，4’-环氧化环己烷甲酯3g；Epoxy resin: bis(2,3-epoxycyclopentyl) ether 4g; 3,4-epoxidized cyclohexanecarboxylic acid 3', 4'-epoxidized cyclohexane methyl ester 3g;
有机硅树脂：信越有机硅树脂KR211 15g；信越有机硅树脂KR214 20g；Silicone resin: Shin-Etsu silicone resin KR211 15g; Shin-Etsu silicone resin KR214 20g;
催化剂：二异辛氧基锌2g；二辛氧基锡1.5g。Catalyst: 2 g of zinc diisooctoxide; 1.5 g of tin dioctoxide.
b)制备工艺：b) Preparation process:
将步骤1制备的端羧基超支化聚酰胺，环氧树脂和有机硅树脂加入装有加热、冷凝和氮气保护装置的反应器中，加入催化剂，升温到120℃保温2小时，升温到155℃保温2.5小时，最后冷却到室温，加入丙二醇甲醚醋酸酯和丁醇调整固含量为70％，得到改性有机硅树脂125g。Add the carboxyl-terminated hyperbranched polyamide prepared in step 1, epoxy resin and silicone resin into a reactor equipped with heating, condensation and nitrogen protection devices, add a catalyst, heat up to 120°C for 2 hours, and heat up to 155°C for heat preservation After 2.5 hours, it was finally cooled to room temperature, and propylene glycol methyl ether acetate and butanol were added to adjust the solid content to 70% to obtain 125 g of modified silicone resin.
c)改性有机硅树脂性能c) Properties of modified silicone resin
改性有机硅树脂的综合性能Comprehensive performance of modified silicone resin
3)涂料3) paint
a)组成a) Composition
改性有机硅树脂：步骤2制备的改性有机硅树脂120g；Modified silicone resin: 120g of modified silicone resin prepared in step 2;
颜料填料：碳化硅10g；二氧化硅10g；Pigment filler: silicon carbide 10g; silicon dioxide 10g;
有机硅助剂：CoatOSil 3500 4g；硅油
高沸点溶剂：丙酸-3-乙醚乙酯(EEP)10g；二价酸酯混合物(DBE)10g。High boiling point solvent: 3-ethyl ether propionate (EEP) 10g; divalent ester mixture (DBE) 10g.
b)制备工艺b) Preparation process
将颜料填料、改性有机硅树脂、有机硅助剂、高沸点溶剂混合均匀，加入研磨机中研磨到所需要粒径，既得。Mix the pigment filler, modified silicone resin, silicone additives, and high-boiling point solvent evenly, add it to a grinder, and grind it to the required particle size.
c)性能c) Performance
涂料的性能指标The performance index of coating
实施例5Example 5
1)端羧基超支化聚酰胺1) Carboxyl-terminated hyperbranched polyamide
a)组成：a) Composition:
三元酸：1，2，4-苯三甲酸252g(1.2mol)；Tribasic acid: 252g (1.2mol) of 1,2,4-benzenetricarboxylic acid;
二元胺：1，4-环己二胺34.2g(0.3mol)；1，6-己二胺29g(0.25mol)；4，4’-二氨基二苯砜111.6g(0.45mol)；Diamines: 1,4-cyclohexanediamine 34.2g (0.3mol); 1,6-hexanediamine 29g (0.25mol); 4,4'-diaminodiphenylsulfone 111.6g (0.45mol);
含氨基烷基羧酸：3-氨基2-甲基丙酸6.06g(0.05mol)；Amino-containing alkyl carboxylic acid: 6.06g (0.05mol) of 3-amino 2-methylpropionic acid;
b)合成步骤：b) synthesis steps:
将三元酸、二元胺和含氨基烷基羧酸加入装有加热，冷凝和氮气保护的反应器中，氮气保护下升温到110℃，保温2h；以每小时20℃加热速度加热至240℃，在0.66kPa下保温2.5h；最后冷却室温，得到400g端羧基超支化聚酰胺。Add tribasic acid, diamine and amino-containing alkyl carboxylic acid into a reactor equipped with heating, condensation and nitrogen protection, raise the temperature to 110°C under nitrogen protection, and keep it for 2 hours; heat to 240°C at a heating rate of 20°C per hour °C, keep warm at 0.66kPa for 2.5h; finally cool down to room temperature to obtain 400g carboxyl-terminated hyperbranched polyamide.
c)端羧基超支化聚酰胺的性能c) Properties of carboxyl-terminated hyperbranched polyamides
端羧基超支化聚酰胺的重均分子量采用凝胶渗透色谱法检测，结果为4002。The weight-average molecular weight of the carboxyl-terminated hyperbranched polyamide was detected by gel permeation chromatography, and the result was 4002.
2)改性有机硅树脂2) Modified silicone resin
a)组成：a) Composition:
端羧基超支化聚酰胺：步骤1制备的端羧基超支化聚酰胺45g；Carboxyl-terminated hyperbranched polyamide: 45g of carboxyl-terminated hyperbranched polyamide prepared in step 1;
环氧树脂：双((3，4-环氧环己基)甲基)己二酸酯4g；3，4-环氧化环己烷甲酸3’，4’-环氧化环己烷甲酯4g；二氧化双环戊二烯2g；Epoxy resin: bis((3,4-epoxycyclohexyl)methyl)adipate 4g; 3',4'-epoxycyclohexanemethyl 3,4-epoxycyclohexanecarboxylate 4g; dicyclopentadiene dioxide 2g;
有机硅树脂：道康宁公司的有机硅树脂233 35g；道康宁公司的有机硅树脂249 10g；Silicone resin: Dow Corning's silicone resin 233 35g; Dow Corning's silicone resin 249 10g;
催化剂：二辛氧基锡3.5g。Catalyst: 3.5 g of dioctyl tin oxide.
b)制备工艺：b) Preparation process:
将步骤1制备的端羧基超支化聚酰胺，环氧树脂和有机硅树脂加入装有加热、冷凝和氮气保护装置的反应器中，加入催化剂，升温到130℃保温1小时，升温到170℃保温1小时，最后冷却到室温，加入异丁醇和丙二醇甲醚调整固含量为65％，得到改性有机硅树脂141g。Add the carboxyl-terminated hyperbranched polyamide prepared in step 1, epoxy resin and silicone resin into a reactor equipped with heating, condensation and nitrogen protection devices, add a catalyst, heat up to 130°C for 1 hour, and heat up to 170°C for heat preservation After cooling to room temperature for 1 hour, isobutanol and propylene glycol methyl ether were added to adjust the solid content to 65%, to obtain 141 g of modified silicone resin.
c)改性有机硅树脂性能c) Properties of modified silicone resin
改性有机硅树脂的综合性能Comprehensive performance of modified silicone resin
3)涂料3) paint
a)组成a) Composition
改性有机硅树脂：步骤2制备的改性有机硅树脂140g；Modified silicone resin: 140g of modified silicone resin prepared in step 2;
颜料填料：碳黑20g；二氧化硅14g；Pigment filler: carbon black 20g; silicon dioxide 14g;
有机硅助剂：CoatOSil 3500 4g；CoatOSil 7650 2g；Silicone additives: CoatOSil 3500 4g; CoatOSil 7650 2g;
高沸点溶剂：甲基异戊基酮(MIAK)2g；异丁酸异丁酯4g。High boiling point solvent: 2 g of methyl isoamyl ketone (MIAK); 4 g of isobutyl isobutyrate.
b)制备工艺b) Preparation process
将颜料填料、改性有机硅树脂、有机硅助剂、高沸点溶剂混合均匀，加入研磨机中研磨到所需要粒径，既得。Mix the pigment filler, modified silicone resin, silicone additives, and high-boiling point solvent evenly, add it to a grinder, and grind it to the required particle size.
c)性能c) Performance
涂料的性能指标The performance index of coating
实施例6Example 6
1)端羧基超支化聚酰胺1) Carboxyl-terminated hyperbranched polyamide
a)组成：a) Composition:
三元酸：1，3，5-苯三甲酸315g(1.5mol)；Tribasic acid: 315g (1.5mol) of 1,3,5-benzenetricarboxylic acid;
二元胺：对苯二胺13g(0.12mol)；异佛尔酮二胺68g(0.4mol)；4，4’-二氨基二苯甲烷75.4g(0.38mol)；1，6-己二胺11.6g(0.1mol)；Diamine: 13g (0.12mol) of p-phenylenediamine; 68g (0.4mol) of isophoronediamine; 75.4g (0.38mol) of 4,4'-diaminodiphenylmethane; 1,6-hexamethylenediamine 11.6g (0.1mol);
含氨基烷基羧酸：3-氨基-2-甲基丙酸1.21g(0.01mol)；3-氨基丙酸0.89g(0.01mol)。Amino-containing alkyl carboxylic acid: 1.21 g (0.01 mol) of 3-amino-2-methylpropionic acid; 0.89 g (0.01 mol) of 3-aminopropionic acid.
b)合成步骤：b) synthesis steps:
将三元酸、二元胺和含氨基烷基羧酸加入装有加热，冷凝和氮气保护的反应器中，氮气保护下升温到110℃，保温2h；以每小时20℃加热速度加热至240℃，在1.33kPa下保温4h；最后冷却室温，得到448g端羧基超支化聚酰胺。Add tribasic acid, diamine and amino-containing alkyl carboxylic acid into a reactor equipped with heating, condensation and nitrogen protection, raise the temperature to 110°C under nitrogen protection, and keep it for 2 hours; heat to 240°C at a heating rate of 20°C per hour °C, heat preservation at 1.33kPa for 4h; finally cool down to room temperature to obtain 448g carboxyl-terminated hyperbranched polyamide.
c)端羧基超支化聚酰胺的性能c) Properties of carboxyl-terminated hyperbranched polyamides
端羧基超支化聚酰胺的重均分子量采用凝胶渗透色谱法检测，结果为3667。The weight-average molecular weight of the carboxyl-terminated hyperbranched polyamide was detected by gel permeation chromatography, and the result was 3667.
2)改性有机硅树脂2) Modified silicone resin
a)组成a) Composition
端羧基超支化聚酰胺：步骤1制备的端羧基超支化聚酰胺49g；Carboxyl-terminated hyperbranched polyamide: 49g of carboxyl-terminated hyperbranched polyamide prepared in step 1;
环氧树脂：二氧化双环戊二烯1g；Epoxy resin: dicyclopentadiene dioxide 1g;
有机硅树脂：道康宁有机硅树脂3074 35g；信越有机硅树脂KR212 15g；Silicone resin: Dow Corning silicone resin 3074 35g; Shin-Etsu silicone resin KR212 15g;
催化剂：二辛氧基锡1g；钛酸四丁酯1g。Catalyst: 1 g of dioctyl tin oxide; 1 g of tetrabutyl titanate.
b)制备工艺b) Preparation process
将步骤1制备的端羧基超支化聚酰胺，环氧树脂和有机硅树脂加入装有加热、冷凝和氮气保护装置的反应器中，加入催化剂，升温到125℃保温2小时，升温到155℃保温2.5小时，最后冷却到室温，加入丙二醇甲醚醋酸酯和二丙二醇甲醚调整固含量为60％，得到改性有机硅树脂144g。Add the carboxyl-terminated hyperbranched polyamide prepared in step 1, epoxy resin and silicone resin into a reactor equipped with heating, condensation and nitrogen protection devices, add a catalyst, heat up to 125°C for 2 hours, and heat up to 155°C for heat preservation After 2.5 hours, it was finally cooled to room temperature, and propylene glycol methyl ether acetate and dipropylene glycol methyl ether were added to adjust the solid content to 60% to obtain 144 g of modified silicone resin.
c)改性有机硅树脂性能c) Properties of modified silicone resin
改性有机硅树脂的综合性能Comprehensive performance of modified silicone resin
3)涂料3) paint
a)组成a) Composition
改性有机硅树脂：步骤2制备的改性有机硅树脂120g；Modified silicone resin: 120g of modified silicone resin prepared in step 2;
颜料填料：碳黑20g；二氧化硅5g；二氧化钛5g；Pigment filler: carbon black 20g; silicon dioxide 5g; titanium dioxide 5g;
有机硅助剂：CoatOSil 3500 4g；CoatOSil 7510 2g；硅油
高沸点溶剂：二价酸酯混合物(DBE)12g。High boiling point solvent: 12 g of dibasic ester mixture (DBE).
b)制备工艺b) Preparation process
将颜料填料、改性有机硅树脂、有机硅助剂、高沸点溶剂混合均匀，加入研磨机中研磨到所需要粒径，既得。Mix the pigment filler, modified silicone resin, silicone additives, and high-boiling point solvent evenly, add it to a grinder, and grind it to the required particle size.
c)性能c) Performance
涂料的性能指标The performance index of coating
实施例7Example 7
1)端羧基超支化聚酰胺1) Carboxyl-terminated hyperbranched polyamide
a)组成a) Composition
三元酸：1，3，5-苯三甲酸210g(1.0mol)；Tribasic acid: 210g (1.0mol) of 1,3,5-benzenetricarboxylic acid;
二元胺：4，4’-二氨基二苯砜91.9g(0.37mol)；1，4-环己二胺57.3g(0.50mol)Diamine: 4,4'-diaminodiphenylsulfone 91.9g (0.37mol); 1,4-cyclohexanediamine 57.3g (0.50mol)
含氨基烷基羧酸：3-氨基2-甲基丙酸1.21g(0.01mol)；Amino-containing alkyl carboxylic acid: 1.21g (0.01mol) of 3-amino 2-methylpropionic acid;
b)合成步骤：b) synthesis steps:
将三元酸、二元胺和含氨基烷基羧酸加入装有加热，冷凝和氮气保护的反应器中，氮气保护下升温到110℃，保温2h；以每小时20℃加热速度加热至240℃，在1.03kPa下保温3.5h；最后冷却室温，得到354g端羧基超支化聚酰胺。Add tribasic acid, diamine and amino-containing alkyl carboxylic acid into a reactor equipped with heating, condensation and nitrogen protection, raise the temperature to 110°C under nitrogen protection, and keep it for 2 hours; heat to 240°C at a heating rate of 20°C per hour ℃, and kept at 1.03kPa for 3.5h; finally cooled to room temperature to obtain 354g carboxyl-terminated hyperbranched polyamide.
c)端羧基超支化聚酰胺的性能c) Properties of carboxyl-terminated hyperbranched polyamides
端羧基超支化聚酰胺的重均分子量采用凝胶渗透色谱法检测，结果为5782。The weight-average molecular weight of the carboxyl-terminated hyperbranched polyamide was detected by gel permeation chromatography, and the result was 5782.
2)改性有机硅树脂2) Modified silicone resin
a)组成a) Composition
端羧基超支化聚酰胺：步骤1制备的端羧基超支化聚酰胺48g；Carboxyl-terminated hyperbranched polyamide: 48g of carboxyl-terminated hyperbranched polyamide prepared in step 1;
环氧树脂：三羟甲基丙烷缩水甘油醚2g；3，4-环氧化环己烷甲酸3’，4’-环氧化环己烷甲酯1g；双酚S环氧树脂1g；Epoxy resin: trimethylolpropane glycidyl ether 2g; 3,4-epoxidized cyclohexanecarboxylic acid 3',4'-epoxidized cyclohexane methyl ester 1g; bisphenol S epoxy resin 1g;
有机硅树脂：瓦克公司的有机硅树脂IC836 20g；道康宁公司的有机硅树脂Z-6108 10g；信越公司的有机硅树脂KR213 18g；Silicone resin: Wacker's silicone resin IC836 20g; Dow Corning's silicone resin Z-6108 10g; Shin-Etsu's silicone resin KR213 18g;
催化剂：钛酸四异丁酯0.3g；二辛氧基锡0.2g。Catalyst: 0.3 g of tetraisobutyl titanate; 0.2 g of dioctyl tin oxide.
b)制备工艺b) Preparation process
将步骤1制备的端羧基超支化聚酰胺，环氧树脂和有机硅树脂加入装有加热、冷凝和氮气保护装置的反应器中，加入催化剂，升温到130℃保温1小时，升温到150℃保温3小时，最后冷却到室温，加入丙二醇甲醚醋酸酯和二丙二醇丁醚调整固含量为70％，得到改性有机硅树脂126g。Add the carboxyl-terminated hyperbranched polyamide prepared in step 1, epoxy resin and silicone resin into a reactor equipped with heating, condensation and nitrogen protection devices, add a catalyst, raise the temperature to 130°C and keep it for 1 hour, then raise the temperature to 150°C and keep it warm After 3 hours, it was finally cooled to room temperature, and propylene glycol methyl ether acetate and dipropylene glycol butyl ether were added to adjust the solid content to 70% to obtain 126 g of modified silicone resin.
c)改性有机硅树脂性能c) Properties of modified silicone resin
改性有机硅树脂的综合性能Comprehensive performance of modified silicone resin
3)涂料3) paint
a)组成a) Composition
改性有机硅树脂：步骤2制备的改性有机硅树脂 110g；Modified silicone resin: 110g of modified silicone resin prepared in step 2;
颜料填料：酞青蓝20g；二氧化硅5g；二氧化钛5g；Pigment filler: phthalocyanine blue 20g; silicon dioxide 5g; titanium dioxide 5g;
高沸点溶剂：二价酸酯混合物(DBE)40g；异丁酸异丁酯20g。High boiling point solvent: 40 g of dibasic ester mixture (DBE); 20 g of isobutyl isobutyrate.
b)制备工艺b) Preparation process
将颜料填料、改性有机硅树脂、有机硅助剂、高沸点溶剂混合均匀，加入研磨机中研磨到所需要粒径，既得。Mix the pigment filler, modified silicone resin, silicone additives, and high-boiling point solvent evenly, add it to a grinder, and grind it to the required particle size.
c)性能c) Performance
涂料的性能指标The performance index of coating
实施例8Example 8
1)端羧基超支化聚酰胺1) Carboxyl-terminated hyperbranched polyamide
a)组成：a) Composition:
三元酸：1，2，4-苯三甲酸42g(0.2mol)；1，3，5-苯三甲酸210g(1.0mol)Tribasic acid: 42g (0.2mol) of 1,2,4-benzenetricarboxylic acid; 210g (1.0mol) of 1,3,5-benzenetricarboxylic acid
二元胺：4，4’-二氨基二苯砜149g(0.6mol)；1，3-丙二胺29.5g(0.4mol)Diamine: 149g (0.6mol) of 4,4'-diaminodiphenylsulfone; 29.5g (0.4mol) of 1,3-propanediamine
含氨基烷基羧酸：3-氨基丙酸8.9g(0.1mol)。Amino-containing alkyl carboxylic acid: 8.9 g (0.1 mol) of 3-aminopropionic acid.
b)合成步骤：b) synthesis steps:
将三元酸、二元胺和含氨基烷基羧酸加入装有加热，冷凝和氮气保护的反应器中，氮气保护下升温到110℃，保温2h；以每小时20℃加热速度加热至240℃，在1.33kPa下保温4h；最后冷却室温，得到404g端羧基超支化聚酰胺。Add tribasic acid, diamine and amino-containing alkyl carboxylic acid into a reactor equipped with heating, condensation and nitrogen protection, raise the temperature to 110°C under nitrogen protection, and keep it for 2 hours; heat to 240°C at a heating rate of 20°C per hour °C, keep warm at 1.33kPa for 4h; finally cool down to room temperature to obtain 404g carboxyl-terminated hyperbranched polyamide.
c)端羧基超支化聚酰胺的性能c) Properties of carboxyl-terminated hyperbranched polyamides
端羧基超支化聚酰胺的重均分子量采用凝胶渗透色谱法检测，结果为3833。The weight-average molecular weight of the carboxyl-terminated hyperbranched polyamide was detected by gel permeation chromatography, and the result was 3833.
2)有机硅树脂2) Silicone resin
a)组成a) Composition
一甲基三乙氧基硅烷：69.1g(0.36mol)Monomethyltriethoxysilane: 69.1g (0.36mol)
二甲基二乙氧基硅烷：34.0g(0.21mol)Dimethyldiethoxysilane: 34.0g (0.21mol)
一苯基三乙氧基硅烷：109.24g(0.43mol)，One-phenyltriethoxysilane: 109.24g (0.43mol),
b)制备工艺b) Preparation process
在装有冷凝管、温度计、滴液漏斗和搅拌器的反应器中按配比依次加入硅氧烷和5.5mmol盐酸后，开始搅拌并升温，升温到70℃后保持温度恒定，在搅拌下滴加42.7g蒸馏水，滴加完毕后，再恒温反应3h后，开始减压蒸馏，压力控制在0.06MPa，蒸去反应过程中产生的小分子，冷却到室温，调整固含量为60％，得到有机硅树脂中间体322g。After adding siloxane and 5.5mmol hydrochloric acid sequentially according to the ratio in the reactor equipped with a condenser tube, a thermometer, a dropping funnel and a stirrer, start stirring and raise the temperature, keep the temperature constant after raising the temperature to 70°C, and drop 42.7g of distilled water, after the dropwise addition, after constant temperature reaction for 3 hours, start vacuum distillation, control the pressure at 0.06MPa, evaporate small molecules generated during the reaction, cool to room temperature, adjust the solid content to 60%, and obtain organic silicon Resin intermediate 322g.
c)性能c) Performance
有机硅树脂中间体的重均分子量采用凝胶渗透色谱法检测，结果为1808；有机硅树脂中间体的羟基含量采用乙酸酐法测定，结果为20％；有机硅树脂中间体的乙氧基含量采用高氯酸乙酰法测定，结果为2.5％；R/Si＝1.21；ph/Me＝0.55。The weight-average molecular weight of the silicone resin intermediate was detected by gel permeation chromatography, and the result was 1808; the hydroxyl content of the silicone resin intermediate was measured by the acetic anhydride method, and the result was 20%; the ethoxy content of the silicone resin intermediate Measured by perchloric acid acetyl method, the result is 2.5%; R/Si=1.21; ph/Me=0.55.
3)改性有机硅树脂3) Modified silicone resin
a)组成a) Composition
端羧基超支化聚酰胺：步骤1制备的端羧基超支化聚酰胺56g；Carboxyl-terminated hyperbranched polyamide: 56g of carboxyl-terminated hyperbranched polyamide prepared in step 1;
环氧树脂：二氧化双环戊二烯9g；Epoxy resin: dicyclopentadiene dioxide 9g;
有机硅树脂：步骤2合成的有机硅树脂35gSilicone resin: 35g of silicone resin synthesized in step 2
催化剂：二辛氧基锌2.5g；二辛氧基锡2g。Catalyst: 2.5 g of dioctyl oxide zinc; 2 g of dioctyl oxide tin.
b)制备工艺b) Preparation process
将步骤1制备的端羧基超支化聚酰胺，环氧树脂和有机硅树脂加入装有加热、冷凝和氮气保护装置的反应器中，加入催化剂，升温到110℃保温3小时，升温到150℃保温3小时，最后冷却到室温，加入丙二醇甲醚醋酸酯调整固含量为65％，得到改性有机硅树脂138g。Add the carboxyl-terminated hyperbranched polyamide prepared in step 1, epoxy resin and silicone resin into a reactor equipped with heating, condensation and nitrogen protection devices, add a catalyst, heat up to 110°C for 3 hours, and heat up to 150°C for heat preservation After 3 hours, it was finally cooled to room temperature, and propylene glycol methyl ether acetate was added to adjust the solid content to 65%, to obtain 138 g of modified silicone resin.
c)改性有机硅树脂性能c) Properties of modified silicone resin
改性有机硅树脂的综合性能Comprehensive performance of modified silicone resin
4)涂料4) paint
a)组成a) Composition
改性有机硅树脂：步骤2制备的改性有机硅树脂150g；Modified silicone resin: 150 g of modified silicone resin prepared in step 2;
颜料填料：碳黑10g；二氧化硅5g；二氧化钛5g；Pigment filler: carbon black 10g; silicon dioxide 5g; titanium dioxide 5g;
有机硅助剂：CoatOSil 3500 5g；硅油
高沸点溶剂：二价酸酯混合物(DBE)10g。High boiling point solvent: 10 g of dibasic ester mixture (DBE).
b)制备工艺b) Preparation process
将颜料填料、改性有机硅树脂、有机硅助剂、高沸点溶剂混合均匀，加入研磨机中研磨到所需要粒径，既得。Mix the pigment filler, modified silicone resin, silicone additives, and high-boiling point solvent evenly, add it to a grinder, and grind it to the required particle size.
c)性能c) Performance
涂料的性能指标The performance index of coating
实施例9Example 9
1)端羧基超支化聚酰胺成1) Synthesis of carboxyl-terminated hyperbranched polyamide
a)组成a) Composition
三元酸：1，2，4-苯三甲酸294g(1.4mol)；Tribasic acid: 294g (1.4mol) of 1,2,4-benzenetricarboxylic acid;
二元胺：4，4’-二氨基二苯砜124g(0.5mol)；1，4-环己二胺57g(0.5mol)Diamine: 124g (0.5mol) of 4,4'-diaminodiphenylsulfone; 57g (0.5mol) of 1,4-cyclohexanediamine
b)合成步骤b) Synthetic steps
将三元酸和二元胺加入装有加热，冷凝和氮气保护的反应器中，氮气保护下升温到110℃，保温2h；以每小时20℃加热速度加热至240℃，在1.33kPa下保温4h；最后冷却室温，得到439g端羧基超支化聚酰胺。Add tribasic acid and diamine into a reactor equipped with heating, condensation and nitrogen protection, raise the temperature to 110°C under nitrogen protection, and keep it for 2 hours; heat it to 240°C at a heating rate of 20°C per hour, and keep it at 1.33kPa 4h; finally cooled to room temperature to obtain 439g carboxyl-terminated hyperbranched polyamide.
c)端羧基超支化聚酰胺的性能c) Properties of carboxyl-terminated hyperbranched polyamides
端羧基超支化聚酰胺的重均分子量采用凝胶渗透色谱法检测，结果为3253。The weight-average molecular weight of the carboxyl-terminated hyperbranched polyamide was detected by gel permeation chromatography, and the result was 3253.
2)有机硅树脂2) Silicone resin
a)组成a) Composition
一甲基三乙氧基硅烷：44.5g(0.25mol)Monomethyltriethoxysilane: 44.5g (0.25mol)
二甲基二乙氧基硅烷：50.3g(0.34mol)Dimethyldiethoxysilane: 50.3g (0.34mol)
一苯基三乙氧基硅烷：98.4g(0.41mol)，One-phenyltriethoxysilane: 98.4g (0.41mol),
b)制备工艺b) Preparation process
在装有冷凝管、温度计、滴液漏斗和搅拌器的反应器中按配比依次加入硅氧烷和7.0mmol盐酸后，开始搅拌并升温，升温到70℃后保持温度恒定，在搅拌下滴加43.1g蒸馏水，滴加完毕后，再恒温反应3h后，开始减压蒸馏，压力控制在0.06MPa，蒸去反应过程中产生的小分子，冷却到室温，调整固含量为80％，得到有机硅树脂中间体230g。After adding siloxane and 7.0mmol hydrochloric acid sequentially according to the ratio in the reactor equipped with a condenser tube, a thermometer, a dropping funnel and a stirrer, start stirring and raise the temperature, keep the temperature constant after raising the temperature to 70°C, and drop 43.1g of distilled water, after the dropwise addition, after constant temperature reaction for 3 hours, start vacuum distillation, control the pressure at 0.06MPa, evaporate small molecules generated during the reaction, cool to room temperature, adjust the solid content to 80%, and obtain organic silicon Resin intermediate 230g.
c)性能c) Performance
有机硅树脂中间体的重均分子量采用凝胶渗透色谱法检测，结果为1986；有机硅树脂中间体的羟基含量采用乙酸酐法测定，结果为15％；有机硅树脂中间体的乙氧基含量采用高氯酸乙酰法测定，结果为3％；R/Si＝1.34；ph/Me＝0.44。The weight-average molecular weight of the silicone resin intermediate was detected by gel permeation chromatography, and the result was 1986; the hydroxyl content of the silicone resin intermediate was measured by the acetic anhydride method, and the result was 15%; the ethoxy content of the silicone resin intermediate Measured by perchloric acid acetyl method, the result is 3%; R/Si=1.34; ph/Me=0.44.
3)改性有机硅树脂3) Modified silicone resin
a)组成a) Composition
端羧基超支化聚酰胺：步骤1制备的端羧基超支化聚酰胺32g；Carboxyl-terminated hyperbranched polyamide: 32 g of carboxyl-terminated hyperbranched polyamide prepared in step 1;
环氧树脂：二氧化双环戊二烯8g；Epoxy resin: dicyclopentadiene dioxide 8g;
有机硅树脂：步骤2合成的60％固含量有机硅树脂100g；Silicone resin: 100g of 60% solid content silicone resin synthesized in step 2;
催化剂：二辛氧基锡1g、二异辛氧基锡0.6g。Catalyst: 1 g of dioctyl tin oxide, 0.6 g of diisooctyl tin oxide.
b)制备工艺b) Preparation process
将步骤1制备的端羧基超支化聚酰胺，环氧树脂和有机硅树脂加入装有加热、冷凝和氮气保护装置的反应器中，加入催化剂，升温到125℃保温2小时，升温到160℃保温2小时，最后冷却到室温，加入丙二醇甲醚醋酸酯调整固含量为60％，得到改性有机硅树脂148g。Add the carboxyl-terminated hyperbranched polyamide prepared in step 1, epoxy resin and silicone resin into a reactor equipped with heating, condensation and nitrogen protection devices, add a catalyst, raise the temperature to 125°C and keep it for 2 hours, then raise the temperature to 160°C and keep it After 2 hours, it was finally cooled to room temperature, propylene glycol methyl ether acetate was added to adjust the solid content to 60%, and 148 g of modified silicone resin was obtained.
c)改性有机硅树脂性能c) Properties of modified silicone resin
改性有机硅树脂的综合性能Comprehensive performance of modified silicone resin
4)涂料4) paint
a)组成a) Composition
改性有机硅树脂：步骤2制备的改性有机硅树脂150g；Modified silicone resin: 150 g of modified silicone resin prepared in step 2;
颜料填料：酞青蓝20g；二氧化钛20g；Pigment filler: phthalocyanine blue 20g; titanium dioxide 20g;
有机助剂：CoatOSil 7510 8g；Organic additives: CoatOSil 7510 8g;
高沸达溶剂：二价酸酯混合物(DBE)2g。High boiling solvent: 2 g of dibasic acid ester mixture (DBE).
b)制备工艺b) Preparation process
将颜料填料、改性有机硅树脂、有机硅助剂、高沸点溶剂混合均匀，加入研磨机中研磨到所需要粒径，既得。Mix the pigment filler, modified silicone resin, silicone additives, and high-boiling point solvent evenly, add it to a grinder, and grind it to the required particle size.
c)性能c) Performance
涂料的性能指标The performance index of coating
实施例10Example 10
1)端羧基超支化聚酰胺1) Carboxyl-terminated hyperbranched polyamide
a)组成：a) Composition:
三元酸：1，2，4-苯三甲酸231g(1.1mol)；Tribasic acid: 231g (1.1mol) of 1,2,4-benzenetricarboxylic acid;
二元胺：4，4’-二氨基二苯砜149g(0.5mol)；异佛尔酮二胺85g(0.5mol)Diamine: 149g (0.5mol) of 4,4'-diaminodiphenylsulfone; 85g (0.5mol) of isophorone diamine
b)合成步骤：b) synthesis steps:
将三元酸和二元胺加入装有加热，冷凝和氮气保护的反应器中，氮气保护下升温到110℃，保温2h；以每小时20℃加热速度加热至240℃，在0.66kPa下保温2h；最后冷却室温，得到428g端羧基超支化聚酰胺。Add tribasic acid and diamine into a reactor equipped with heating, condensation and nitrogen protection, raise the temperature to 110°C under nitrogen protection, and keep it for 2 hours; heat it to 240°C at a heating rate of 20°C per hour, and keep it at 0.66kPa 2h; finally cooled to room temperature to obtain 428g carboxyl-terminated hyperbranched polyamide.
c)端羧基超支化聚酰胺的性能c) Properties of carboxyl-terminated hyperbranched polyamides
端羧基超支化聚酰胺的重均分子量采用凝胶渗透色谱法检测，结果为3907。The weight-average molecular weight of the carboxyl-terminated hyperbranched polyamide was detected by gel permeation chromatography, and the result was 3907.
2)改性有机硅树脂2) Modified silicone resin
a)组成：a) Composition:
端羧基超支化聚酰胺：步骤1制备的端羧基超支化聚酰胺51g；Carboxyl-terminated hyperbranched polyamide: 51 g of carboxyl-terminated hyperbranched polyamide prepared in step 1;
环氧树脂：三羟甲基丙烷缩水甘油醚1g；双(2，3-环氧环戊基)醚3g；Epoxy resin: trimethylolpropane glycidyl ether 1g; bis(2,3-epoxycyclopentyl) ether 3g;
有机硅树脂：信越有机硅树脂KR9218 25g；道康宁有机硅树脂Z-6108 20g；Silicone resin: Shin-Etsu silicone resin KR9218 25g; Dow Corning silicone resin Z-6108 20g;
催化剂：二辛氧基锌0.6g；二异辛氧基锌0.41g。Catalyst: 0.6 g of dioctyloxyzinc; 0.41 g of diisooctyloxyzinc.
b)制备工艺：b) Preparation process:
将步骤1制备的端羧基超支化聚酰胺，环氧树脂和有机硅树脂加入装有加热、冷凝和氮气保护装置的反应器中，加入催化剂，升温到120℃保温2小时，升温到175℃保温2小时，最后冷却到室温，加入丙二醇甲醚醋酸酯调整固含量为65％，得到改性有机硅树脂136g。Add the carboxyl-terminated hyperbranched polyamide prepared in step 1, epoxy resin and silicone resin into a reactor equipped with heating, condensation and nitrogen protection devices, add a catalyst, raise the temperature to 120°C and keep it for 2 hours, then raise the temperature to 175°C and keep it After 2 hours, it was finally cooled to room temperature, propylene glycol methyl ether acetate was added to adjust the solid content to 65%, and 136 g of modified silicone resin was obtained.
c)改性有机硅树脂性能c) Properties of modified silicone resin
改性有机硅树脂的综合性能Comprehensive performance of modified silicone resin
3)涂料3) paint
a)组成a) Composition
改性有机硅树脂：步骤2制备的改性有机硅树脂120g；Modified silicone resin: 120g of modified silicone resin prepared in step 2;
颜料填料：铁红30g；二氧化钛20g；二氧化硅10g；Pigment filler: iron red 30g; titanium dioxide 20g; silicon dioxide 10g;
有机硅助剂：CoatOSil 7510：2g；Silicone additives: CoatOSil 7510: 2g;
高沸点溶剂：二价酸酯混合物(DBE)：18g。High boiling point solvent: dibasic acid ester mixture (DBE): 18 g.
b)制备工艺b) Preparation process
将颜料填料、改性有机硅树脂、有机硅助剂、高沸点溶剂混合均匀，加入研磨机中研磨到所需要粒径，既得。Mix the pigment filler, modified silicone resin, silicone additives, and high-boiling point solvent evenly, add it to a grinder, and grind it to the required particle size.
c)性能c) Performance
涂料的性能指标Performance indicators of coatings
