Method of producing polyhexamethylene guanidine hydrochloride

FIELD: chemistry.

SUBSTANCE: method of producing a disinfectant involves first carrying out polycondensation of hexamethylenediamine and guanidine hydrochloride. Polycondensation starts with preparation of a reaction mass in form of a suspension of crystalline guanidine hydrochloride in molten hexamethylenediamine, taken in ratio of 1:(1-1.5). The suspension is obtained by gradually adding crystalline guanidine hydrochloride, preheated to temperature of 90-120°C, to molten hexamethylenediamine and then stirring. The reaction mass is then heated in steps: holding for 4 hours at 120°C, then for 8 hours at 160°C and then for 3 hours at 180°C. Temperature is then gradually raised to 210°C at a rate of 3-4°C/h. The reaction mass is then subjected to vacuum treatment and cooled.

EFFECT: method enables to reduce toxicity of the end product and obtain a polymer with the required molecular weight and sufficient purity without washing steps.

2 tbl

 

The proposed method relates to the field of polymeric organic chemistry, in particular to a method for polyhexamethylene guanidine hydrochloride, which can be used as an effective disinfectant, used in medicine, veterinary medicine, sewage treatment, and in industries where the use of biocidal products.

A method of obtaining a disinfectant, comprising the polycondensation of diamine and guanidine hydrochloride and subsequent heating (see the description of the author's certificate of the Russian Federation No. 1616898, IPC SS 279/00, A61L 2/16, publ. 30.12.1990).

In the known method a uniform introduction of molten diamine in the melt guanidine hydrochloride is carried out in a ratio of 1:(0,85-0,95) for 2.5 h, the mixture is heated to a temperature of 180°C, and after the introduction of the diamine, the temperature was raised to 240°C and maintain it for 5 hours

Disinfectant obtained in a known manner, has a low bacteriostatic activity and high toxicity, due to contamination of its hexamethylenediamine were, which is the toxic substance of the second class of danger that is his fault.

The closest to the essential features to the proposed method is adopted as a prototype, is a method of obtaining a disinfectant, comprising the polycondensation of diamine and guanidine hydrochloride and subsequent stepwise heating of the reaction mass (see the description of the invention to the patent of Russian Federation №2165268, IPC A61L 2/16, C08G 73/00, publ. 20.04.2001).

In the known method previously get guanidine hydrochloride by reacting ammonium chloride with dicyandiamide when heated. Then assetsat the polycondensation of a guanidine hydrochloride with hexamethylenediamine were under heating, adding to the resulting polyhexamethylene guanidine hydrochloride water to the concentration in the solution is not higher than 40%, the introduction in the resulting alkaline solution and the reaction saponification, the Department obtained the founding of guanidine, his washing, introduction to the basis of the acid and the subsequent allocation of the target product, and polycondensation of the salt of guanidine with hexamethylenediamine were carried out by heating in three stages, by heating this reaction mass in the first stage to a temperature not higher than 130°C, the second to a temperature not above 150°C, and the third to a temperature not above 180°C, the saponification reaction is carried out at a temperature not exceeding 60°C, and washing the Foundation carried out with a solution of chloride of an alkali metal, giving the basis of the acid and then allocate CE the eve of the product.

The known method does not allow to obtain a final product of sufficient purity without washing stages, and the need for multiple washing leads to the formation of large amounts of sewage and pollution, what is the disadvantages of this method.

The technical objective of the proposed method is the cheaper way and improving its environmental performance.

The technical problem is solved in that in the method of obtaining a disinfectant, comprising the polycondensation of diamine and guanidine hydrochloride and subsequent stepwise heating of the reaction mass, the polycondensation process starts with preparation of the reaction mass in the form of a suspension of crystalline guanidine hydrochloride in the melt diamine, taken in the ratio 1: (1-1,5), the suspension get a smooth introduction into the melt of the crystalline diamine Gunaydin hydrochloride, preheated to a temperature of 90-120°C. and further stirring, after which the resulting reaction mass incubated 4 hours at a temperature of 120°C, then 8 hours at a temperature of 160°C 3 hours at a temperature of 180°C and then the temperature is gradually raised to 210°C at the rate of 3-4°C/hour, then the reaction mass is subjected to vacuum and cooling.

The inventive method allows to get the final product of sufficient purity without washing stages, removing from the reaction mass volatile impurities through a process of degassing of the reaction mixture does not pollute the environment.

The polycondensation process, the proposed method starts with the preliminary preparation of a crystalline suspension of guanidine hydrochloride in the melt diamine at a temperature of 90-120°C, which in the pre-molten hexamethylenediamine were, with a temperature of 90-120°C. gradually add crystalline guanidine hydrochloride, preheated to the same temperature and produce their mixing. This allows you to get the original oligomer components, excluding the destruction of guanidine hydrochloride, what happens when you melt termostabilno guanidine hydrochloride, and exclude the output from the reaction zone volatile diamine.

The proposed method allows to carry out the polycondensation with optimal speed, maintaining the optimum viscosity of the melt and eliminate foaming of the reaction mixture, and to form the desired polymer molecular weight.

A method for production of polyhexamethylene guanidine hydrochloride in the laboratory implemented as follows.

The process is carried out in a round-bottom chetyrehvalkovoj the flask with a capacity of 500 ml equipped with a stirrer and a thermometer.

Heating is carried out in carbonaria is barely LAB SC-500.

In round-bottom chetyrehmetrovuyu flask fall asleep 110 grams of diamine in solid form, set heating mantle to 100°C and maintained at this temperature for 1 hour until complete melting. After that, when the stirrer and vacuum in the flask was poured 100 grams of crystalline guanidine hydrochloride. In the mixing produces a suspension of guanidine hydrochloride in the melt diamine in the ratio 1:1,1, which is then transferred to the reaction mass.

After the reaction mass is heated to 120°C and maintained for 4 hours, controlling for the response on selection of the ammonia.

When slowing down of the reaction the reaction mass is heated to 160°C and incubated for 8 hours while passing through the reaction of the ammonia.

Then the temperature of the reaction mass was raised to 180°C and maintained for 3 hours. After this exposure raises the temperature to 210°C gradually 3-4°C per hour until the termination of allocation of ammonia and receive polyhexamethylene guanidine hydrochloride of the desired molecular weight, which is determined by the viscosity of the reaction mass.

Upon reaching polyhexamethylene guanidine hydrochloride (phmg-GC) of the desired molecular weight of the heating is stopped and the product is subjected to degassing, removing from the reaction mass volatile impurities, and there is but ammonia NH 3, unreacted hexamethylenediamine were, free chlorine, etc.

When reaching a vacuum of 30 MAG vacuum stop. Release the vacuum with nitrogen. The finished product in the form of a melt is poured on a metal tray to cool to ambient temperature.

Similarly processes were conducted in other molar ratios of guanidine hydrochloride (HGH) and hexamethylenediamine were (HMDA)equal to 1:1.2 and 1:1,5. The results and data analysis are summarized in tables 1 and 2.

Table 1
Rheological properties.
The molar ratio of HGH:HMDAThe aggregate stateColorSmellSolubility in water
1,1A solid crystalline substanceA transparent substance with a slight yellow tintNoFull
1,2A solid crystalline substanceA transparent substance with a slight yellow tintNo Full
1,5A solid crystalline substanceA transparent substance with a slight yellow tintNoFull

Table 2
Physico-chemical properties.
The molar ratio of HGH:HMDAOutput pgmg-GC, %PH of 1%water solutionMolecular weightResidual HGH, %Residual GMD, %Free ChlorineAmmonia
1,197,29,2≈280000,0250,054neobar.no
1,298,67,6≈200000,0510,025neobar no
1,596,96,9≈150000,1000,025neobarno

In all three examples produced in this way was obtained macromolecular polymer - pgmg-GC, completely soluble in water with a high content of basic substance, and a minimum number of dangerous impurities. The effectiveness test set:

The death of the bacteria E.coli and S.aureus provides a 0.05% solution of the obtained substances pgmg-GC current substance within 60 minutes of exposure by wiping. Death on the surfaces of C.albicans achieved a 1% solution under the current substance within 120 minutes of exposure in the same way.

The method of obtaining a disinfectant, comprising the polycondensation of diamine and guanidine hydrochloride and subsequent stepwise heating of the reaction mixture, characterized in that the polycondensation process starts with preparation of the reaction mass in the form of a suspension of crystalline guanidine hydrochloride in the melt diamine, taken in the ratio 1: (1-1,5), the suspension get a smooth introduction into the melt diamine, cristalli the definition guanidine hydrochloride, preheated to a temperature of 90-120°C., and then stirring, after which the resulting reaction mass incubated 4 hours at a temperature of 120°C, then 8 hours at a temperature of 160°C, 3 h at 180°C and then the temperature is gradually raised to 210°C at the rate of 3-4°C/h, then the reaction mass is subjected to vacuum and cooling.



 

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