CN102002000B - Method for producing 5,5-dimethyl hydantoin - Google Patents

The invention discloses a method for producing 5,5-dimethyl hydantoin which is prepared from the following substances in parts by weight according to the steps as follows: adding water to ammonium bicarbonate and acetone cyanohydrin, stirring until the ammonium bicarbonate and the acetone cyanohydrin are fully dissolved, and sealing up while heating up to 10 DEG C; introducing ammonia to the mixture, heating slowly to 50-65 DEG C, stirring, heating up to 75-85 DEG C after keeping temperature constant for 1-2 hours, introducing air for 30-50 minutes, and filtering after cooling to a room temperature, thus obtaining crude dimethyl hydantoin and a mother liquid; and putting the crude dimethyl hydantoin into the mixture of water and the mother liquid while stirring, adding active carbon after heating up to 80-98 DEG C, decolouring, removing the active carbon by filtration, recooling, crystallizing, filtering centrifugally, and drying, thus obtaining the finished product of dimethyl hydantoin. The method has the advantages of simple technological reaction, low reaction temperature, short reaction time, less side reaction and high yield reaching 85%, and is easy to control; the raw material of ammonium bicarbonate applicable to the method belongs to chemical fertilizers, and is easy to obtain; and the filtrate produced by the technology can be used repeatedly, and no three wastes are discharged.

5, the working method of 5-DMH

Technical field

The present invention relates to a kind of 5, the working method of 5-DMH.

Background technology

5, the 5-DMH has another name called 5,5-T10 (to call DMH in the following text).

DMH is a kind of important organic synthesis intermediate of having many uses, and is the heterogeneous ring compound with certain rigid backbone.Can prepare a series of valuable verivates through substitution reaction.As: C5H6Br2N2O2, two chlordantoins etc. is widely used in production fields such as organic synthesis, medicine, plastics, food, makeup, agricultural chemicals.

DMH abroad twentieth century seventies suitability for industrialized production just, the production equipment of producing thousands of tons of per year is all had in the U.S., Britain and Switzerland.Also there is production in Japan, but scale has only 600 tons of annual outputs.

China just begins to carry out the research of this respect the beginning of the nineties, and has realized suitability for industrialized production, is mainly used in the production of DMH verivate sterilizing agent.Research unit is by Hubei University, Institutes Of Technology Of Taiyuan, Shenyang Chemical Engineering Inst etc.There is Quzhou County, Hebei province synthetic glass factory (produce 100 tons of devices per year, built up in 1989) in factory, Hengshui Prefecture, Hebei province chemical industry pilot plant (producing 2000 tons of devices, nineteen ninety-fives per year builds up).In recent years, flourish along with the fine chemistry industry industry, acetone cyanohydrin output increase progressively the increase in demand with DMH, built up a collection of production DMH factory at home, its synthesis technique generally adopts the cyclisation method, mainly contains interrupter method and continuous processing two lines.As in the patent No. being 200610038040.0 open source literature, a kind of preparation 5 is also disclosed, the working method of 5-DMH but yield be low, be not easy to control.

Summary of the invention

The present invention is intended to overcome the deficiency of prior art, developed a kind of 5, the working method of 5-DMH.

Of the present invention 5, the working method of 5-DMH is made through following steps by following material by weight:

A, 500～700 parts in 600～800 parts in bicarbonate of ammonia, acetone cyanohydrin is added water stir fully dissolving, airtight when being heated to 10 ℃;

B, in the material that makes through a step, feed 30～50 parts of ammonias again, slowly heat to 50～65 ℃, constant temperature 1～2 hour, and stir;

C, will be heated to 75～85 ℃ through the material of b step system, air inducing 30～50 minutes is cooled to the room temperature after-filtration again, promptly makes DMH bullion and mother liquor;

D, will be in 950～1150 parts of DMH bullions that the c step makes be rendered to 150～300 parts the mother liquor mixture of water and 700～900 parts; Stir while throwing in; Add 3～8 parts of activated carbon after being heated to 80～98 ℃, decoloured 20～40 minutes, remove by filter activated carbon; Crystallisation by cooling, centrifuging, oven dry more promptly makes the DMH finished product.

The market of DMH can be considered from purposes two aspects of water quality stabilizer and DMH verivate.China is the very not abundant country of a water resources, and in process water, the consumption of water coolant ranks first.Generally account for more than 60%.Therefore, recycling of water coolant is one of important channel of water saving.At this moment need add various medicaments such as inhibiter in the recirculated water.DMH can directly be used for the anti-stick mud agent of cooling water system.In addition, the multiple verivate of DMH can be done the sterilant of recirculated cooling water.

See from the purposes aspect of DMH verivate, be mainly used in the engineering of water treatment sterilization, algae removal, deodorization and swimming sterilizing sterilization etc.Increasing rapidly at halogen glycolylurea series product consumption aspect U.S.'s swimming sterilizing sterilization.In addition, according to the demand of water treatment and entertainment industry, U.S. Zuo Long company produces in several kinds of reagent combinations of killing AIDS, also contains the halogenated hydantoin verivate.

Of the present invention 5, the working method technological reaction of 5-DMH is simple, temperature of reaction is low, the time is short, be easy to control, and side reaction is few, and yield can reach 85%; The raw material bicarbonate of ammonia that this method was suitable for belongs to fertilizer type, raw material is easy to get; The filtrating that is produced in this technology can recycle, and does not have the discharging of " three wastes ".

Embodiment

Embodiment 1

Of the present invention 5, the working method of 5-DMH is by following material, makes through following steps by weight:

A, 500～700 parts in 600～800 parts in bicarbonate of ammonia, acetone cyanohydrin is added water stir fully dissolving, airtight when being heated to 10 ℃;

B, in the material that makes through a step, feed 30～50 parts of ammonias again, slowly heat to 50～65 ℃, constant temperature 1～2 hour, and stir;

C, will be heated to 75～85 ℃ through the material of b step system, air inducing 30～50 minutes is cooled to the room temperature after-filtration again, promptly makes DMH bullion and mother liquor;

D, will render in 150～300 parts of water and 700～900 parts of mother liquor mixtures through 950～1150 parts of DMH bullions that the c step makes; Stir while throwing in; Add 3～8 parts of activated carbon after being heated to 80～98 ℃, decoloured 20～40 minutes, remove by filter activated carbon; Crystallisation by cooling, centrifuging, oven dry more promptly makes the DMH finished product.

Embodiment 2

Of the present invention 5, the working method of 5-DMH is by following material, makes through following steps by weight:

A, 600 parts in 700 parts in bicarbonate of ammonia, acetone cyanohydrin is added water stir fully dissolving, airtight when being heated to 10 ℃;

B, in the material that makes through a step, feed 40 parts of ammonias again, slowly heat to 60 ℃, constant temperature 2 hours, and stir;

C, will be heated to 80 ℃ through the material of b step system, air inducing 40 minutes is cooled to the room temperature after-filtration again, promptly makes DMH bullion and mother liquor;

D, will render in the mixture of 800 parts in 200 parts in water and mother liquor through 1050 parts of DMH bullions that the c step makes; Stir while throwing in; Add 5 parts of activated carbon after being heated to 95 ℃, decoloured 30 minutes, remove by filter activated carbon; Crystallisation by cooling, centrifuging, oven dry more promptly makes the DMH finished product.

Embodiment 3

Of the present invention 5, the working method of 5-DMH is by following material, makes through following steps by weight:

A, 500 parts in 600 parts in bicarbonate of ammonia, acetone cyanohydrin is added water stir fully dissolving, airtight when being heated to 10 ℃;

B, in the material that makes through a step, feed 30 parts of ammonias again, slowly heat to 50 ℃, constant temperature 1.5 hours, and stir;

C, will be heated to 75 ℃ through the material of b step system, air inducing 30 minutes is cooled to the room temperature after-filtration again, promptly makes DMH bullion and mother liquor;

D, will render in the mixture of 700 parts in 150 parts in water and mother liquor through 950 parts of DMH bullions that the c step makes; Stir while throwing in; Add 3 parts of activated carbon after being heated to 90 ℃, decoloured 20 minutes, remove by filter activated carbon; Crystallisation by cooling, centrifuging, oven dry more promptly makes the DMH finished product.

Embodiment 4

Of the present invention 5, the working method of 5-DMH is by following material, makes through following steps by weight:

A, 700 parts in 800 parts in bicarbonate of ammonia, acetone cyanohydrin is added water stir fully dissolving, airtight when being heated to 10 ℃;

B, in the material that makes through a step, feed 50 parts of ammonias again, slowly heat to 65 ℃, constant temperature 2 hours, and stir;

C, will be heated to 85 ℃ through the material of b step system, air inducing 50 minutes is cooled to the room temperature after-filtration again, promptly makes DMH bullion and mother liquor;

D, will render in the mixture of 300 parts of water and 900 parts of mother liquors through 1150 parts of DMH bullions that the c step makes; Stir while throwing in; Add 8 parts of activated carbon after being heated to 95 ℃, decoloured 40 minutes, remove by filter activated carbon; Crystallisation by cooling, centrifuging, oven dry more promptly makes the DMH finished product.