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CN102730771B - Production of high purity sodium-free high activity composite nickel carbonate by three-step continuous process - Google Patents

  • ️Wed Nov 27 2013
Production of high purity sodium-free high activity composite nickel carbonate by three-step continuous process Download PDF

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Publication number
CN102730771B
CN102730771B CN2012101605587A CN201210160558A CN102730771B CN 102730771 B CN102730771 B CN 102730771B CN 2012101605587 A CN2012101605587 A CN 2012101605587A CN 201210160558 A CN201210160558 A CN 201210160558A CN 102730771 B CN102730771 B CN 102730771B Authority
CN
China
Prior art keywords
reactor
cobalt
reaction
salt
nickel
Prior art date
2012-05-23
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN2012101605587A
Other languages
Chinese (zh)
Other versions
CN102730771A (en
Inventor
郑景宜
吕文广
吕铂頤
郑玉琦
唱祺
陈译哲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zheng Jingyi
Original Assignee
JILIN CITY FRIEND TECHNOLOGY Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
2012-05-23
Filing date
2012-05-23
Publication date
2013-11-27
2012-05-23 Application filed by JILIN CITY FRIEND TECHNOLOGY Co Ltd filed Critical JILIN CITY FRIEND TECHNOLOGY Co Ltd
2012-05-23 Priority to CN2012101605587A priority Critical patent/CN102730771B/en
2012-10-17 Publication of CN102730771A publication Critical patent/CN102730771A/en
2013-11-27 Application granted granted Critical
2013-11-27 Publication of CN102730771B publication Critical patent/CN102730771B/en
Status Expired - Fee Related legal-status Critical Current
2032-05-23 Anticipated expiration legal-status Critical

Links

  • 229910000008 nickel(II) carbonate Inorganic materials 0.000 title claims abstract description 45
  • ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 title abstract description 24
  • 239000002131 composite material Substances 0.000 title abstract description 4
  • 230000000694 effects Effects 0.000 title abstract description 4
  • 238000004519 manufacturing process Methods 0.000 title abstract description 4
  • 238000010924 continuous production Methods 0.000 title abstract 2
  • DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 24
  • 239000011734 sodium Substances 0.000 claims abstract description 24
  • 229910052708 sodium Inorganic materials 0.000 claims abstract description 24
  • 239000000376 reactant Substances 0.000 claims abstract description 22
  • 238000000034 method Methods 0.000 claims abstract description 21
  • 238000005406 washing Methods 0.000 claims abstract description 16
  • 238000001035 drying Methods 0.000 claims abstract description 12
  • 150000002815 nickel Chemical class 0.000 claims abstract description 10
  • ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 6
  • 239000001099 ammonium carbonate Substances 0.000 claims abstract description 6
  • -1 compound nickelous carbonate Chemical class 0.000 claims description 27
  • 230000009257 reactivity Effects 0.000 claims description 26
  • PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 25
  • 150000003839 salts Chemical class 0.000 claims description 22
  • 238000012545 processing Methods 0.000 claims description 20
  • 229910017052 cobalt Inorganic materials 0.000 claims description 19
  • 239000010941 cobalt Substances 0.000 claims description 19
  • GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 19
  • 238000003860 storage Methods 0.000 claims description 12
  • 229910052759 nickel Inorganic materials 0.000 claims description 11
  • 238000003756 stirring Methods 0.000 claims description 10
  • 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 9
  • 150000001868 cobalt Chemical class 0.000 claims description 9
  • 229910052500 inorganic mineral Inorganic materials 0.000 claims description 9
  • 239000011707 mineral Substances 0.000 claims description 9
  • KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical group [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 8
  • QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims description 5
  • HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 5
  • 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 4
  • QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
  • 150000007530 organic bases Chemical class 0.000 claims description 4
  • SAEBCFDIJRQJQB-UHFFFAOYSA-N carbonic acid;nickel Chemical compound [Ni].OC(O)=O SAEBCFDIJRQJQB-UHFFFAOYSA-N 0.000 claims description 3
  • GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
  • UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
  • 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
  • 239000013078 crystal Substances 0.000 claims description 2
  • 238000006243 chemical reaction Methods 0.000 abstract description 24
  • CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 19
  • 239000001569 carbon dioxide Substances 0.000 abstract description 9
  • 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 9
  • 150000001412 amines Chemical class 0.000 abstract description 2
  • 239000000463 material Substances 0.000 abstract description 2
  • 235000012501 ammonium carbonate Nutrition 0.000 abstract 2
  • QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract 1
  • 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
  • 238000000926 separation method Methods 0.000 abstract 1
  • 239000002994 raw material Substances 0.000 description 5
  • 238000010586 diagram Methods 0.000 description 3
  • BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 3
  • 238000002360 preparation method Methods 0.000 description 3
  • CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
  • BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
  • 239000000243 solution Substances 0.000 description 2
  • 239000000126 substance Substances 0.000 description 2
  • ODIGIKRIUKFKHP-UHFFFAOYSA-N (n-propan-2-yloxycarbonylanilino) acetate Chemical compound CC(C)OC(=O)N(OC(C)=O)C1=CC=CC=C1 ODIGIKRIUKFKHP-UHFFFAOYSA-N 0.000 description 1
  • BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
  • 229910000861 Mg alloy Inorganic materials 0.000 description 1
  • 229910021588 Nickel(II) iodide Inorganic materials 0.000 description 1
  • FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
  • 235000009754 Vitis X bourquina Nutrition 0.000 description 1
  • 235000012333 Vitis X labruscana Nutrition 0.000 description 1
  • 240000006365 Vitis vinifera Species 0.000 description 1
  • 235000014787 Vitis vinifera Nutrition 0.000 description 1
  • MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
  • 239000002253 acid Substances 0.000 description 1
  • 239000013543 active substance Substances 0.000 description 1
  • 239000003513 alkali Substances 0.000 description 1
  • DBAHSLAQEKZNEZ-UHFFFAOYSA-J calcium nickel(2+) dicarbonate Chemical compound C([O-])([O-])=O.[Ca+2].[Ni+2].C([O-])([O-])=O DBAHSLAQEKZNEZ-UHFFFAOYSA-J 0.000 description 1
  • 235000011089 carbon dioxide Nutrition 0.000 description 1
  • 238000006555 catalytic reaction Methods 0.000 description 1
  • 239000011248 coating agent Substances 0.000 description 1
  • 238000000576 coating method Methods 0.000 description 1
  • 229910000001 cobalt(II) carbonate Inorganic materials 0.000 description 1
  • 238000009826 distribution Methods 0.000 description 1
  • 238000009472 formulation Methods 0.000 description 1
  • 230000000977 initiatory effect Effects 0.000 description 1
  • 229910017053 inorganic salt Inorganic materials 0.000 description 1
  • 239000000203 mixture Substances 0.000 description 1
  • 229940078494 nickel acetate Drugs 0.000 description 1
  • 229910000480 nickel oxide Inorganic materials 0.000 description 1
  • IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-UHFFFAOYSA-L 0.000 description 1
  • HKFZDVPCCOOGEV-UHFFFAOYSA-N nickel(3+);borate Chemical compound [Ni+3].[O-]B([O-])[O-] HKFZDVPCCOOGEV-UHFFFAOYSA-N 0.000 description 1
  • BFSQJYRFLQUZKX-UHFFFAOYSA-L nickel(ii) iodide Chemical compound I[Ni]I BFSQJYRFLQUZKX-UHFFFAOYSA-L 0.000 description 1
  • DITXJPASYXFQAS-UHFFFAOYSA-N nickel;sulfamic acid Chemical compound [Ni].NS(O)(=O)=O DITXJPASYXFQAS-UHFFFAOYSA-N 0.000 description 1
  • GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
  • 239000002245 particle Substances 0.000 description 1
  • 229910052697 platinum Inorganic materials 0.000 description 1
  • 102220042174 rs141655687 Human genes 0.000 description 1
  • 102220076495 rs200649587 Human genes 0.000 description 1
  • 102220043159 rs587780996 Human genes 0.000 description 1
  • 239000012266 salt solution Substances 0.000 description 1
  • 229910000029 sodium carbonate Inorganic materials 0.000 description 1
  • 229910001415 sodium ion Inorganic materials 0.000 description 1

Images

Landscapes

  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The present invention discloses a method for producing high purity sodium-free high activity composite nickel carbonate by a three-step continuous process. According to the method, a nickel salt reacts with ammonium carbonate in a reaction kettle 1 at a normal temperature with controlling of pH value of 7-7.5; the resulting reactant overflows to a reaction kettle 2, ammonium carbonate is added, and the reaction is performed in the reaction kettle 2 with controlling of the temperature of 30-40 DEG C and the pH value of 7.5-8.5; the resulting reactant overflows to a reaction kettle 3, an amine base is added to carry out an reaction with controlling of the temperature of 40-50 DEG C and the pH value of 8.5-11.5; and the resulting reactant overflows to a continuous washing machine to carry out washing, and then directly enters an integrated drying and crushing machine to carry out drying and crushing. With the present invention, the prepared nickel carbonate does not contain sodium and sulfate, has the carbon dioxide content more than 20%, and has high activity; and the method is suitable for large-scale production. The present invention further provides special reaction kettles for the method of the present invention, wherein the reaction kettle is provided with a separation plate with an opening, such that the reaction kettle is divided into two reaction chambers of an upper reaction chamber and a lower reaction chamber so as to ensure complete reaction of the overflowed reactant and no material residue.

Description

Three step continuous processings are produced high-purity without the compound nickelous carbonate of sodium high reactivity

Technical field

The invention belongs to chemical field, is exactly that three step continuous processings are produced high-purity method without the compound nickelous carbonate of sodium high reactivity or cobalt.

Background technology

Nickelous carbonate is mainly used in the active substance of (1) catalyzer; (2) presoma of nickel oxide and nickel powder; (3) produce the raw material (nickelous bromide, nickelous iodide etc.) of other inorganic nickel; (4) produce the raw material (nickel sulfamic acid, nickel borate acylate, nickel acetate, grape acid nickel) of organic nickel salt; (5) chemically coating nickel by magnesium-alloy.The quality of nickelous carbonate determines the quality of nickel catalyst.

The nickelous carbonate production method is mainly: nickel salt (nickelous nitrate, single nickel salt, nickelous chloride) solution is that react 9 left and right with carbonate (sodium carbonate, volatile salt, bicarbonate of ammonia etc.) at pH value.The nickelous carbonate prepared like this is actually basic nickel carbonate---the complex body of nickelous carbonate and nickel hydroxide.Preparing pure nickelous carbonate is actually and be difficult to realizes.

The carbon dioxide content of basic nickel carbonate product is the standard that detects nickelous carbonate in basic nickel carbonate, and the content of the high explanation of carbon dioxide content nickelous carbonate is high, and the content of nickel hydroxide is low.The carbon dioxide content of basic nickel carbonate is high, and its micropore is many, in catalyzer, demonstrates high reactivity.

The conventional nickelous carbonate of producing, carbonic acid gas are contained in 10-15% left and right, D 50More than granularity was greater than 10 μ m, micropore seldom.

The ratio that in the basic nickel carbonate of producing, nickelous carbonate accounts for is large, nickel hydroxide accounting example is little, is the target that pursue in the nickel catalyst field always

The inventor utilize microporous ultrafine high activity nickel carbonate the preparation method (Chinese patent: ZL201010201046.1), the basic nickel carbonate of production, D 50Granularity can reach the 1-5 micron, and the size ratio surface-area reaches (every gram square metre) more than 300, and carbon dioxide content is greater than 20%, and micropore is many, and nickel content is the powdery nickelous carbonate of 49-51% and little, and particle size distribution is narrow and even, D10=0.93 μ m; D50=1.81 μ m; D90=2.82 μ m, good dispersity.

Lv Wenguang; Zheng Jingyi; Lu's platinum chin or cheek is shown in that in " high reactivity superfine composite nickelous carbonate signs " periodical " Industrial Catalysis ", " high reactivity superfine composite nickelous carbonate characterizes---double discussion to new formulation national standard " prepared calcium carbonate nickel " " see " Chemical Industry and Engineering Society of China inorganic salt Annual Conference collection of thesis in 2010 ", has introduced carbon dioxide content at compound nickelous carbonate and preparation method thereof more than 20%.Not yet find that there is at present other reports.

Goal of the invention

The purpose of this invention is to provide without sodium ion, the carbon dioxide content preparation method at 20% above nickelous carbonate or cobalt, three step continuous processings are produced high-purity method without the compound nickelous carbonate of sodium high reactivity or cobalt.

Three step continuous processings are produced high-purity method without the compound nickelous carbonate of sodium high reactivity or cobalt, comprise the following steps:

1) nickel or cobalt salt, with volatile salt and/or ammonium bicarbonate soln and flow in reactor 1, stir, and pH value is controlled at 7-7.5, and temperature is normal temperature, and reactant 1 enters

reactor

2 from overflow port;

2)

reactor

2 stream add volatile salt or ammonium bicarbonate soln, stir, and control temperature at 30-40 ℃, pH value 7.5-8.5, and reactant 2 overflows enter

reactor

3;

3)

reactor

3 stream add organic bases solution, described organic bases is ethamine and/or diethylamine, stir, control temperature 40-50 ℃, pH value 8.5-11.5, reactant 3 overflows enter in mineral salt deposit continuous washing machine washs, and after washing, directly enters drying and crushing in the drying and crushing all-in-one, obtains combined type carbonic acid nickel or cobalt;

Described mineral salt deposit continuous washing machine is Chinese patent ZL200920093696.1, and the drying and crushing all-in-one is ZL200920093766.3;

Between described reactor 1,

reactor

2,

reactor

3 and mineral salt deposit continuous washing machine, be provided with storage tank; Reactant is pressed reactor 1, storage tank 1,

reactor

2,

storage tank

2,

reactor

3,

storage tank

3, the overflow of mineral salt deposit continuous washing machine order;

Described nickel salt is nickelous nitrate and/or nickelous chloride; Described cobalt salt is Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and/or cobalt chloride;

Step

1 and 2 described nickel or cobalt salt concentration are 40-100 g/L, and volatile salt and/or bicarbonate of ammonia concentration are 40-200 g/L, are 40-200 g/L;

The described ethamine concentration of

step

2 is 40-100 g/L, and diethylamine concentration is 40-100 g/L.

Another object of the present invention is to provide a kind of three step continuous processings and produces high-purity method special reactor without the compound nickelous carbonate of sodium high reactivity or cobalt.

Three step continuous processings are produced high-purity reactor without the compound nickelous carbonate of sodium high reactivity or cobalt: it is comprised of reactor body, reaction kettle cover and agitator, in described body, also is provided with dividing plate, and dividing plate is provided with opening, and the upper and lower of dividing plate is equipped with paddle; On body, the below of dividing plate also is provided with and flows feed-pipe, and the body top is provided with upflow tube.

Three step continuous processings provided by the invention are produced high-purity method without the compound nickelous carbonate of sodium high reactivity or cobalt, adopt nickel or cobalt salt and amine carbonate at normal temperatures, control pH value 7-7.5, at reactor 1, react, reactant overflows to

reactor

2, add again amine carbonate, control temperature at 30-40 ℃, pH value 7.5-8.5, in

reactor

2 reactions,

reactant overflow reactor

3, add amine alkali to react, control temperature 40-50 ℃, pH value 8.5-11.5, the reactant overflow directly enters drying and crushing in the drying and crushing all-in-one after entering in continuous washing machine and washing; In nickelous carbonate or cobalt, do not contain sodium, sulfate radical, carbon dioxide content is greater than 20%, has high reactivity, is applicable to scale operation.The present invention also provides the special reactor of the inventive method, and it is provided with the dividing plate with opening, and reactor is divided into to upper and lower two reaction chambers, has guaranteed that the reactant reaction overflowed is complete, residual without raw material.

The accompanying drawing explanation

Fig. 1 is that three step continuous processings are produced high-purity method flow diagram without the compound nickelous carbonate of sodium high reactivity or cobalt;

Fig. 2 is that three step continuous processings are produced the reactor schematic diagram without the method for the compound nickelous carbonate of sodium high reactivity or cobalt;

Fig. 3 is the reactor dividing plate schematic diagram of three step continuous processing lifes without the method for the compound nickelous carbonate of sodium high reactivity or cobalt.

Embodiment

The present invention is except following embodiment elaboration, and other is same as the prior art.

Embodiment 1 continuous processing is produced high-purity method without the compound nickelous carbonate of sodium high reactivity or cobalt

Refer to Fig. 1

1), nickel or cobalt salt and volatile salt, and stream adds in reactor 1, stirs, and by adjusting the flow velocity of nickel salt and volatile salt, controls pH value at 7-7.5, temperature is normal temperature, reactant 1 overflows to storage tank 1 from reactor 1 top;

2, reactant 1 in storage tank 1 is pumped into to

reactor

2, also stream adds volatile salt in

reactor

2 simultaneously, stirs, and controls temperature at 30-40 ℃, pH value 7.5-8.5, and reactant 2 overflows to

storage tank

3 from

reactor

2 tops;

3, reactant in

storage tank

2 is pumped into to

reactor

3, also stream adds ethamine and/or diethylamine simultaneously, stir, control temperature 40-50 ℃, pH value 8.5-11.5, reactant 3 enters mineral salt deposit continuous washing machine and washs from

reactor

3 top overflows, after washing, directly enters drying and crushing in the drying and crushing all-in-one, obtains combined type carbonic acid nickel; Described mineral salt deposit continuous washing machine is Chinese patent ZL200920093696.1, and the drying and crushing all-in-one is ZL200920093766.3; Obtain high-purity without the compound nickelous carbonate of sodium high reactivity.

Described nickel salt is nickelous nitrate or nickelous chloride, and the concentration of nickel salt solution is 40-100g/L, and the concentration of volatile salt is 40-200 g/L.

Embodiment

2 continuous processings are produced high-purity method without the compound nickelous carbonate of sodium high reactivity

With bicarbonate of ammonia, replace volatile salt, or the use that is mixed of volatile salt and bicarbonate of ammonia, other is identical with embodiment 1.

Embodiment

3 continuous processings are produced high-purity method without the compound cobaltous carbonate of sodium high reactivity

With cobalt salt, replace nickel salt, the other the same as in Example 1 or 2.

In

embodiment

1,2 and 3 nickelous carbonates of producing or cobalt, do not contain sodium, sulfate radical, carbon dioxide content is greater than 20%, has high reactivity, and present method has been saved human and material resources, has reduced cost, is applicable to scale operation.

Embodiment

4 three step continuous processings are produced high-purity method special reactor without the compound nickelous carbonate of sodium high reactivity

Refer to Fig. 2,3, three step continuous processings are produced high-purity reactor without the compound nickelous carbonate of sodium high reactivity or cobalt, it is comprised of reactor body 1,

reaction kettle cover

2 and

agitator

3, in described body, also be provided with dividing

plate

4, dividing

plate

4 is provided with opening 41, and the

paddle

31 of

agitator

3 and

paddle

32 are located at respectively below and the top of dividing plate; Body 1, the below of dividing plate also be provided with and flow feed-

pipe A

5 and and flow feed-

pipe B

6, body 1 side, top is provided with upflow tube 7.

During use, the

paddle

31 of

agitator

3 is by the

opening

41 of dividing

plate

4, enter dividing

plate

4 belows, and stream feed-pipe A and and flow feed-pipe B and stream adds reaction raw materials, enter the reaction chamber of dividing

plate

4 belows, after

paddle

31 carries out initial action, then pass through the reaction chamber of the

opening

41 of dividing

plate

4 to the dividing plate top, paddle 32 stirs and reacts, that the end reaction thing overflows to next reactor by upflow tube 7 and flow feed-pipe.

Three step continuous processings of the present invention are produced high-purity reactor without the compound nickelous carbonate of sodium high reactivity, are provided with dividing

plate

4, and reactor is divided into to upper and lower two reaction chambers, have guaranteed that the reactant reaction overflowed is complete, residual without raw material.

Claims (4)

1. three step continuous processings are produced high-purity method without the compound nickelous carbonate of sodium high reactivity or cobalt, comprise the following steps:

1) nickel or cobalt salt, with volatile salt and/or ammonium bicarbonate soln and flow in reactor 1, stir, and pH value is controlled at 7-7.5, and temperature is normal temperature, and reactant 1 enters reactor 2 from overflow port;

2) reactor 2 stream add volatile salt and/or ammonium bicarbonate soln, stir, and control temperature at 30-40 ℃, pH value 7.5-8.5, and reactant 2 overflows enter reactor 3;

3) reactor 3 stream add organic bases solution, described organic bases is ethamine and/or diethylamine, stir, control temperature 40-50 ℃, pH value 8.5-11.5, reactant 3 overflows enter in mineral salt deposit continuous washing machine washs, and after washing, directly enters drying and crushing in the drying and crushing all-in-one, obtains combined type carbonic acid nickel or cobalt; Described nickel salt is nickelous nitrate and/or nickelous chloride, and described cobalt salt is Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and/or cobalt chloride.

2. root a tree name three step continuous processings claimed in claim 1 are produced high-purity method without the compound nickelous carbonate of sodium high reactivity, it is characterized in that: between described reactor 1, reactor 2, reactor 3 and mineral salt deposit continuous washing machine, be respectively equipped with storage tank, reactant is pressed reactor 1, storage tank 1, reactor 2, storage tank 2, reactor 3, storage tank 3, the overflow of mineral salt deposit continuous washing machine order.

3. the described three step continuous processings of root a tree name claim 1 or 2 are produced high-purity method without the compound nickelous carbonate of sodium high reactivity or cobalt, it is characterized in that: step 1 and 2 described nickel or cobalt salt concentration are 40-100g/L, and volatile salt and/or bicarbonate of ammonia concentration are 40-200g/L.

4. root a tree name three step continuous processings claimed in claim 3 are produced high-purity method without the compound nickelous carbonate of sodium high reactivity or cobalt, and it is characterized in that: the described ethamine concentration of step 3 and/or diethylamine concentration are 40-100g/L.

CN2012101605587A 2012-05-23 2012-05-23 Production of high purity sodium-free high activity composite nickel carbonate by three-step continuous process Expired - Fee Related CN102730771B (en)

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CN104556248B (en) * 2013-10-12 2017-06-27 中国电子科技集团公司第十八研究所 The method of continuous production large granular spherical cobalt carbonate
CN113044895B (en) * 2019-12-27 2023-09-05 荆门市格林美新材料有限公司 Preparation method of low-impurity high-nickel basic nickel carbonate
CN112939099B (en) * 2021-02-09 2023-05-12 荆门市格林美新材料有限公司 Preparation method of basic nickel carbonate

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Inventor after: Zheng Jingyi

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