Method of making antibacterial polymer membrane

FIELD: process engineering.

SUBSTANCE: invention relates to membrane technology, particularly, to production of antibacterial polymer membranes to be used in water and aqueous solution treatment in food and pharmaceutical industries, and medicine. Proposed method comprises making polymer solution, forming of polymer membrane and processing with antibacterial substance. Produced membrane is dried, rinsed with water and subjected to final drying. Said antibacterial substance represents composition containing the following components in wt %: 5-10 of poorly soluble or insoluble slats of silver, 2-25 of formic acid an 65-93 of water.

EFFECT: prolonged antibacterial properties.

9 ex

 

The invention relates to membrane technology and can be widely used for treatment of water and aqueous solutions in the food, pharmaceutical and other industries, as well as medicine.

One of the most important problems of membrane technology is the performance degradation of the membrane due to the formation on their surface precipitation. Unlike pollution membranes of colloidal and crystalline sediments, bacteria and microorganisms not only deposited on the membrane surface, but in the future breed, grow through the pores and contaminate the filtrate. The use of different antibacterial (antimicrobial next antibacterial) additives is a very promising method of dealing with biological contamination of polymeric membranes.

Antibacterial activity has a significant amount of natural and synthetic substances and compounds, but only some of them can be used for immobilization on the membrane surface. These may be presented with the following requirements:

- safety for the human body bactericidal agents modifiers in concentrations sufficient to suppress microorganisms;

- high activity of active substances, and a wide range of their antibacterial is Astia, which must be retained for the required period of operation,

The emergence of new strains of bacteria resistant to conventional antibiotics has become a serious problem for the health of the people; this fact has served as a powerful stimulus for the development of new bactericides. It is known that silver and some of its salts have a strong toxic to most microorganisms; for this reason, silver in various modifications, as well as the compositions containing silver, is extensively used as antibacterial additives.

To this problem the use of silver preparations interest is not waning and now: her many publications, for example, Silver nanoparticles as antimicrobial agents", publ. in "Colloid and Interface Science" in 2004 (275, 177-182). "Polysulfone ultrafiltration membranes impregnated with silver nanoparticles for removal of viruses with high resistance to biofouling", publ. in "Water Research/ Journal of the International Water Association" in 2009(No. 43 SS-723), article domestic scientists "Silver with delivery in a cage" (publ. on the website of the company ARGO). The above research work are ways to create antibacterial drugs based on silver nanoparticles. The disadvantages of these developments are technological difficulties of introducing n is nocaster silver in the required quantity, as well as reducing the effectiveness of their application due to the leaching of nanoparticles from the polymer matrix membrane with its usage.

Known application for U.S. patent No. 20110024355 firm Polymers CRC (publ. 2011) "Antimicrobial membrane". The invention relates to antimicrobial compositions for polymeric membranes in gas and water, representing silver zeolites, combined with the compounds of zinc and elemental silver with a highly developed surface. The disadvantage of this solution is to reduce the stability of the antibacterial properties of the membrane in its application due to the gradual leaching of the applied compounds from the polymer matrix.

The closest technical solution to the claimed is a method of obtaining a polymer ultrafiltration and microfiltration membranes with high resistance to contamination by the addition of silver nanoparticles on the application Korea No. 20070071766 "Method for obtaining asymmetric ultrafiltration and microfiltration membranes the introduction of the silver nanoparticles" (publ. in 2007). In accordance with the decision of the prototype of the claimed method includes the preparation of the polymer solution, its mixing with silver nanoparticles with a size of 5-50 nm, followed by DiaryOne received mortar mixture, molding the membrane under General who adopted the technology and its drying. The main disadvantages of the prototype are the following facts: 1. With the introduction of silver nanoparticles prior to forming the membrane portion of silver nanoparticles washed away, reducing their total number in the membrane; 2. IN accordance with the stated sequence of stages of the particles NanoEurope. have an antimicrobial effect, are incorporated into the polymer matrix, resulting in the use of membranes with the filtered medium is in contact only a small fraction of the nanoparticles, which reduces the effectiveness of their actions.

The essence of the invention is as follows.

Technical problem on which the invention is directed is to develop a composition for treatment of polymeric membranes, imparting antibacterial properties, as well as the sequence of stages of polymeric membranes, including the introduction of the specified structure.

The technical result of the invention is to increase the duration of antibacterial properties of the resulting polymer membrane.

The claimed technical result is achieved by preparing a polymer solution, forming a polymer membrane processing the obtained membrane antibacterial substance, drying, cleaning and final drying, with that as antibacterial agents used the following structure (m is SSC):

Sol silver poorly soluble or insoluble 5-10;

Formic acid 2-25;

Water - the rest.

Additional studies conducted by the applicant have shown that the application of the composition containing water, partially soluble or insoluble salts of silver, and formic acid at a given concentration promotes the "growing" silver salts to the polymer matrix of the membrane due to partial swelling of the polymer in the result of its interaction with formic acid and, as a consequence, to enhance the adhesion processes. The claimed sequence of stages capable of handling antibacterial composition after molding of the membrane, allows introduction of silver salts on the surface of the polymer matrix, which certainly improves the antibacterial properties of the resulting membrane. When using the obtained membranes in contact with aqueous environments, these reagents are not practically washed out.

The claimed invention is as follows.

Molded polymer membrane by placing the polymer in the estimated amount of solvent, and then cast to the appropriate slide and immersed in a coagulation bath containing herstorical (precipitator). ("Introduction to membrane technology". M. Mulder, M., Mir, 1999, pp.96-97), and then placed in the pre is satisfactory, the prepared composition, contains (MASC): 2-25 formic acid, 5-10 salt of silver, partially soluble or insoluble in water, the water (the rest) for 5-30 seconds. The thus treated membrane is dried at a temperature of 40-80°C, washed in running water from the remnants of formic acid. followed by a final drying. The result of antibacterial polymer membrane, whose properties are evaluated by the method of filtration of a suspension of the test culture containing 5×103SOME E.coli.

To implement the invention can be used the following substances:

Of silver salts, soluble or insoluble in water (note: in accordance with generally accepted classification of the solubility of salts in water salts are soluble if dissolve 1 g of the indicated salt in 100 g of water, partially soluble, if soluble 0.001 g in 100 g of water, insoluble, if soluble less than 0.001 g per 100 g water): in particular, silver bromide, silver bromate, silver sulfate, silver phosphate.

Formic acid GOST 1706-78.

Water.

Solvents and polymers required for the formation of polymer membranes.

A concrete implementation of the claimed invention is illustrated by the following examples.

Example 1

In accordance with the above method is formed into microfiltration polyamide membrane by dissolving (MASC): polyamide (16)in a mixture of formic acid (72) and water (12), followed by processing precipitator - with a mixture of water (60) and formic acid (40). Microfiltration polyamide membrane is placed for 5 seconds in a solution. consisting of a mixture containing (MASC): 2 formic acid, 5 silver bromate (solubility in water at 20°C is 0.18 g/100 ml), 93 water. Then, the treated membrane is dried at a temperature of 50°C, washed in running water residue from the acid. After the final drying receive antibacterial polymer membrane, which after filtration of the suspension of the test culture containing 5×103SOME E. coli inhibits the growth of bacteria within 10 days.

Example 2

In accordance with the above method is formed into ultrafiltration polyamide membrane by dissolving (MASC): polyamide (18) in a mixture of formic acid (72) and water (10) with subsequent processing precipitator - water (100). Ultrafiltration polyamide membrane was placed for 20 seconds in a solution consisting of a mixture containing (MASC): 10 formic acid, 10 silver sulfate (solubility in water at 20°C 0.79 g/100 ml)80 water. Then, the treated membrane is dried at a temperature of 80°C, washed in running water. After the final drying receive antibacterial polymer membrane, which after filtration of the suspension of the test culture containing 5×103SOME E. coli inhibits the growth of bacteria within 10 days.

Example 3

Rela is availa able scientific C with the above method is formed into microfiltration polyamide membrane by dissolving (MASC): polyamide (16) in a mixture of formic acid (72) and water (12), followed by processing precipitator - with a mixture of water (60) and formic acid (40). Microfiltration polyamide membrane was placed for 15 seconds in a solution. consisting of a mixture containing (MASC): 15 formic acid 7-phosphate silver (poorly soluble in water), 78 water. Then, the treated membrane is dried at a temperature of 60°C, washed in running water. After the final drying receive antibacterial polymer membrane, which after filtration of the suspension of the test culture containing 5×103CFU E. coli inhibits the growth of bacteria within 14 days.

Example 4

In accordance with the above method is formed into ultrafiltration polysulfonamide membrane by dissolving (MASC): polyamide (16) in a mixture of N,N-dimethylacetamide (83,5) and polyvinylpyrrolidone (0,5), followed by processing precipitator dimethylacetamide (83,5) and polyvinylpyrrolidone (0,5), followed by processing precipitator - water (100). Ultrafiltration polysulfonamide the membrane was placed for 30 seconds in a solution consisting of a mixture containing (MASC): 20 formic acid, 8 silver bromide (insoluble in water), 72 water. Then, the treated membrane is dried at a temperature of 40°C, washed in running water. After the final drying receive antibacterial polymer membrane, which after filtration of the suspension of the test culture containing 5×103SOME E. coli inhibits the growth during the 10 days.

Example 5

In accordance with the above method is formed into microfiltration polyethersulfone membrane by dissolving (MASC): polyethersulfone (16) in the mixture in a mixture of N,N-dimethylacetamide (83,5) and polyvinylpyrrolidone (0,5), followed by processing precipitator - a mixture of water (50) and dimethylacetamide acid (500). Microfiltration polyethersulfone the membrane was placed for 10 seconds in a solution consisting of a mixture. contains (MASC): 5 formic acid, 10 silver sulfate (solubility in the will of 0.79 g/100 ml), 85 water. Then, the treated membrane is dried at a temperature of 70°C, washed in running water. After the final drying receive antibacterial polymer membrane, which after filtration of the suspension of the test culture containing 5×103SOME E. coli inhibits the growth of bacteria within 10 days.

Example 6

In accordance. with the above method is formed into microfiltration polyamide membrane by dissolving (MASC): polyamide (16) in a mixture of formic acid (72) and water (12), followed by processing precipitator - a mixture of water (60) and formic acid (40)Microfiltration polyamide membrane was placed for 30 seconds in a solution. consisting of a mixture containing (MASC): 25 formic acid, 10 silver phosphate (poorly soluble in water), 65 water. Then, the treated membrane is dried at a temperature of 70°C, when the Ute in running water. After the final drying receive antibacterial polymer membrane, which after filtration of the suspension of the test culture containing 5×103SOME E. coli inhibits the growth of bacteria within 20 days.

Example 7

To obtain a polyamide nanofiltration membrane ultrafiltration membrane of the aromatic polyamide is placed in an aqueous solution of metaphenylenediamine concentration of 0.5%, allow to drain excess solution, and then placed in a solution mixture (mass): isophthalonitrile and trimethylurea (30) in hexane with a total concentration of 0.5%. stand for 1 min, then washed with water and dried. The obtained polyamide nanofiltration membrane is placed for 30 seconds in a solution consisting of a mixture containing (MASC): 10 formic acid, 8 silver sulfate (solubility in water at 20°C is 0,79 g/100 ml), 82 water. Then, the treated membrane is dried at a temperature of 90°C, washed in running water. After the final drying receive antibacterial polymer membrane, which after filtration of the suspension of the test culture containing 5×103SOME E. coli inhibits the growth of bacteria within 10 days.

Example 8

In accordance with the above method is formed into cellulose acetate reverse osmosis membrane by dissolving (MASC): cellulose acetate (15) in a mixture of acetic acid (10),Cetona (10) and water (5) with the subsequent processing precipitator - with a mixture of water (95) and acetic acid (5). Reverse osmosis cellulose acetate membrane is placed for 10 seconds in a solution consisting of a mixture containing (MASC): 10 formic acid, 10 silver bromide (insoluble in water), 80 water. Then, the treated membrane is dried at a temperature of 95°C, washed in running water. After the final drying receive antibacterial polymer membrane, which after filtration of the suspension of the Test culture containing 5×103SOME E. coli inhibits the growth within 14 days.

Example 9 (comparative in accordance with the prototype)

In accordance with the decision of the prototype received a polymeric microfiltration membrane by solution-based polyethersulfone and subsequent) about the introduction of silver nanoparticles size of 8 nm in an amount of 0.2% of the mass. in relation to polyethersulfone. After drying receive antibacterial polymer membrane after filtration of the suspension of the test culture containing 5×103SOME E. coli, it inhibits the growth of bacteria within 6 days.

Bibliographic data

1. Silver nanoparticles as antimicrobial agents, publ. in "Colloid and Interface Science" in 2004(275, 177-182).

2. Polysulfone ultrafiltration membranes impregnated with silver nanoparticles for removal of viruses with high resistance to biofouling, publ. in "Wate Research/Journal of the International Water Association" in 2009 (No. 43 SS-723).

3. Silver with delivery into the cell (publ. on the website of the company ARGO argonet.ru).

4. Application for U.S. patent No. 20110024355 (publ. 2011).

5. Patent application Korea No. 20070071766 (publ. 2007).

The method of obtaining the antibacterial polymer membrane comprising preparing a polymer solution, the processing of antibacterial substance, molding the polymer membrane and drying, characterized in that the processing of the membrane antibacterial substance is carried out after the forming of the membrane, followed by additional drying, water rinse, and final drying, the antibacterial agents used the following composition, parts by weight:

Sol silver, partially soluble or insoluble5-10
Formic acid2-25
Water65-93



 

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