Method of producing highly purified disinfectant

FIELD: chemistry.

SUBSTANCE: described is a method of producing a highly purified disinfectant which contains polyhexamethylene guanidine hydrochloride, characterised by that flush water from production of polyhexamethylene guanidine hydrochloride in solid form is used. The flush water is mixed with 25% NaCl solution in ratio of 1:1 (polyhexamethylene guanidine hydrochloride solution with impurities: NaCl solution) while stirring constantly for 1 hour at temperature in the range of 50-60°C. Stirring is stopped and the mixture is cooled to 5°C, thereby dividing the mixture into two parts; the bottom part is drained, neutralised and sent for recycling and the top part containing up to 60-70% polyhexamethylene guanidine hydrochloride is further diluted to 50% with an aqueous solution of quaternary ammonium salts (QAS) to QAS concentration of not higher than 5%.

EFFECT: extracting highly purified, concentrated high-molecular weight polyhexamethylene guanidine hydrochloride from flush water, reducing the amount and toxicity of waste water, improving disinfecting properties and increasing output of the commercial-grade product when producing polyhexamethylene guanidine hydrochloride in solid form, reducing cost.

1 cl, 1 ex, 2 tbl

 

The proposed method relates to the field of polymeric organic chemistry, in particular to a method for producing high-purity disinfectant that 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 (see the description of the author's certificate of the Russian Federation No. 1616898, IPC C07C 279/00, A61L 2/16, publ. 30.12.1990).

The known method is based on the polycondensation of a diamine (HMDA) and guanidine hydrochloride (HGH), resulting in a receive end - product disinfectant - polyhexamethylene guanidine hydrochloride (phmg-GC) in solid form. The polycondensation is performed by heating and uniform introduction of the melt, HMDA in the melt HGH in the ratio 1:(0,85-0,95) for 2.5 h, the mixture is heated to a temperature of 180°C, and after the introduction of GMDA the temperature was raised to 240°C and maintain it for 5 hours

After discharge of each batch of finished product equipment should be washed and the wash water is drained. Wash water partially contain pgmg-GC, resulting in the contamination of the environment.

Obtained in a known manner pgmg-GC has a small bacteriol the political activity and high toxicity due to contamination of its HMDA, which is the toxic substance of the second class of danger.

A method of obtaining a disinfectant, adopted as a prototype (see the description of the invention to the patent of Russian Federation №2165268, IPC A61L 2/16, C08G 73/00, publ. 20.04.2001).

The known method is based on polycondensation of HMDA and HGH. In the known method previously get HGH by reacting ammonium chloride with dicyandiamide when heated. The polycondensation of the salt of guanidine with HMDA 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 higher than 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 base of the acid, and then allocate pgmg-GC in solid form.

In the known method requires multiple rinsing of the equipment, leading to the formation of large amounts of flush water flowing into the waste water polluting the environment, which is the main disadvantage of this method. Wastewater contain the product pgmg-GC, and impurities such as the unreacted HMDA, which vysokoletuchie and toxic, low molecular weight oligomers, polymerge the Chelyabinsk, which are less toxic, but degrades the quality of the finished product.

Get pgmg-GH is an effective polymeric biocide against wide spectrum of gram-positive and gram-negative bacteria do not form toxic products in the water, not inactivated protein, is easily decomposed by enzyme systems of the person, but does not destroy bacteria with hydrophobic lipid wax shell.

The technical objective of the proposed method is the extraction of highly purified, concentrated pgmg-GC high molecular weight (about 20 000) of wash water, reducing the amount and toxicity of waste water, the improvement disinfectant properties and increase the yield of marketable products in the production pgmg-GC in solid form, reducing the cost.

The technical problem is solved in that in the method of obtaining high-purity disinfectant containing polyhexamethylene guanidine hydrochloride, used wash water from the production of polyhexamethylene guanidine hydrochloride in solid form, which is collected, then mixed with 25%NaCl solution at a ratio of 1:1 (solution of guanidine hydrochloride with impurities:NaCl solution) under stirring for 1 hour at a temperature in the range of 50-60°C, and then the stirring is stopped, Hledat to a temperature of 5°C, thereby making the separation into two parts, the lower part of the waste is neutralized and sent for recycling, and the upper part containing up to 60-70% polyhexamethylene guanidine hydrochloride, optionally diluted with 50% aqueous solution HOUR to HOUR concentration not higher than 5%.

The proposed method allows to:

to get to production of the disinfectant highly purified solution of polyhexamethylene guanidine hydrochloride high concentrations;

- reduce the amount and toxicity of wastewaters;

- to increase output per unit of raw material in the production of polyhexamethylene guanidine hydrochloride in solid form;

to ensure the ability of the disinfectant on the basis of polyhexamethylene guanidine hydrochloride to destroy a wide spectrum of gram-positive and gram-negative bacteria as well as bacteria with hydrophobic lipid wax shell.

The inventive method consists of isolating highly purified, concentrated pgmg-GC of flushing water, polecamy in the production pgmg-GC in solid form. Wash water is used repeatedly, as a result they accumulate pgmg-GC. After saturation of the wash water pgmg-H.H. the washing quality is deteriorating, the wash water is fed into the apparatus, and for washing equipment serves a portion of fresh water.

AP is Arat equipped with a stirrer, jacket heating / cooling and bottom discharge with dividing lantern. In the apparatus gradually add 25%NaCl solution with constant stirring for 1 hour. The temperature in the apparatus is maintained within the range of 50-60°C with a sharp pair. Then stop stirring and shirt apparatus serves the coolant from brine installation with a temperature of 5°C. When cooling is delamination of the contents of the device into two parts. The top layer contains high-purity aqueous solution pgmg-GC for the production of a disinfectant, in which there are no low molecular weight oligomers and free amines, which become the bottom layer of NaCl solution.

The bottom layer is separated using a separating lantern, neutralized with 1%HCl solution to pH 5-6 and sent for recycling. A purified solution pgmg-GC upper layer was diluted to 50% (commercial product) in an aqueous solution of H (Quaternary ammonium salts), for example, CATPAW CAS No. 61798-71-7 or KATHHOJ CAS No. 85736-63-6. Diluted so that the total number of HOURS in the solution did not exceed 5%.

Example

Wash water received 10 cycles of washing equipment in the production pgmg-GC in solid form consisting of water and 3000 kg and KZT 446.4 kg impurities in the number 3446,4 kg fed into the apparatus, equipped with a stirrer, jacket heating of the-cooling and bottom discharge with dividing lantern and then gradually add 25%solution of NaCl at a ratio of 1:1 by weight (solution pgmg-GC with impurities:NaCl) with constant stirring for 1 hour. The temperature in the apparatus is maintained within the range of 50-60°C with a sharp pair. Then stop stirring and shirt apparatus serves the coolant from brine installation with a temperature of 5°C. When cooling is delamination of the contents of the device into two parts. The top layer contains high-purity aqueous solution pgmg-GC for the production of a disinfectant, in which there are no low molecular weight oligomers and free amines, which become the bottom layer of NaCl solution.

The bottom layer is separated using a separating lantern, neutralized with 1%HCl solution to pH 5-6 and sent for recycling.

Next, measure the concentration of a purified solution pgmg-GC upper layer, which may be 60-70%.

Depending on the results of measurement of the top layer in the device is again heated to 50-60°C and further diluted with up to 50% (commercial product) in an aqueous solution of H (Quaternary ammonium salts), CATPAW CAS No. 61798-71-7. Diluted so that the total number of HOURS in the solution did not exceed 5%, necessary for the destruction of disinfectant bacteria with hydrophobic lipid wax shell.

Was the analysis of the composition of the layers, which are shown in table 1.

Table 1
pHCommodity pgmg-GCTotal impurities, including NaClWaterTotal
%kg%kg%kg%kg
The top layer7.969,900,0530,05100,00
352,100,25151,37503,72
The bottom layer6.80,00 14,9685,04100,00
0,00955,705433,466389,16

As can be seen from table 1, managed to get 352,1 kg macromolecular pgmg-GC (calculated on the dry product) of highly purified (>99%) and concentrate the solution up to 69.9%. It is possible to increase the yield of marketable product per unit of raw material by 4.7%.

The remaining bottom layer with a pH of 6.8 in the number 6389,16 kg transfer for recycling, representing 21% of the same amount of wastewater. A large part of the pollution goes into neutral compounds do not pose a great threat to the environment.

Analysis of the composition of the wash water at a pH of 10.5 are shown in table 2.

Table 2
HGHHMDAOligomers and low molecular weight polymer homologuesovary pgmg-GC Uncertain to 100%WaterTotal
%1,310,160,8010,450,2387,05100,00
kg45,32the ceiling of 5.6027,52360,10of 7.903000,003446,44

The method of obtaining high-purity disinfectant containing polyhexamethylene guanidine hydrochloride, characterized in that the used wash water from the production of polyhexamethylene guanidine hydrochloride in solid form, which is collected, then mixed with 25%NaCl solution at a ratio of 1:1 (solution of guanidine hydrochloride with impurities: NaCl solution) under stirring for 1 hour at a temperature in the range of 50-60°C, then stop stirring, cooled to a temperature of 5°C, thereby making the separation into two parts, the lower part of the waste is neutralized and sent for recycling, and the upper the part containing up to 60-70% of polyhexamethyl the guanidine hydrochloride, further diluted with 50% aqueous solution of H (Quaternary ammonium salts) to the concentration of the HOUR of not more than 5%.



 

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1 cl, 18 ex, 1 tbl

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3 cl, 4 ex, 4 tbl

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7 cl, 4 tbl, 10 ex

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1 cl, 2 tbl

FIELD: chemistry.

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5 ex, 7 cl

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2 tbl, 2 ex

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EFFECT: invention enable to obtain heteropolymer salts with high antimicrobial activity.

4 cl, tbl, 7 ex

FIELD: organic chemistry, medicine, cardiology.

SUBSTANCE: invention describes compounds of the formula (I): wherein R1 and R2 mean hydrogen atom (H), alkyl, fluorine (F), chlorine (Cl), bromine (Br) atom, alkoxy-group, -S(O)nR7, polyfluoroalkyl, polyfluoroalkoxy-group; R3 means Alk-R8, cycloalkyl; R8 means H, cycloalkyl, polyfluoroalkyl, phenyl or -OH; R4, R5 and R6 mean H or alkyl; R7 means alkyl. Also, invention relates to a method for synthesis of these compounds and a pharmaceutical composition possessing inhibitory activity with respect to Na+/K+ cellular exchange. Proposed compounds are suitable as anti-arrhythmic medicinal agents with a cardioprotective component used in prophylaxis of infarction and treatment of infarction and treatment of stenocardia. Compounds inhibit also pathophysiological process by prophylactic effect associated with development of disorders induced by ischemia, in particular, arising ischemia-induced cardiac arrhythmia and cardiac insufficiency.

EFFECT: valuable medicinal properties of compounds and pharmaceutical composition.

17 cl, 59 ex

The invention relates to a method for disinfectants that can be used in medicine, veterinary medicine, agriculture, water purification and air in the housing and communal services

FIELD: medicine.

SUBSTANCE: invention refers to disinfection. The experimental method for the elimination of pathogenic and opportunistic microorganisms is characterized by the fact that a mixture containing the pathogenic and opportunistic microorganisms are processed with a disinfection composition which is metal oxyhydrate gel prepared by alkaline metal chloride deposition by 2% ammonia in a min. 5-litre reactor; fresh metal oxyhydrate 20-10-6 m3 is placed in an electrochemical cells with graphite electrodes of a charged cluster metal particle generator; what is added is a bacterial solution of the medium of 105 microbial cells in 1 ml dissolved in distilled water 10 ml; the medium is exposed to polarized currents of the cluster oxyhydrate particles of metal oxyhydrate gel for 2 to 6 hours; metal oxyhydrate gels are prepared by using metal chloride salts presented by zirconium or iron chloride salts with the electrode distance no more than 70 mm.

EFFECT: invention provides the more effective inactivation of pathogenic and opportunistic microorganisms that are infectious agents in human and animals.

7 tbl, 2 dwg, 6 ex

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