Method for antiseptic treatment of fibrous materials

FIELD: textile industry.

SUBSTANCE: invention relates to technology of treating genuine and synthetic fibrous materials to protect their surface against growth of microorganisms and can find use in manufacture of decorative and finishing or structural materials for spatial objects, in different forms in submarines, in surface or underground tightly sealed rooms, and in precision objects (e.g. electronics) assembly shops. Method comprises radiation graft polymerization of vinyl carboxylic acid from vapors thereof upon irradiation of the yarn with γ-emission source (60Co), neutralization of carboxylic groups of grafted poly(vinyl carboxylic acid) through soaking in aqueous solution of sodium or potassium hydroxide, carbonate, or bicarbonate, and immobilization of alkyl(benzyl)dimethylammonium cation as counter ion.

EFFECT: provided prolonged protection of fibrous materials against attacks of microorganisms.

5 tbl, 15 ex

 

The present invention relates to the processing of natural and synthetic fibrous materials that can protect these materials from microbial growth on their surface.

Most effectively the invention can be used in objects, which imposed requirements on the level of microbial load.

The relevance of the developed method is to use products made of cotton and arimidex fibers in the presence of people in the areas shops, where regulated microbial load, and hermozamente premises, which do not permit the growth of microorganisms on the surface of the material even in conditions of high humidity.

Currently known (Patent Poland No. 96626, CL 08 F 251/02, publ. 1978) method antiseptic treatment of textile materials containing cellulose fibers, consisting in the application of an aqueous solution of acrylate metals with antimicrobial properties.

The disadvantages of this method are the use of compounds of heavy metals, which are not desirable for subsequent use in the presence of the people, and low antimicrobial efficiency of use of compounds of this type, due to their low solubility in water during processing of the material.

Also known (U, patent No. 2114229, class D 06 M 13/463, publ. 1998) method antiseptic treatment of textile material with biocide - alkylbenzyldimethylammonium (Catalina AB).

The disadvantage of this method is to protect only hosiery and underwear products from exposure to microorganisms that cause specific fungal infections of the feet and groin area, as well as the need for preliminary dyeing fibers direct dyes, which changes the appearance of the product.

The closest in technical essence and the achieved result of the present invention is a method (RU, patent No. 2037592, class D 06 M 13/328, publ. 1995) antiseptic treatment of textile material inoculation vinylcarbazole acid with the subsequent introduction of a cation having biocidal properties, and additional treatment with aqueous solutions of triethanolamine, its hydrochloric acid salt or Tris-(2-hydroxyethyl)methylaminomethyluridine.

However, this method of finishing cellulose-containing textile material has biocidal properties only with a high degree of grafting (6-8 wt.% for acrylic acid). The need to achieve such a high degree of grafting increases the rigidity of the fiber to change its appearance. The disadvantage of this method is also a waste of vinylcarbazole to the slots in the formation of its homopolymer, which is washed out during subsequent processing of the fiber.

The technical result of the present work is prolonged protection of fibrous materials from exposure to microorganisms by graft-polymerization vinylcarbazole acid followed by treatment with an antiseptic substance.

This technical result is achieved by the proposed method, antiseptic processing of cotton and arimidex fiber, which consists in radiation grafting polymerization vinylcarbazole acid from its vapours in the process of irradiation fiber source γ-radiation60With neutralizing the carboxyl groups grafted polyvinylcarbazole acid by soaking in an aqueous solution of a hydroxide, carbonate or bicarbonate of sodium or potassium and immobilization as counterion alkylbenzyldimethylammonium cation.

Grafting polymerization vinylcarbazole acids on cotton and Ariminum the fiber is carried out under irradiation in pairs corresponding monomer when bubbling through nitrogen at room temperature. The degree of grafting polyvinylcarbazole acids regulate both the dose and the concentration of the vapor of the monomer, which depends on the speed of bubbling nitrogen through the liquid monomer. The degree of grafting calculated by the formula:

where Δp is the degree of grafting, %; m1and m0the mass of the sample after and before vaccination, Dose change from 16 to 40 kGy, which provides a degree of grafting of from 1.5 to 2.7%. At lower degrees of grafting is not achieved complete inhibition of growth of microorganisms. Higher degree vaccinations lead to a deterioration of physical and mechanical properties of the fiber and to change its appearance.

Translation grafted polyvinylcarbazole acid from the acid in the salt form is performed by soaking the fiber in an aqueous solution of a hydroxide, carbonate or potassium bicarbonate or sodium by rinsing in distilled (deionized) water. The cation exchange metal alkylbenzyldimethylammonium cation is performed by soaking the fibers in aqueous or aqueous-alcoholic solution of alkylbenzyldimethylammonium (catamine AB) followed by rinsing in distilled (deionized) water. Solutions catamine AB different concentrations prepared from its 50% aqueous solution.

When testing the antimicrobial activity of the fibers subjected to graft polymerization vinylcarbazole acids, determine the duration and degree of protection materials in conditions periodically generated high microbial load.

Evaluation of antimicrobial activity of the samples is carried out by determining gribomont in points according to GOST 9802-84 and against bacterial and fungal Association, consisting of Staphylococcus epidermidis, Bacillus polymyxa, Bacillus pumilus, Penicillium chrysogenum, Aspergillus niger and Cladosporium cladosporioides, which monthly inoculant 5 samples of materials to each experience to obtain reliable data. The content of each species in the mixture is 1×105-2×105colony forming units (CFU) on 1 cm2square. Then your sample is placed in a thermostat and incubated at 28°C, relative humidity ≥90% within 3 months sampling in 14 days to determine the number of viable units of microorganisms on the studied materials. For this purpose, the samples otbelivaut in physiological solution and washings are sown on the surface of nutrient media: protection of čapek-doksa to determine CFU of fungi, environment mastopathy agar to determine CFU of bacteria.

The following examples illustrate the proposed method of processing cotton and arimidex fiber.

Example 1

Spend grafting polymerization of acrylic acid on cotton fiber in the form of surgical tape (GOST 4514-78) at the dose of 16 kGy, achieving this degree of grafting of polyacrylic acid of 1.5%. Next to the translation of the grafted polyacrylic acid in the salt form the fiber for 30 min soak in a 1 N solution of potassium hydroxide, rinsed with distilled water and glaubman of counterion on alkylbenzyldimethylammonium cation fiber for 30 min soaked 6.7% solution of catamine AB in isopropanol, followed by rinsing in distilled water.

For the evaluation of antimicrobial activity of the samples repeatedly infect bacteria and fungi. Table 1 presents the content of SOME bacteria and fungi these samples and samples of the prototype.

Making last conducted under the following conditions. Dose of 15 kGy, the degree of grafting poly (acrylic acid) - 8%. Next, the sample is treated for 20 min in a 7.5% solution of triethanolamine and for 20 min in a 10% solution of catamine AB.

As a control using native samples of surgical tape.

After 14 days of incubation in thermostat all infected samples carry out sampling for the determination of viable units of microorganisms in these samples according to methods described above. The average number of bacteria and fungi in this experiment are shown in table 1.

Table 1.
The content of colony-forming units of bacteria and fungi in the samples of example 1 and the samples of the prototype.
Example1-fold infection2-fold infection3x infection
No.bacteriamushroomsbacteriamushroomsbacteria mushrooms
13×1012×1013×1036×104--
The placeholder6×1035×103----
Control2×1054×106----

As can be seen from this table, the number of microorganisms in a single contamination on the samples of the prototype was significantly lower than in control samples (a difference of two orders of magnitude), and the samples of example 1 was significantly lower than in the samples of the prototype. After re-infection samples according to method 1, the number of bacteria and fungi on them increases significantly.

Therefore, for sample preparation method 1 is not achieved complete kill of microorganisms.

Funginertness samples according to GOST 9.082-84 matches in example 1 is equal to 0 points, the prototype is 3 points, and control is equal to 5 points.

Examples 2-10

Surgical tape modify analogously to example 1, achieving different degrees of grafting of polyacrylic acid change doses. The terms of the modification are given in table 2.

Table 2.
Conditions modification surgical tape when grafting polymerization of acrylic acid in examples 2-10.
ExampleDose

GSR
ΔR %The alkali solution(1The solution catamine AB(2
No.close-tion, Ntime minsolventtime min
2140,71,015isopropanol30
3181,70,230water60
4202,20,230the same60
5202,20,290-"-30
6202,20,230water/isopropanol (1/1 by volume)15
7202,20,230water/ethanol (1/1 by volume)60
8202,20,2 30water/ethanol (1/8 by volume)60
9252,31,012isopropanol30
10402,70,160water60
1 - samples 2 and 9 is treated with a solution of potassium hydroxide, and samples 3-8 and 10 treated with solutions of sodium hydroxide.
2 - concentration of the solution catamine AB when processing samples 2 and 9 6.7%, while processing samples 3-8-10%, while processing a sample 10-5%.

The results of the evaluation of antimicrobial activity of the samples is given in table 3. From the data presented in the table shows that the number of bacteria and fungi is observed only in 2 samples. Samples 3-10 completely suppressed microorganisms in single, double and triple infection samples.

Funginertness GOST 9.802-84 samples according to example 2 is equivalent to 4 points, and the remaining samples the growth of fungi is missing - 0 points.

Table 3.
The content of colony-forming units of bacteria and fungi in the samples of surgical tape and subjected to surface modification./td>
Example1-fold infection2-fold infection3x infection
No.bacteriamushroomsbacteriamushroomsbacteriamushrooms
24×1037×103----
3000000
4000000
5000000
6000000
7000000
8000000
9000000
1000000 0
Note: 0 is not found.

Example 11

Spend grafting polymerization of acrylic acid on cotton fiber in the form of gauze (GOST 9412-93) at the dose of 20 kGy, achieving this degree of grafting of polyacrylic acid of 2.2%. Next to the translation of the grafted polyacrylic acid in the salt form the fiber for 30 min soaked in 5% sodium hydrogen carbonate solution, rinsed with deionized water and for the exchange of the counterion on alkylbenzyldimethylammonium cation fiber for 15 min soak in a 10% solution of catamine AB in a mixture of water/isopropanol (1/8 by volume), followed by rinsing in deionized water.

On the thus modified fiber growth of fungi according to GOST 9.802-84 missing and not found SOME bacteria and fungi with 3-fold transmission.

Example 12

Spend grafting polymerization of methacrylic acid on cotton fiber in the form of surgical tape in the same conditions as grafting polymerization of acrylic acid. At the dose of 30 kGy degree of grafting of poly (methacrylic acid is 2.4%. Subsequent processing of the sample is similar to the processing of the sample in example 4.

The growth of fungi according to GOST 9.802-84 missing and at 3 times the contamination of the modified fiber suspension m is croorganisms SOME bacteria and fungi were not found.

Examples 13-15

Spend grafting polymerization of acrylic acid on arimitsu fabric in the form of a tape technical (TU 154-82) in the same conditions as in grafting polymerization of acrylic acid, by changing the irradiation dose (table 4). Next to the translation of the grafted polyacrylic acid in the salt form fiber for 15 min soaked in 5% sodium carbonate solution, rinsed with deionized water and for the exchange of the counterion on alkylbenzyldimethylammonium cation fiber for 15 min soak in a 6.7% aqueous solution of catamine AB with rinsing with deionised water.

Table 4.
Conditions modification arimidex fiber during grafting polymerization of acrylic acid.
Example No.Dose, kGyΔR %
13201,7
14262,3
15402,7

The results of the evaluation of antimicrobial activity of the samples is given in table 5.

Table 5.
The content of colony-forming units of bacteria and fungi in the samples arimi the aqueous fiber, subjected to surface modification.
Sample1-fold infection2-fold infection3x infection
No.Bacteriamushroomsbacteriamushroomsbacteriamushrooms
13000000
14000000
15000000
Note: 0 is not found.

From the data of this table shows that for all samples subjected to surface modification, there was complete inhibition of microorganisms.

Funginertness samples No. 13, 14 and 15 according to GOST 9.802-84 0 points.

Therefore, only when the degree of grafting of polyacrylic acid from 0.7 to 1.5% (examples 2 and 1, respectively) is not achieved complete inhibition of growth of microorganisms. But even when the degree of grafting of 1.5% (example 1) the growth of microorganisms is lower than in the sample prototype, which is not achieved complete inhibition of growth of microorganisms.

Thus, min is supplemented flax degree of grafting of polyacrylic acid, which guarantees prolonged suppression of microbial growth on the surface of the fibrous materials, is 1.5%.

The proposed method antiseptic processing of cotton and arimidex fibers may be applied when using them:

as a decorative or structural materials of space objects;

- different as in submarines;

- ground or underground hermetically closed space;

in assembling accurate products, such as electronics.

Method antiseptic treatment of fibrous materials by grafting polymerization vinylcarbazole acid followed by treatment with an antiseptic substance, characterized in that the grafting polymerization vinylcarbazole acid is carried out with simultaneous irradiation vapor vinylcarbazole acid and fibrous materials source γ-radiation60With up to absorbed doses 16-40 GSR and degrees vaccinations polyvinylcarbazole acid 1.5 to 2.7%, and then treated with an aqueous solution of a hydroxide, carbonate or bicarbonate of sodium or potassium and water or a water-alcohol solution of alkylbenzyldimethylammonium.



 

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