Biotechnological method of obtaining aqueous solutions of acrylamide

 

(57) Abstract:

The invention relates to chemistry and biotechnology-based organic compounds. The method is carried out by the hydration of Acrylonitrile in an aqueous medium in the presence of the biocatalyst containing microorganisms with nitrilgidrataznoi activity. Hydration of Acrylonitrile is carried out in its 4-20% water mixture (2-4)10-5% anionic and (1,25-2,5)10-5% cationic copolymers. As biocatalyst used the biomass of the bacterial strain Rhodococcus rhodochrous. In the suspension of biomass pre-consistently give 0,4-3,0% aluminum sulphate, 0,05-0,30% anionic and 0.02-0.20% of cationic copolymers (by weight of dry cells). As the anionic copolymer is used copolymers of acrylamide containing 5-30 mol.% units of acrylic acid or its salts of ammonium or alkali metals. As the cationic copolymer is used copolymers of acrylamide and dialkylaminoalkyl(meth)acrylate, or their salts with hydrochloric or sulfuric acid, or their quaternionic salts dimethylsulfate, methyl chloride, containing 50-100 mole%, of cationic groups. The technical result of the present invention is taller than the first rate of hydration of Acrylonitrile under the action of the biocatalyst is quite high and is from 1.5 to 3.0 h-1. 1 C.p. f-crystals, 3 tables.

The invention relates to chemistry and technology of organic compounds, namely, to obtain aqueous solutions of acrylamide.

Acrylamide is used for the synthesis of high molecular weight polymers used in various technological processes: as thickeners in oil production, flocculants, superabsorbents for agricultural and medical purposes, as a waterproofing chemical processes in gas and oil production.

A method of obtaining aqueous solutions of acrylamide heterogeneous catalytic hydration of Acrylonitrile (Polyacrylamide / L. I. Abramov, I. A. Baiburdov, E. P. Grigoryan and others; Ed. by C. F. Kurenkov - M.: Chemistry, 1992 - S. 9-16).

This method allows you to obtain highly concentrated solutions of acrylamide with a mass fraction of 20-50%.

However, when the catalytic method of obtaining aqueous solutions of acrylamide produces many by-products and impurities ions of metals of variable valence, therefore, to obtain the target product required an additional step of purification of aqueous solutions of acrylamide, for example, various types of ion exchange resins from impurity ions of metals of variable valence is utilizatorul and ion exchange resins.

Biotechnological method of obtaining aqueous solutions of acrylamide, which is highly selective, environmentally friendly, energy-saving, allows to obtain concentrated solutions of monomer, containing no by-products. Thus, known methods for producing aqueous solutions of acrylamide by the hydration of Acrylonitrile in an aqueous medium under the action of the biocatalyst - strain Phodococcus rhodochrous (producer of enzyme nitrilimines) /Patent of USSR 1811698, CL 12 P 13/02, Appl. 11.06.91; RF Patent 2077588, CL 12 P 13/02, Appl. 16.01.96/.

Hydration of Acrylonitrile is carried out at pH 4.5-11 and at a temperature of from 3 to 50oWith in aqueous suspensions of biocatalyst containing 0.08 to 0.4 g/l biomass of strain Phodococcus rhodochrous M8 and m. Acrylonitrile is introduced into the reactor so that its concentration in the reaction medium did not exceed 2%. Get 7-50% solution of acrylamide.

However, to obtain the target product required an additional step of purification of aqueous solutions of acrylamide from waste biomass, for example, various methods of filtration (separation, centrifugation, filtration). The problem arises wastewater from washing of the filtration equipment.

Preliminary stadim the hydrogel, allows, on the one hand, to save nitrilimines the activity of microorganisms and, on the other hand, to obtain the target product (aqueous solutions of the monomer of high purity) without additional purification stages.

The closest in technical essence is a method of obtaining aqueous solutions of acrylamide by hydration of Acrylonitrile in the presence of microorganisms having nitrilgidrataznoi activity, immobilized cationic polymer hydrogel [U.S. Pat. USA 442855, 12 P 13/02, With 12 N 11/08, Appl. 14.08.1981, publ. 20.12.1983]. This method is as follows: pre-cook the biocatalyst, mix the biocatalyst with water and injected into the resulting suspension of biocatalyst aqueous solution of Acrylonitrile.

To obtain a biocatalyst mixed suspension of biomass with nitrilgidrataznoi activity, with acrylamide, a crosslinking agent and a water-soluble cationic acrylic monomer and/or copolymer, type initiators and polimerizuet at pH 5 to 10 and a temperature of from 0 to 30oC. the polymerization Time is 30-60 minutes will Polimerizuet Monomeric mixture in aqueous solution with mass fraction of 2-30%. The biomass content of the composition is about monomer and/or copolymer in the monomer mass is 50-95%, 0.1 to 20% 1-50%, respectively. Water-soluble cationic acrylic copolymers of acrylamide and dialkylaminoalkyl(meth)acrylate, or dialkylaminoalkyl(meth)acrylamides, or quaternionic salts used with the molecular weight (0.5 to 2.0)106. As initiators using potassium persulfate and dimethylaminopropionitrile.

The obtained water-insoluble cationic polymer hydrogel with immobilized microorganisms in it grind in the mixer and further treated for 1 h with stirring with glutaraldehyde of 0.25% by weight of the hydrogel, in 0.05 M phosphate buffer solution at a mass ratio of hydrogel to a solution of 1:3 and at a temperature of 10oC. Then the gel particles are washed in water.

The estimated amount of biocatalyst containing 1-4 g/l (by weight of dry cells) immobilized cells or enzymes of strain B-771 species Corynebacterium, strain N-774 species Corynebacterium strain N-775 Nocardia species, placed in the reaction column and passed through her water solution of Acrylonitrile with a concentration of not more than 5 wt.% at a rate of 0.5-0.8 h-1at a temperature of from 0 to 30oC and at pH 5 to 10.

On this biotechnology cleansing stage.

The performance of biotechnological process of obtaining the target product is determined by the volumetric rate of hydration of Acrylonitrile, showing the time of contact of source materials and immobilized microorganisms or enzymes needed to obtain the target product. The volumetric rate of the process of obtaining aqueous solutions of acrylamide with a mass fraction of 5-15% is 0.5-0.8 h-1. The number of processed biocatalyst is 3-12 g/kg of the desired product (100% basis).

The process of preparation of the biocatalyst is laborious and time consuming, there is the problem of disposal of sewage waste phosphate buffer solution used for washing jeleobraznyh polymer particles of the biocatalyst.

The task of the invention to provide aqueous solutions of acrylamide high purity by the method of high performance and environmental safety.

The technical result of the present invention is a significant increase in flow rate of the process to obtain the product, its quality, technical requirements, excluding time-consuming and laborious the tva spent biocatalyst.

The proposed method is as follows.

In a high-speed mixer prepare 4-10% aqueous suspension of microorganisms, dispersive pasta biomass in the water. The estimated amount of the obtained aqueous suspension of microorganisms introduced into the reaction column equipped with a jacket to regulate the temperature in the column within the required limits. In the lower part of the column in series with a pump injected aqueous solutions of aluminum sulphate, aminoacylase and cationic acrylic copolymer comprising by weight of dry cells 0,40-3,0%; 0.05 to 0.30% and 0,02-0,20%, respectively.

The biocatalyst can be prepared in a similar manner in a separate container, which is under mechanical stirring consistently injected aqueous suspension of microorganisms and aqueous solutions of aluminum sulphate, anionic and cationic copolymers.

The cooking time of the biocatalyst is 10-30 min depending on the desired amount of biocatalyst.

In the lower part of the column using a pump with a bulk velocity of 0.8 to 3.0 h-1enter the source reagent in aqueous mixtures containing 4-20% of Acrylonitrile, (2,0-4,0)10-5% aminooctanoic maintain a constant temperature, equal 3-50oC. Through the upper part of the column is continuously output the received 6-27% aqueous solution of acrylamide.

To obtain a highly concentrated aqueous solution of acrylamide 6-15% aqueous solution of the monomer from the 1st column, pre-mixed with the required amount of Acrylonitrile, with a bulk velocity of 0.8 to 3.0 h-1served through the lower part in the 2nd column, containing the biocatalyst prepared as described above. Through the top of the 2nd column output 20-32% aqueous solution of acrylamide, which is mixed with the required amount of Acrylonitrile and sent to the 3rd column with the biocatalyst, or used as a product.

The filing of the original substance in aqueous mixtures with anionic copolymer of acrylamide and a cationic copolymer of acylaminoalkyl(meth)acrylate, you can make a counter-current or direct-flow methods.

The proposed method uses one or more columns that are joined together into blocks, filled with a biocatalyst that continuously serves Acrylonitrile. Feed speed in the column of the source reagent may be different depending on the content in the biocatalyst strain and con the source reagent served continuously into the inlet of the separate sections of the column. Submission of Acrylonitrile in an aqueous mixture of anionic and cationic copolymers is provided in the first column, the next column in the process of obtaining highly concentrated solutions of acrylamide obtained by introducing aqueous solutions of acrylamide, pre-mixed only with Acrylonitrile. Use water mixed with Acrylonitrile copolymers in the proposed concentrations allows, on the one hand, to stabilize the biocatalyst - suspension strain of bacteria and, on the other hand, do not affect the purity of the target product.

Unlike the prototype of the proposed method, the target product is obtained by hydration of Acrylonitrile in its concentrated 4-20-percentage aqueous mixtures under the action of the biocatalyst containing strain Phodococcus rhodochrous - producenta nitrilimines. The proposed terms of the preliminary preparation of the biocatalyst and the implementation of the hydration of Acrylonitrile allow to increase the volumetric rate of the process while maintaining nitrilgidrataznoi activity of the biocatalyst in an aqueous mixtures of Acrylonitrile high concentrations, and also to reduce the amount of waste biocatalyst.

The volumetric rate of the receiving water right product (100% basis). Wastewater from the stage of preparation of the biocatalyst excluded.

For the preparation of the biocatalyst use biomass Phodococcus rhodochrous M8 or Phodococcus rhodochrous m - producer nitrilimines produced according to TU 9291-001-04836741-95 and THE 9291-003-04836741-97.

Use aluminium sulphate produced according to GOST 3758-65.

As anionic acrylic copolymer used copolymers of acrylamide, containing 5-30% of carboxylate units and having a characteristic viscosity 6-20 DL/g (determined in 10% sodium chloride solution at 25oWith the viscometer, Ballade with the diameter of the capillary of 0.54 mm).

As water-soluble cationic acrylic copolymer used copolymers of acrylamide and dialkylaminoalkyl (meth)acrylate or quaternionic salts dimethylsulfate, methyl chloride, and so on, the Content of cationic groups in the acrylic copolymer is 50-mol % . Cationic copolymers have a characteristic viscosity of 0.5 to 8 DL/g (determined in 10% sodium chloride solution at 25oWith the viscometer, Ballade with the diameter of the capillary of 0.54 mm).

The target product should be considered as aqueous solutions of acrylamide, trila not more than 0.1%, the content of acrylic acid is not more than 0.2%; the optical density of the solution is not more than 0.02, the content of polymer - absence. The concentration of acrylamide and the impurity content of Acrylonitrile and acrylic acid in the product is determined by gas chromatography. The presence of polymer in the target product is assessed visually by changing the opacity of a mixture of 100 ml methanol and 10 ml of acrylamide. If the solution of the acrylamide polymer is present, its alcoholic solution becomes cloudy or acquires opalestiruty shade. The optical density of a solution of acrylamide is determined on the photocolorimeter with a wavelength of 540 nm (green filter). The optical density of the target product, the component is not more than 0.02 demonstrates the absence of residual quantities of microorganisms.

Upon receipt of aqueous solutions of acrylamide that do not meet the quality requirements of the technical requirements, the filing of Acrylonitrile in the reaction column stop and conduct a comparative evaluation of received technical result is the flow rate of the process of obtaining the target product and the quantity of the spent biocatalyst.

The volumetric rate (OS, h-1) compute relative
The content of the spent biocatalyst (g/kg) calculated by the ratio of quantity of biomass used strain (M, g) to the amount of the target product in 100% basis (CC.etc., l):

ABOUT=M/SC.etc.< / BR>
Distinctive features of the proposed method to obtain aqueous solutions of acrylamide are conducting the hydration of Acrylonitrile in his 4-20% water mixture (2-4)10-5% anionic and (1,25-2,5)10-5% cationic copolymers under the action of the biocatalyst prepared by the sequential mixing of the aqueous slurry of the biomass of the bacterial strain with 0,40-3,00% aluminum sulphate, 0,05-0,30% anionic and 0.02-0.20% of the cationic copolymer (by weight of dry cells).

Using a strain of bacteria Phodococcus rhodochrous (producer of enzyme nitrilimines) in biotechnological production method of 5-50% of the energy of aqueous solutions of acrylamide is known.

Hydration of Acrylonitrile in its concentrated aqueous mixtures under the action of the biocatalyst, pre-cooked sequential mixing of the biomass of the bacterial strain with aluminum sulfate, anionic and cationic copolymers, in biotechnological method malonitrile in its concentrated aqueous mixtures with anionic and cationic copolymers in biotechnological method for obtaining aqueous solutions of acrylamide in scientific and technical literature is not described.

The essential features of the invention enables the achievement of a new technical result is increased productivity and environmental safety of the process of obtaining aqueous solutions of acrylamide. The volumetric rate of hydration of Acrylonitrile under the action of the biocatalyst is from 1.5 to 3.0 h-1. The amount of exhaust biocatalyst amount of 1.0 to 3.3 g/kg of the desired product (100% basis)

Osushestvljali method illustrated by the following examples.

Example 1.

In a vessel equipped with a stirrer and a jacket for cold water supply, was dispersed 20 g of 20% of the biomass of the strain Phodococcus rhodochrous M8 in 20 g of distilled water, the resulting suspension of biomass at room temperature sequentially injected with 30 ml of 0.17%-aqueous solution of aluminum sulphate, 30 ml of 0.025% aqueous solution of anionic copolymer of acrylamide containing 30 mol.% , carboxylate groups and having a characteristic viscosity of 15 DL/g, 30 ml of 0.017% aqueous solution of a cationic copolymer of acrylamide and methyl chloride Quaternary salt and dimethylaminoethylmethacrylate containing 80% of cationic groups and having kharakteristicheskoi activity in suspensions containing 4.0 g mass of dry cells, 1,28% aluminum sulphate, 0,19% anionic and 0.13% cationic copolymers (by weight of dry cells).

Installing column of chemical glass with a height of 70 cm and a diameter of 10 mm, with a capacity of 86 ml biocatalyst Prepared quantitatively transferred into a column. Then in column injected at a temperature of 15-18oWith a bulk velocity of 0.8 h-1Acrylonitrile 15.4% water mixture containing 410-5% anionic and 2,510-5% cationic copolymers used in the preparation of the biocatalyst with nitrilgidrataznoi activity.

Get 29,2 l 20,3%-aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 percent acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases the concentration of Acrylonitrile is above the allowed value.

100% calculation of the yield of acrylamide is 6.0 kg Content of the spent biocatalyst and 3.3 g/kg of the desired product (100% basis). Wastewater in the preparation of the biocatalyst is missing.

Comparative data is the totype)

In the polymerization reactor equipped with a stirrer and a jacket for cold water supply, was dispersed 50 g of 20% of the biomass of the strain Phodococcus rhodochrous M8 with 30 g of distilled water. Injected under stirring of the obtained suspension of the biomass of 4.2 g of acrylamide, 0.4 g of N,N - methylenebisacrylamide and 0.4 g of cationic copolymer and methyl chloride Quaternary salt and dimethylaminoethylmethacrylate to obtain a homogeneous suspension. Cationic copolymer contains 80 mol.% cationic groups and has a characteristic viscosity of 1 DL/g To polymerization in the resulting suspension containing 75% acrylamide, 5% methylenebisacrylamide and 20% cationic copolymer of acrylamide administered 5 ml of 5% aqueous solution of dimethylaminopropionitrile and 10 ml of 2.5% aqueous solution of potassium persulfate. Polymerization occurs at a temperature of not higher than 10oC for 1 h Obtained crosslinked water-absorbing cationic copolymer with immobilized biomass in the amount of 100 g crushed to fine polymer particles of size 1x3 mm and mixed with 300 ml of 0.05 M phosphate buffer solution containing 0.5 g of a 50% aqueous solution of glutaric aldehyde, for 1 h at a temperature not exceeding 10oC. Then poly is trihydrate activity containing 10 g mass of dry cells of strain.

Installing column of chemical glass with a height of 70 cm and 1 cm in diameter, with a capacity of 86 ml column load of 40 g of biocatalyst containing 4 g mass of dry cells, and injected at a temperature of 8-10oWith a bulk velocity of 0.8 h-1Acrylonitrile 15.4% water mixture, neutralized to pH 7.5 with sodium carbonate. At the outlet from the column will receive a 9% aqueous solution of acrylamide 8% solution of Acrylonitrile. To obtain the target product obtained aqueous solution of the Monomeric mixture of Acrylonitrile and acrylamide is injected at a temperature of 8-10oWith a bulk velocity of 0.8 h-1in the second column with a capacity of 150 ml, containing 60 g of biocatalyst (6 g mass of dry cells). Get 52 l 20,3%-aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 percent acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases the concentration of Acrylonitrile is above the allowed value.

100% calculation of the yield of acrylamide was 10.3 kg Content of the spent biocatalyst - 9.7 g/kg of the desired product (100% estimate the KTA (100% basis).

Comparative data method of producing an aqueous solution of acrylamide is shown in table. 1.

Example 2.

In a vessel equipped with a stirrer and a jacket for cold water supply, dispersed 2.5 g 20% of the biomass of the strain Phodococcus rhodochrous M8 in 40 g of distilled water. The resulting suspension of biomass quantitatively transferred into a column of chemical glass (height 700 mm and 10 mm in diameter, with a capacity of 86 ml). Then in the column at room temperature sequentially injected by a pump 30 ml of 0.017% aqueous solution of aluminum sulphate, 30 ml of 0.005% aqueous solution of anionic copolymer of acrylamide containing 30 mol.% carboxylate groups and having a characteristic viscosity of 15 DL/g, 30 ml 0,0035% aqueous solution of a cationic copolymer of acrylamide and methyl chloride Quaternary salt and dimethylaminoethylmethacrylate containing 80% cationic group and having a characteristic size 5 DL/g After 30 min of stirring by bubbling air get biocatalyst with nitrilgidrataznoi activity in suspensions containing 0.5 g mass of dry cells to 1.0% aluminum sulphate, 0.3% of anionic and 0.2% cationic copoly the d 3,0 h-14% aqueous solution of Acrylonitrile containing 4,010-5% anionic and 2,510-5% cationic copolymers used in the preparation of the biocatalyst with nitrilgidrataznoi activity. Get 14,7 l 5,1%-aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.1% of acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases the concentration of Acrylonitrile is above the allowed value.

100% calculation of the yield of acrylamide 0.75 kg. Content of the spent biocatalyst and 3.3 g/kg of the desired product (100% basis). Wastewater in the preparation of the biocatalyst is missing.

Comparative data method of producing an aqueous solution of acrylamide is shown in table. 1.

Example 2 comparative (prototype)

In the polymerization reactor equipped with a stirrer and a jacket for cold water supply, dispersed 6.25 g of 20% of the biomass of the strain Phodococcus rhodochrous M8 with 67,5 g of distilled water. Injected under stirring of the obtained suspension of the biomass of 4.2 g of acrylamide, 0.4 g of N,N-methylenebisacrylamide and 0.4 g Catino who produce a homogeneous suspension. Cationic copolymer contains 80 mol.% cationic groups and has a characteristic viscosity of 1 DL/g To polymerization in the resulting suspension containing 75% acrylamide, 5% methylenebisacrylamide and 20% cationic copolymer of acrylamide administered 5 ml of 5% aqueous solution of dimethylaminopropionitrile and 10 ml of 2.5-aqueous solution of potassium persulfate. Polymerization occurs at a temperature of not higher than 10oC for 1 h Obtained crosslinked water-absorbing cationic copolymer with immobilized biomass in the amount of 100 g crushed to fine polymer particles of size 1x3 mm and mixed with 300 ml of 0.05 M phosphate buffer solution containing 0.5 g of a 50% aqueous solution of glutaraldehyde for 1 h at a temperature not exceeding 10oC. Then the polymer gel particles with immobilized biomass was washed with water. Get 100 g of the biocatalyst with nitrilgidrataznoi activity containing 1,25 g mass of dry cells of strain.

Installing column of chemical glass with a height of 70 cm and 1 cm in diameter, with a capacity of 86 ml column load of 40 g of biocatalyst containing 0.5 g mass of dry cells, and injected at a temperature of 8-10oWith a bulk velocity of 3.0 HR-Ucaut 3% aqueous solution of acrylamide 1.8% solution of Acrylonitrile. To obtain the target product obtained aqueous solution of the Monomeric mixture of Acrylonitrile and acrylamide is injected at a temperature of 8-10oWith a bulk velocity of 3.0 HR-1in the second column with a capacity of 150 ml, containing 60 g of biocatalyst (0.75 g mass of dry cells). Get 14,7 l 5,1%-aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 percent acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases the concentration of Acrylonitrile is above the allowed value.

100% calculation of the yield of acrylamide 0.75 kg. Content of the spent biocatalyst - 133,3 g/kg of the desired product (100% basis). The content of wastewater (buffer solution in the preparation of biocatalyst) - 500 ml/kg of the desired product (100-NR-on-year).

Comparative data method of producing an aqueous solution of acrylamide is shown in table. 1.

Example 3

Analogously to example 2 fill in equal shares 2 columns suspension of biomass, prepared in dispersion of 10 g of 20% of the biomass of the strain Phodococcus rhodochrous M8 in 30 g of distilled water. Then in each column is of aluminum, 30 ml of 0.005% aqueous solution of anionic copolymer of acrylamide containing 30 mol.% carboxylate groups and having a characteristic viscosity of 15 DL/g, 33 ml of 0.003% aqueous solution of a cationic copolymer of acrylamide and methyl chloride Quaternary salt and dimethylaminoethylmethacrylate containing 80% cationic group and having a characteristic size 5 DL/g After 30 min stirring the bubbling of air in each column have the biocatalyst with nitrilgidrataznoi activity in a suspension containing 1.0 g mass of dry cells, of 1.0% of aluminum sulfate, 0.15% of anionic and 0.1% cationic copolymers (by weight of dry cells).

Then in the 1st column is injected at a temperature of 15-18oWith a bulk velocity of 0.8 h-1Acrylonitrile 20% water mixture containing 4,010-5% anionic and 2,510-5% cationic copolymers used in the preparation of the biocatalyst. Received 26,5% aqueous solution of acrylamide mixed with 10.3% of Acrylonitrile and send at a temperature of 8-10oWith a bulk velocity of 0.8 h-1in the second column. Get 7,2 l of 40.3%-aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 per cent and is to participate, as in an aqueous solution of acrylamide increases the concentration of Acrylonitrile is above the allowed value.

100% calculation of the yield of acrylamide is 3.0 kg Content of the spent biocatalyst and 3.3 g/kg of the desired product (100% basis). Wastewater in the preparation of the biocatalyst is missing.

Comparative data method of producing an aqueous solution of acrylamide is shown in table. 1.

Example 3 comparative (prototype)

In the polymerization reactor equipped with a stirrer and a jacket for cold water supply, dispersed 12.5 g of 20% of the biomass of the strain Phodococcus rhodochrous M8 with 67,5 g of distilled water. Injected under stirring of the obtained suspension of the biomass of 4.2 g of acrylamide, 0.4 g of N,N-methylenebisacrylamide and 0.4 g of cationic copolymer of acrylamide and methyl chloride Quaternary salt and dimethylaminoethylmethacrylate to obtain a homogeneous suspension. Cationic copolymer contains 80 mol.% cationic groups and has a characteristic viscosity of 1 DL/g To polymerization in the resulting suspension containing 75% acrylamide, 5% methylenebisacrylamide and 20% cationic copolymer of acrylamide administered 5 ml of 5% aqueous is the temperature not higher than 10oC for 1 hour. The obtained crosslinked water-absorbing cationic copolymer with immobilized biomass in the amount of 100 g crushed to fine polymer particles of size 1x3 mm and mixed with 300 ml of 0.05 M phosphate buffer solution containing 0.5 g of a 50% aqueous solution of glutaraldehyde for 1 h at a temperature not exceeding 10oC. Then the polymer gel particles with immobilized biomass was washed with water. Get 100 g of the biocatalyst with nitrilgidrataznoi activity, containing 2.5 g mass of dry cells of strain.

Installing column of chemical glass with a height of 70 cm and 1 cm in diameter, with a capacity of 86 ml column load of 40 g of biocatalyst containing 0.5 g mass of dry cells, and injected at a temperature of 8-10oWith a bulk velocity of 0.8 h-1Acrylonitrile 20% water mixture, neutralized to pH 7.5 with sodium carbonate. At the outlet from the column gain of 18.1% aqueous solution of acrylamide, 6.5% solution of Acrylonitrile. To obtain the target product obtained aqueous solution of the Monomeric mixture of Acrylonitrile and acrylamide is injected at a temperature of 8-10oWith a bulk velocity of 0.8 h-1in the second column with a capacity of 150 ml, containing 60 g of 0.1% Acrylonitrile, 0,2% acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increase above the required rate, the concentration of Acrylonitrile, and the optical density of the solution.

100% calculation of the yield of acrylamide 1.5 kg. Content of the spent biocatalyst - 66,7 g/kg of the desired product (100% basis). The content of wastewater (buffer solution in the preparation of biocatalyst) - 500 ml/kg of the desired product (100% basis).

Comparative data method of producing an aqueous solution of acrylamide is shown in table. 1.

Example 4

Analogously to example 1 fill a column with a slurry of biomass, prepared for the dispersion of 12.5 g of 20% of the biomass of the strain Phodococcus rhodochrous M8 in 20 g of distilled water. Then in the column at room temperature sequentially injected by a pump 30 ml 0,083% aqueous solution of aluminum sulphate, 30 ml of a 0.012% aqueous solution of anionic copolymer of acrylamide containing 20 mol.% carboxylate groups and having a characteristic viscosity 12 DL/g, 30 ml 0,008% aqueous solution of cationic acrylic copolymer is Rupp and having a characteristic size 6 DL/g After 30 min stirring by bubbling air get biocatalyst with nitrilgidrataznoi activity in suspensions containing 2.5 g mass of dry cells to 1.0% aluminum sulphate, 0.14% of the anionic and 0.1% cationic copolymers (by weight of dry cells).

Then in column injected at a temperature of 18-20oWith a bulk velocity of 0.8 h-1Acrylonitrile 16% water mixture containing 410-5% anionic and 2,510-5% cationic copolymers used in the preparation of the biocatalyst with nitrilgidrataznoi activity, with a pH of 8. Get 7,8 l 21,1% aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 percent acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases the concentration of Acrylonitrile is above the allowed value.

The yield of the desired product (100% basis) is 3.75 kg. Content of the spent biocatalyst and 3.3 g/kg of the desired product (100% basis). Wastewater in the preparation of the biocatalyst is missing.

Comparative data method of producing an aqueous solution of acrylamide Ptolemey when the dispersion of 5.0 g of 20% of the biomass of the strain Phodococcus rhodochrous M8 in 40 g of distilled water. Then in the column at room temperature sequentially injected by a pump 30 ml of 0.017% aqueous solution of aluminum sulphate, 30 ml of 0.005% solution of anionic copolymer of acrylamide containing 5 mol.% carboxylate groups and having a characteristic viscosity of 15 DL/g, 30 ml of 0.003% aqueous solution of a cationic copolymer of acrylamide and Quaternary salts dimethylsulfate and dimethylaminoethylmethacrylate containing 60% cationic group and having a characteristic size of 4 DL/g After 30 min of stirring by bubbling air get biocatalyst with nitrilgidrataznoi activity in a suspension containing 1.0 g mass of dry cells of 1.7% aluminum sulphate, 0.15% of anionic and 0.1% cationic copolymers (by weight of dry cells).

Then in column injected at a temperature of 10-14oWith a bulk velocity of 0.8 h-1Acrylonitrile 20% water mixture containing 4,010-5% anionic and 2,510-5% cationic copolymers used in the manufacture of the biocatalyst. Get a 5.4 l 26,5%-aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 percent acrylic acid and having the optical density of the solution, rtrace Acrylonitrile above the allowed value.

The yield of the desired product (100% basis) is 1.5 kg. Content of the spent biocatalyst and 3.3 g/kg of the desired product (100% basis). Wastewater in the preparation of the biocatalyst is missing.

Comparative data method of producing an aqueous solution of acrylamide is shown in table. 2.

Example 6

Analogously to example 1 fill a column with a slurry of biomass prepared in the dispersion of 2.5 g of 20% of the biomass of the strain Phodococcus rhodochrous M8 in 40 g of distilled water. Then in the column at room temperature sequentially injected by a pump 30 ml of 0.013% aqueous solution of aluminum sulphate, 25 ml of 0.003% aqueous solution of anionic copolymer of acrylamide containing 30 mol.% carboxylate groups and having a characteristic viscosity of 15 DL/g, 25 ml of 0.002% aqueous solution of a cationic copolymer of acrylamide and muriate of dimethylaminoethylmethacrylate containing 75% of cationic groups and having a characteristic size 5 DL/g After 30 min of stirring by bubbling air get biocatalyst with nitrilgidrataznoi activity in suspensions containing 0.5 g mass of dry cells, 0.8% of sernac the eat in column injected at a temperature of 12-16oWith a bulk velocity of 3.0 HR-1Acrylonitrile 16% water mixture containing 4,010-5% anionic and 2,510-5% cationic copolymers used in the preparation of the biocatalyst, with a pH of 8. Get a 3.4 l of 21.1%-aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 percent acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases the concentration of Acrylonitrile is above the allowed value.

The yield of the desired product (100% basis) is 0,73 kg Content of the spent biocatalyst - 3.4 g/kg of the desired product (100% basis). Wastewater in the preparation of the biocatalyst is missing.

Comparative data method of producing an aqueous solution of acrylamide is shown in table. 2.

Example 7.

Analogously to example 1 fill a column with a slurry of biomass prepared in the dispersion of 1.25 g of 20% of the biomass of the strain Phodococcus rhodochrous M8 in 30 g of distilled water. Then in the column at room temperature sequentially injected by a pump 25 ml of 0.02% aqueous solution of aluminum sulphate, 40 ml of 0.001% in racteristics viscosity of 15 DL/g, 25 ml of 0.001% aqueous solution of a cationic copolymer of acrylamide and nitrate salts diethylaminoethylmethacrylate containing 50% cationic group and having a characteristic size 5 DL/g After 30 min of stirring by bubbling air get biocatalyst with nitrilgidrataznoi activity in suspensions containing 0.25 g mass of dry cells, and 2.0% aluminum sulphate, 0.16% of anionic and 0.01% cationic copolymers (by weight of dry cells).

Then in column injected at a temperature of 10-12oWith a bulk velocity of 0.8 h-1Acrylonitrile 20% water mixture containing 4,010-5% anionic and 2,510-5% cationic copolymers used in the preparation of the biocatalyst, with a pH of 8. Get a 1.5 l 26,5%-aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 percent acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases the concentration of Acrylonitrile is above the allowed value.

The yield of the desired product (100% basis) is 0.4 kg. Content of the spent biocatalyst - 3.1 g/kg target p is positive data method of producing an aqueous solution of acrylamide is shown in table. 2.

Example 8.

Analogously to example 1 fill a column with a slurry of biomass prepared in the dispersion of 2.5 g of 20% of the biomass of the strain Phodococcus rhodochrous M8 in 40 g of distilled water. Then in the column at room temperature sequentially injected by a pump 30 ml of 0.05% aqueous solution of aluminum sulphate, 25 ml of 0.001% aqueous solution of anionic copolymer of acrylamide containing 30 mol.% carboxylate groups and having a characteristic viscosity of 15 DL/g, 33 ml 0,0003% aqueous solution of a cationic copolymer of acrylamide and methyl chloride Quaternary salt and dimethylaminoethylmethacrylate containing 80% cationic group and having a characteristic size 5 DL/g After 30 min of stirring by bubbling air get biocatalyst with nitrilgidrataznoi activity in suspensions containing 0.5 g mass of dry cells, a 3.0% aluminum sulfate, 0.005% of anionic and 0.02% cationic copolymers (by weight of dry cells).

Then in column injected at a temperature of 22oWith a bulk velocity of 3.0 HR-1a 6.5% aqueous solution of Acrylonitrile containing 4,010-5% anionic and 2,510-5% cationactive acrylamide, containing 0.1% of Acrylonitrile, 0.2 percent acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases the concentration of acronitrile above the allowed value.

The yield of the desired product (100% basis) is 0,73 kg Content of the spent biocatalyst - 3.4 g/kg of the desired product (100% basis). Wastewater in the preparation of the biocatalyst is missing.

Comparative data method of producing an aqueous solution of acrylamide is shown in table. 2.

Example 9.

Analogously to example 1 fill a column with a slurry of biomass prepared in the dispersion of 2.5 g of 20% of the biomass of the strain Phodococcus rhodochrous M8 in 40 g of distilled water. Then in the column at room temperature sequentially injected by a pump 30 ml 0,033% aqueous solution of aluminum sulphate, 30 ml 0,0025% aqueous solution of anionic copolymer of acrylamide containing 30 mol.% carboxylate groups and having a characteristic viscosity of 15 DL/g, 50 ml of 0.001% aqueous solution of a cationic copolymer of acrylamide and methyl chloride Quaternary salt and dimethylamine min stirring by bubbling air get biocatalyst with nitrilgidrataznoi activity in suspensions containing 0.5 g mass of dry cells, and 2.0% aluminum sulphate, 0.15% of anionic and 0.1% cationic copolymers (by weight of dry cells).

Then in column injected at a temperature of 50oWith a bulk velocity of 3.0 HR-1a 6.5% aqueous solution of Acrylonitrile containing 4,010-5% anionic and 2,510-5% cationic copolymers used in the preparation of the biocatalyst, with a pH of 7.0. Get 8,9 l 8,3% aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 percent acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases the concentration of Acrylonitrile is above the allowed value.

The yield of the desired product (100% basis) 0.75 kg. Content of the spent biocatalyst and 3.3 g/kg of the desired product (100% basis). Wastewater in the preparation of the biocatalyst is missing.

Comparative data method of producing an aqueous solution of acrylamide is shown in table. 2.

Example 10

Analogously to example 1 fill a column with a slurry of biomass prepared in dispersion 2.5 g 20%-but edutella injected by a pump 30 ml 0,007% aqueous solution of aluminium sulphate, 30 ml of 0.005% aqueous solution of anionic copolymer of acrylamide containing 30 mol.% carboxylate groups and having a characteristic viscosity of 15 DL/g, 33 ml of 0.003% aqueous solution of a cationic copolymer of acrylamide and methyl chloride Quaternary salt and dimethylaminoethylmethacrylate containing 80% cationic group and having a characteristic size 5 DL/g After 30 min of stirring by bubbling air get biocatalyst with nitrilgidrataznoi activity in suspensions containing 0.5 g mass of dry cells to 0.4% aluminum sulphate, 0,3 aminoacylase and 0.2% cationic copolymers (by weight of dry cells).

Then in column injected at a temperature of 3 to 10oWith a bulk velocity of 2.0 h-1a 6.5% aqueous solution of Acrylonitrile containing 4,010-5anionic and 2,510-5% cationic copolymers used in the preparation of the biocatalyst, with a pH of 8. Get 8,9 l 8,4%-aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 percent acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases the concentration of Acrylonitrile spent biocatalyst - 3,3 g/kg of the desired product (100% basis). Wastewater in the preparation of the biocatalyst is missing.

Comparative data method of producing an aqueous solution of acrylamide is shown in table. 2.

Example 11

Analogously to example 1 fill a column with a slurry of biomass prepared in the dispersion of 2.5 g of 20% of the biomass of the strain Phodococcus rhodochrous M8 40 mg of distilled water. Then in the column at room temperature sequentially injected by a pump 30 ml of 0.017% aqueous solution of aluminum sulphate, 30 ml 0,0025% aqueous solution of anionic copolymer of acrylamide containing 30 mol.% carboxylate groups and having a characteristic viscosity of 15 DL/g, 50 ml of 0.001% aqueous solution of a cationic copolymer of acrylamide and methyl chloride Quaternary salt and dimethylaminoethylmethacrylate containing 80% cationic group and having a characteristic size 5 DL/g After 30 min of stirring by bubbling air get biocatalyst with nitrilgidrataznoi activity in suspensions containing 0.5 g mass of dry cells, of 1.0% of aluminum sulfate, 0.15% of anionic and 0.1% cationic copolymer (by weight of dry cells).

-5anionic and 1,2510-5% cationic copolymers used in the preparation of the biocatalyst, with a pH of 4.5. Get a 4.5 l 16,5%-aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 percent acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases the concentration of Acrylonitrile is above the allowed value.

The yield of the desired product (100% basis) 0.75 kg. Content of the spent biocatalyst and 3.3 g/kg of the desired product (100% basis). Wastewater in the preparation of the biocatalyst is missing.

Comparative data method of producing an aqueous solution of acrylamide is shown in table. 2.

Example 12.

Analogously to example 3 is filled with equal parts of 2 columns suspension of biomass prepared in the dispersion of 5.0 g of 20% of the biomass of the strain Phodococcus rhodochrous m in 40 g of distilled water. Then in each column at room temperature sequentially injected by a pump 30 ml of 0.017% aqueous solution of aluminum sulphate, 30 ml 0,0025% aqueous solution of anionic copolymer akrilovogo solution of a cationic copolymer of acrylamide and methyl chloride Quaternary salt and dimethylaminoethylmethacrylate, containing 80% cationic group and having a characteristic size 5 DL/g After 30 min of stirring by bubbling air get biocatalyst with nitrilgidrataznoi activity in suspensions containing 0.5 g mass of dry cells, of 1.0% of aluminum sulfate, 0.15% of anionic and 0.1% cationic copolymers (by weight of dry cells).

Then in the 1st column is injected at a temperature of 16-18oWith a bulk velocity of 3.0 HR-1Acrylonitrile 12.6% water mixture containing 4,010-5% anionic and 2,510-5% cationic copolymers used in the preparation of the biocatalyst with nitrilgidrataznoi activity. Received 16.5% aqueous solution of acrylamide are mixed with 11.2 wt.% Acrylonitrile and injected at a temperature of 16-18oWith a bulk velocity of 3.0 HR-1in the 2nd column. Get a 15.1 l 31,5%-aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 percent acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases the concentration of Acrylonitrile is above the allowed value.

The yield of the desired product (100% basis) is in the preparation of the biocatalyst is missing.

Comparative data method of producing an aqueous solution of acrylamide is shown in table. 3.

Example 13

Analogously to example 3 is filled with equal parts of 2 columns suspension of biomass prepared in the dispersion of 5.0 g of 20% of the biomass of the strain Phodococcus rhodochrous m in 40 g of distilled water. Then in each column at room temperature sequentially injected by a pump 30 ml of 0.017% aqueous solution of aluminum sulphate, 30 ml 0,0025% aqueous solution of anionic copolymer of acrylamide containing 30 mol.% carboxylate groups and having a characteristic viscosity of 15 DL/g, 50 ml of 0.001% aqueous solution of cationic polymer methyl chloride Quaternary salt and dimethylaminoethylmethacrylate containing 100% cationic group and having a characteristic size of 0.5 DL/g After 30 min of stirring by bubbling air get biocatalyst with nitrilgidrataznoi activity in suspensions containing 0.5 g mass of dry cells, of 1.0% of aluminum sulfate, 0.15% of anionic and 0.1% cationic copolymer (by weight of dry cells).

Then in the 1st column is injected at a temperature of 16-18oWith a bulk velocity of 2.0 h-1Acrylonitrile in the preparation of the biocatalyst with nitrilgidrataznoi activity. Received 16.5% aqueous solution of acrylamide are mixed with 11.2 wt.% Acrylonitrile and injected at a temperature of 16-18oWith a bulk velocity of 2.0 h-1in the 2nd column. Get 15,5 l 31,5%-aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 percent acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases the concentration of Acrylonitrile is above the allowed value.

The yield of the desired product (100% basis) is 5.0 kg Content of the spent biocatalyst - 1.0 g/kg of the desired product (100% basis). Wastewater in the preparation of the biocatalyst is missing.

Comparative data method of producing an aqueous solution of acrylamide is shown in table. 3.

Example 14

Analogously to example 3 is filled with equal parts of 2 columns suspension of biomass prepared in the dispersion of 5.0 g of 20% of the biomass of the strain Phodococcus rhodochrous m in 40 g of distilled water. Then in each column at room temperature sequentially injected by a pump 30 ml of 0.017% aqueous solution of aluminum sulphate, 30 ml 0,0025% aqueous solution aminoate 15 DL/g, 50 ml of 0.001% aqueous solution of a cationic copolymer of acrylamide and muriate of dimethylaminoethylacrylate containing 80% cationic group and having a characteristic size of 2 DL/g After 30 min of stirring by bubbling air will receive the biocatalyst with nitrilgidrataznoi activity in suspensions containing 0.5 g mass of dry cells, of 1.0% of aluminum sulfate, 0.15% of anionic and 0.1% cationic copolymers (by weight of dry cells).

Then in the 1st column is injected at a temperature of 16-18oWith a bulk velocity of 1.5 h-1Acrylonitrile 12.6-Noah aqueous mixture containing 4,010-5% anionic and 2,510-5% cationic copolymers used in the preparation of the biocatalyst with nitrilgidrataznoi activity. Received 16.5% aqueous solution of acrylamide are mixed with 11.2% wt.% Acrylonitrile and injected at a temperature of 16-18oWith a bulk velocity of 1.5 h-1in the 2nd column. Get 15,5 l 31,5%-aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 percent acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases conc what is 5.0 kg The content of the spent biocatalyst - 1.0 g/kg of the desired product (100% basis). Wastewater in the preparation of the biocatalyst is missing.

Comparative data method of producing an aqueous solution of acrylamide is shown in table. 3.

Example 15

Analogously to example 3 is filled with equal parts of 3 columns suspension of biomass prepared in the dispersion of 7.5 g of 20% of the biomass of the strain Phodococcus rhodochrous m in 60 g of distilled water. Then in each column at room temperature sequentially injected by a pump 30 ml of 0.017% aqueous solution of aluminum sulphate, 30 ml 0,0025% aqueous solution of anionic copolymer of acrylamide containing 30 mol.% carboxylate groups and having a characteristic viscosity 6 DL/g, 50 ml of 0.001% aqueous solution of a cationic copolymer of acrylamide and methyl chloride Quaternary salt and dimethylaminoethylmethacrylate containing 50% cationic group and having a characteristic size of 8 DL/g After 30 min of stirring by bubbling air get biocatalyst with nitrilgidrataznoi activity in suspensions containing 0.5 g mass of dry cells, of 1.0% of aluminum sulfate, 0.15% of an at a temperature of 16-18oWith a bulk velocity of 3.0 HR-1a 6.5% aqueous solution of Acrylonitrile containing 4,010-5% anionic and 2,510-5% cationic copolymer used in the preparation of the biocatalyst with nitrilgidrataznoi activity. Received 8.7 percent aqueous solution of acrylamide are mixed with 11.2 wt.% Acrylonitrile and injected at a temperature of 16-18oWith a bulk velocity of 3.0 HR-1in the 2nd column. All of 23,6% aqueous solution of acrylamide from the 2nd column is mixed with 11 wt. % of Acrylonitrile and enter in the 3rd column at a temperature of 16-18oWith a bulk velocity of 3.0 HR-1. Get 18,8 l 38,1% aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 percent acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases the concentration of Acrylonitrile is above the allowed value.

The yield of the desired product (100% basis) is 7.4 kg Content of the spent biocatalyst - 1.0 g/kg of the desired product (100% basis). Wastewater in the preparation of the biocatalyst is missing.

Comparative data method of producing an aqueous solution by crispinian biomass, prepared in dispersion of 7.5 g of 20% of the biomass of the strain Phodococcus rhodochrous m in 60 g of distilled water. Then in each column at room temperature sequentially injected by a pump 30 ml of 0.017% aqueous solution of aluminum sulphate, 30 ml 0,0025% aqueous solution of anionic copolymer of acrylamide containing 30 mol.% carboxylate groups and having a characteristic viscosity of 15 DL/g, 50 ml of 0.001% aqueous solution of a cationic copolymer of acrylamide and methyl chloride Quaternary salt and dimethylaminoethylmethacrylate containing 80% cationic group and having a characteristic size 5 DL/g After 30 min of stirring by bubbling air get biocatalyst with nitrilgidrataznoi activity in suspensions containing 0.5 g mass of dry cells, of 1.0% of aluminum sulfate, 0.15% of anionic and 0.1% cationic copolymers (by weight of dry cells).

Then in the 1st column is injected at a temperature of 16-18oWith a bulk velocity of 1.5 h-1a 6.5% aqueous solution of Acrylonitrile containing 4,010-5% anionic and 2,510-5; cationic copolymers used in the preparation of the biocatalyst with nitrilgidrataznoi 16-18oWith a bulk velocity of 1.5 h-1in the 2nd column. All of 28,7% aqueous solution of acrylamide from the 2nd column is mixed from 12.6 wt.% Acrylonitrile and enter in the 3rd column at a temperature of 12-14oWith a bulk velocity of 1.5 h-1. Get to 15.4 l of 45.3%-aqueous solution of acrylamide containing 0.1% of Acrylonitrile, 0.2 of acrylic acid and having an optical density of a solution of 0.01. Next, the filing of the original substances cease, as in an aqueous solution of acrylamide increases the concentration of Acrylonitrile is above the allowed value.

The yield of the desired product (100% basis) is 7.2 kg Content of the spent biocatalyst - 1.0 g/kg of the desired product (100% basis). Wastewater in the preparation of the biocatalyst is missing.

Comparative data method of producing an aqueous solution of acrylamide is shown in table. 3.

1. Biotechnological method of obtaining aqueous solutions of acrylamide by hydration of Acrylonitrile in an aqueous medium in the presence of the biocatalyst containing microorganisms with nitrilgidrataznoi activity, characterized in that the hydration of Acrylonitrile is carried out in its 4-20% water mixture (2-4) 10-5dnow suspension of the biomass of the bacterial strain Rhodococcus rhodochrous - producer nitrilimines, in which pre-consistently give 0,4-3,0% aluminum sulphate, 0,05-0,30% anionic and 0.02-0.20% of cationic copolymers (by weight of dry cells).

2. The method according to p. 1, characterized in that as the anionic copolymer is used copolymers of acrylamide containing 5-30 mol. % of units of acrylic acid or its salts of ammonium or alkali metals, and as a cationic copolymer used copolymers of acrylamide and dialkylaminoalkyl (meth)acrylate, or their salts with hydrochloric, or sulfuric acid, or their quaternionic salts dimethylsulfate, methyl chloride, containing 50 to 100 mol. % cationic groups.

 

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