RU2366771C1 - Method of enzyme peroxide preparation of highly lignified flaxen roving for spinning - Google Patents

Abstract

FIELD: textile, paper. ^ SUBSTANCE: invention concerns method of flaxen roving preparation for spinning and can be applied in textile industry. Method of enzyme and peroxide preparation of highly lignified flaxen roving for spinning involves deacidification, enzyme processing at 40-50C for 90-95 minutes by polyenzyme preparation solution with enzyme activity indicators, units per ml: endopolygalacturonase - 20-25; pectinesterase - 2.5-4.7; protease - 0.2-0.3; exopolygalacturonase - 0.6-0.1; exogalactosidase - 0.2-0.4; exoxylosidase - 0.3-0.5; and exoglucanase - 0.6-0.8. Further the roving is heated to the boiling point and matured for 20-25 minutes, flushed by water and processed for 90-95 minutes in alkaline peroxide solution at hydro peroxide concentration of 0.6-0.8 g/l of active oxygen and total alkalinity of 6.5-7.0 g/l rated per caustic soda. Then the roving is flushed with detergent and water and undergoes counter-microbe processing. ^ EFFECT: fiber whitening degree enhanced up to 54-56%; obtainment of thin yarn meeting the requirements for both "1 high-flaxen" and "1 high tow" grades by GOST 10078-85 in line density and line density and tear load variation rates; reduced yarn tear rate in weaving process to 40-50 tears for 100 spindles per hour; enhanced yarn strength in 1,2-1,4 times; improved esthetics of woven canvas exterior. ^ 1 tbl, 3 ex

Description

The invention relates to the textile industry, and in particular to a technology for preparing flax rovings for spinning.

State of the art

One of the drawbacks of domestic flax raw materials is the high degree of lignin binder in the structure of the bast bundles, due to the high content of lignin - one of the cellulose satellites, which gives the fiber rigidity (coarseness), specific brown color and prevents the fragmentation of the bundles by thickness to obtain high yarn (fineness) ) The lignin content in the medium soft fiber is 5.5-7 wt.% Versus 2.5-4 wt.% In soft varieties of bast-fiber raw materials, and in tows used for the production of filament yarn - 8-12 wt.%.

Traditional methods of chemical preparation of flax rovings for spinning are based on the hydrolytic destruction of polymeric cellulose satellites during multistage and prolonged exposure of flax fiber to low-concentrated solutions of acids, alkalis and oxidizing agents [Regulated technological processes of processing rovings, yarn, fabrics / M .: FSUE TSNIILKA, 1982, 104, 104, from.]. The permissible amount of impurities removed in this case, controlled by the indicator of fiber mass loss, should not exceed 20%. In this case, the effective destruction of lignin is ensured only when using chlorine-containing oxidizing agents, in particular sodium chlorite, followed by neutralization, alkaline cooking, and treatment with acetic acid and acetone solutions with intermediate washes [Ivanov AN Physico-chemical principles of the technology of cooking flax // Diss. ... Doct. tech. sciences. - Kostroma, 1989. - 535 p.].

However, the use of chlorine-containing oxidizing agents does not meet modern environmental safety requirements for production processes and products.

A known method of preparing flax rovings for spinning by selective destruction of polymeric cellulose satellites under the action of enzyme preparations instead of alkaline cooking followed by oxidative treatment in a solution of hydrogen peroxide [Ossola M., Galante Y.M. Scouring of flax rove with aid of enzymes / Enzyme and Microbial Technology, 2004, V.34. - P.177-186]. The method includes the following steps:

- enzymatic treatment with a solution of the enzyme preparation at 55 ° C for 30 min in the presence of 1 g / l of surfactant and 2 g / l of complex-forming preparation with a bath modulus of 1:10;

- washing at 80 ° C;

- bleaching in a solution containing 5.5 g / l NaOH 36Вè, 5 ml of 11.61 M H ₂ O ₂ per 1 kg of roving and 0.6 g / l of peroxide stabilizer, when heated from 40 to 95 ° C for 45 min and holding at 95 ° C for 45 min;

- triple washing;

- anti-mold treatment with acetic acid solution.

For enzymatic treatment, one of the following enzyme preparations is used, indicating the manufacturer and the level of activity of the enzyme present:

- Pulpzyme (Novozymes) - xylanase 2.3 units / ml;

- experimental product (Novozymes) - galactomannanase 1.24 units / ml;

- Bioprep 3000L (Novozymes) pectinase (endopolygalacturonase) 16.8 units / ml;

- NS 45003 (Novozymes) - lipase 0.038 units / ml;

- Purafect 40001 (Genencor) - a protease of 5.4 units / ml;

- DeniLeit ^tm Base + DeniLeit ^tm Assist (Novozymes) - laccase + mediator (2: 1) 1.6 units / ml.

All variants of this enzymatic-peroxide method for preparing flax rovings provide an increase in the strength of the resulting yarn and a decrease in the unevenness coefficient. However, an increase in the number (fineness) of yarn is observed only when exposed to pectinase. According to the presented series of decreasing the effectiveness of enzyme preparations for the total set of controlled yarn parameters: pectinase> protease = xylanase = galactomannanase> lipase ≥ laccase, the best result is the cleavage of pectin impurities with the bioprep 3000 L enzyme preparation based on pectinases, and the smallest - lignin degradation by action laccase, belonging to the class of oxidoreductase enzymes.

To accelerate the process of delignification of flax fiber when receiving medical cotton wool, methods for preparing fibrous material using compositions of pectolytic enzymes with lipases are known [RU 2157434 C1, D21F 11/14, D04H 1/02, C12S 3/04, 3/06, 2000] or cellulases [Nadtoka IB Creation of cotton-like hygroscopic materials based on flaxseed waste // Diss. ... cand. tech. sciences. - Ivanovo, 2000. - 166 p.]. However, in this case, the requirements for whiteness and hydroscopicity are imposed on the fibrous material and it is not required to maintain a certain level of bonding of elementary fibers, which is necessary for processing the fiber into yarn.

When preparing flax rovings from domestic varieties of medium-soft flax fiber, the ineffective effect of pectinase enzyme preparations is also recommended to be strengthened by the addition of domestic or imported cellulase enzyme preparations [Cheshkova A.V. and others. New in the technology of preparation of linen rovings / Izv. universities. Technology text. Industry, 2000, No. 6. - S. 45-49]. Cellulase enzyme (endoglucanase, classification number K.F. 3.2.1.4), as well as pectinase (endopolygalacturonase K.F. 3.2.1.15), belong to the same group of enzymes - glycosidases, catalyzing the hydrolysis of glucosidic bonds in O-glycosyl compounds (respectively, in cellulose and pectin). An increase in the degree of lignin removal by 5-8% with the addition of cellulases in comparison with treatment with pectinases alone, according to the authors, is due to a violation of the connection of the lignin component with cellulose.

This variant of enzyme treatment implements, in particular, the well-known method of enzymatic-peroxide preparation for spinning rovings of medium soft flax fiber or coarse hair fiber using Viscozyme L and Cellusim preparations mixed in solution (F. Novozymes, Denmark), which are characterized by standard enzyme activity indicators respectively pectinase 1200 units / g and cellulase 150 units / g [Cheshkova A.V. Enzymatic modification of natural fiber-forming polymers at various stages of preparation of textile materials // Thesis ... Doct. tech. sciences. - Ivanovo, 2005. - 338 p.]. The method includes the following steps:

1 - enzymatic treatment of flax rovings at a temperature of 50-55 ° C, pH 5.0-7.5 and a bath modulus of 1:50 for 10-180 min with a solution of a mixture of viscose L and Cellulose at a concentration of 0.5 g / l each, which provides the level of enzyme activity in solution, units / l:

- pectinase (endopoligalacturonase) - 600;

- cellulase (endoglucanase) - 75;

2 - washing with hot water 86 ° C for 5 min;

3 - treatment (bleaching) with an alkaline peroxide solution containing, g / l: hydrogen peroxide - 1.4-1.7 (in terms of active oxygen); sodium silicate - 8-12; soda ash - 14; syntanol BV - 0.2; Trilon B - 0.2 and magnesium sulfate - 0.1; with heating to 98 ° C and a total stage duration of 60-90 minutes;

4 - three times washing with hot water;

5 - re-treatment with an alkaline peroxide solution with concentration, temperature and time parameters similar to those indicated in stage 3;

6 - washing with a solution of tripolyphosphate of 0.4 g / l at 80 ° C for 20 minutes and then twice with hot water at 70 and 65 ° C for 10 minutes;

7 - antimicrobial treatment with acetic acid 0.9 g / l at 55 ° C for 15 minutes

The weight loss of the fiber during the preparation of the roving by this method is 9.5-18.1%, the degree of lignin removal is 44.5-48.1%, the brightness of the roving from the filament fiber is 47.4-57.9%, and technical fiber - 73.6-77.1%.

However, this method has several significant disadvantages. It takes a long (double) treatment with an alkaline peroxide solution with a high concentration of hydrogen peroxide and a stabilizer of peroxide - sodium silicate, as well as increased alkalinity of the solution. Rigid conditions for bleaching rovings in combination with the previous exposure to cellulases cause significant damage to the main fiber-forming polymer, as evidenced by a decrease in the specific viscosity of copper-ammonium cellulose solutions by 1.4-1.9 times. The removal of technologically necessary hemicelluloses is too large - 59-78%, and the technically feasible destruction of pectin substances does not exceed 40-55%. Damage to the cell wall of elementary fibers by cellulases leads to the destruction of amorphous structures of lignin with hemicelluloses, which reduces the technological properties of the fibrous material. Similar results of preparation are considered unfavorable [Ivanov A.I. et al. Study of the chemical composition of flax fibers of various breeding varieties // Izv. universities. Technology text. Industry, 1986, No. 1. - S.19-21].

The closest to the claimed invention in essence and the technical result achieved is a method of enzymatic-peroxide preparation of rovings from domestic flax fiber of medium softness using at the stage of enzymatic processing a polyenzyme preparation in the form of Pectofoetidin P10x and microscopic fungi oxidase reductases of the genus Coriolus C of the Polyporace family .BUT. Development of energy-saving environmentally friendly technologies for the preparation of flax materials based on bioprocesses // Diss ... Cand. tech. sciences. - Ivanovo, 1999. - S.114-119]. Pectofoetidine P10x is an industrially produced preparation (TU 64-13-04-87) and is a complex of enzymes of the microscopic fungus Aspergillus foetidus M45. Along with pectinase (endopolygalacturonase, activity of 1500 units / g) and cellulase (endoglucanase, 19 units / g), it contains pectin esterase 80 units / g, acid protease (10 units / g). Exogenous polygalacturonases and xylanases are also present in trace amounts in the preparation, but taking into account dilution in the technological solution, their content is negligible. The experimental preparation of oxidoreductases contains peroxidase (activity for benzidine 0.82-3.5 units / g), laccase (activity for benzidine 0.7-3.8 units / g) and polyphenol oxidase (activity 1.8-2.5 units / g). The method includes the following steps:

1 - enzymatic treatment at 40-45 ° C and a pH of 6.5-7.5 for 60 min with a solution comprising the preparation Pectofoetidin P10x 0.9-3 g / l and the preparation of oxidoreductases 0.75-3 g / l, which provides the level of enzyme activity, units / l:

- endopoligalacturonase (pectinase) - 1125-4500;

- endoglucanase (cellulase) - 17.1-57;

- pectin esterase - 60-240;

- protease - 7.5-30;

- peroxidase - 2.5-2.6;

- laccase - 2.1-2.9;

- polyphenol oxidase - 1.9-5.4;

2 - washing with hot water 86 ° C for 5 min;

3 - treatment with an alkaline peroxide solution containing the following reagents, g / l: hydrogen peroxide - 1.7 g / l (in terms of active oxygen), sodium metasilicate - 8-12; soda ash to a total alkalinity of 8.5 (in terms of caustic soda); syntanol BV - 0.2; Trilon B - 0.2; magnesium sulfate - 0.1; with heating to 98 ° C and a total process duration of 60 minutes;

4 - washing with a solution of tripolyphosphate of 0.4 g / l at 80 ° C for 20 minutes and then twice with hot water at 70 ° C and 65 ° C for 10 minutes;

5 - antimicrobial treatment with acetic acid 0.9 g / l at 55 ° C for 15 minutes

The method allows to exclude the repeated processing of rovings with an alkaline peroxide solution, the decrease in the content of acid-insoluble lignin reaches 60% with a total fiber weight loss of 8.3%.

The main disadvantages of this method include the impossibility of its industrial implementation due to the lack of industrial production both in Russia and abroad of the necessary compositions of oxidoreductases, which differ in their complex composition and require the inclusion of special substances - redox mediators that are involved in the destruction of high molecular weight lignin structures for subsequent oxidation of the products of depolymerization with polyphenol oxidases, peroxidase or laccase (Golovleva L.A., Ganbarov Kh.G. Microbial degradation of leagues Nina // USSR Academy of Sciences. Advances in Microbiology, 1982, T.17. - P.137-158; Gracheva IM, Krivova A.Yu. Technology of enzyme preparations / 3rd ed., revised and additional - M .: Elevar. 2000. - 512 p.].

In addition, this method has a number of technical disadvantages:

- a low degree of whiteness of the fiber, amounting to only 22.8%, due to the high residual lignin content in the fiber at the level of 3.0 wt.% for medium soft rovings and 3.4-4.8 wt.% for coarse fiber and flax roving ;

- the inability to obtain thin yarn that simultaneously satisfies the requirements of the 1st grade according to GOST 10078-85 in terms of both linear density (T) and coefficient of variation in linear density (C _T ) and breaking load (C _P ). So, for yarn with a linear density of 56 Tex, the uniformity characteristics of yarn С _Т and С _Р normalized by the standard should be no more than 3.5% and 20%, respectively. For the prototype, in the actual production of yarn with T = 56.6 Tex, the values of the coefficient of variation are С _Т = 5.4% and С _Р = 21.5%, which corresponds to grade “1 srednyanny”. The disadvantage is due to the low degree of removal of pectins, which are the adhesive base of binders in flax complexes, not exceeding 50%, and the insufficient preparation of the fibrous material for crushing, as evidenced by the decrease in the breaking load of the rovings in the wet state relative to the level for the untreated roving by no more than 43 %;

- increased yarn breakage in weaving processes - 80 breaks per 100 spindles per hour, which is due to a number of factors associated with excessive removal of hemicellulose compounds (up to 62-65%), including:

- a low level of strength of the yarn obtained (breaking load of 1147 cN, specific breaking load of 20.3 cN / Tex, the work of the gap of 40.4 kgf · cm / g, the coefficient of variation in the work of the gap of 7.9%);

- insufficient deformation and elastic properties of the yarn (actual twist of 512-524 torsions per 1 m, coefficient of variation in twist of 9.4%; the proportion of slowly reversible relaxation in the total elongation during single-cycle testing of the yarn does not exceed 18%);

- low endurance of the yarn to repeated bending and abrasion (5380-5450 cycles);

- insufficient aesthetics of the appearance of the formed woven fabrics due to the presence in the yarn of a large number of defects in the form of thickenings exceeding 1.5 times the average diameter of the yarn, Y _1.5 = 3570 pcs / km and thinning with a diameter of less than 0.7 the average diameter of _0.7 = 3960 pcs./km.

Thus, the known methods of preparation for spinning flax rovings using enzyme preparations do not provide effective destruction of lignin and pectin impurities in the intercellular formations of binders of complex fibers of highly lignified types of flax raw materials. Removal of lignin does not exceed 45-60%, and pectin impurities - 40-55%. This does not allow to achieve an effective increase in the spinning ability of the fibrous material, the uniformity of its crushing on the spinning equipment to obtain high-quality yarn with the necessary level and high stability of its geometric dimensions, strength and deformation indicators. Low strength, elasticity and wear resistance of the yarn determine the high breakage of the semi-finished product in the processes of winding and weaving, and the presence of a large number of defects in the structure of the yarn in the form of thickenings and thinning reduces the aesthetic properties of woven fabrics.

SUMMARY OF THE INVENTION

The inventive task was to find a method of enzymatic-peroxide preparation for spinning a highly lignified flax rove, including enzymatic treatment with a multi-enzyme preparation solution, including endopoligalacturonase, pectin esterase, protease and exopoligalacturonase, rinsing with water, alkaline-and-peroxide washing with rinse and water treatment which would allow the processing of domestic bast-fiber raw materials of increased stiffness to increase the degree of whiteness in it is local, to obtain fine yarn that meets the requirements of the 1st grade according to GOST 10078-85 simultaneously in terms of both linear density and variation coefficients in linear density and breaking load, to reduce the breakage of the yarn in weaving processes by increasing its strength, deformation and elastic properties and endurance to repeated bending and abrasion, to improve the aesthetics of the appearance of the formed woven fabrics by reducing the number of defects in the structure of the yarn in the form of thickenings and thinning.

The problem is solved in that in the method of enzymatic-peroxide preparation for spinning highly lignified flax rovings, comprising enzymatic treatment with a solution of a multienzyme preparation, including endopoligalacturonase, pectin esterase, protease and exopoligalacturonase, rinsing with water, rinsing with alkaline and peroxide water treatment, before enzymatic treatment with a polyenzyme preparation, the roving is deoxidized, as a polyenzyme preparation, . Comfort solution further comprising ekzogalaktozidazu, ekzoksilozidazu ekzoglyukanazu and with measures of enzyme activity U / ml:

- endopolygalacturonase - 20-25;

- pectin esterase - 2.5-4.7;

- protease - 0.2-0.3;

- exopoligalacturonase - 0.6-1.0;

- exogalactosidase - 0.2-0.4;

- exoxylosidase - 0.3-0.5;

- exoglucanase - 0.6-0.8;

enzyme treatment is carried out at a temperature of 40-50 ° C for 90-95 minutes, followed by heating to a boil and holding for 20-25 minutes, and treatment with an alkaline-peroxide solution is carried out at a concentration of hydrogen peroxide of 0.6-0.8 g / l (active oxygen) and total alkalinity of 6.5-7.0 g / l (in terms of sodium hydroxide) for 90-95 minutes

The invention allows to obtain the following advantages:

to increase the degree of whiteness of the fiber to 54-56% by reducing the residual lignin content in the medium soft fiber to 1.9 wt.%, in the coarse fiber to 2.15 wt.% and up to 3.05 wt.% in the hairy roving at the total decrease in fiber mass in the preparation process is 11-14%, i.e. within the limits of technologically permissible values - not more than 20%;

- to obtain fine yarn that meets the requirements of grades “1 high yielded” and “1 high yielded” according to GOST 10078-85 simultaneously in terms of both linear density (T) and coefficient of variation in linear density (С _T ) and breaking load (С _P ) . So, for yarn with a nominal linear density of 56 Tex, the characteristics of uniformity of yarn С _T and С _P do not exceed 2.2–2.6% and 12.4%, respectively. This is due to an increase in the degree of removal of pectins to 80-85% against 45% in the prototype and an increase to 65-70% of the reduction in the breaking load of the rovings in the wet state relative to the level of the indicator for untreated rovings, which is the criterion for the preparation of fibrous material for crushing, against 43% for the prototype ;

- to reduce the breakage of yarn in the weaving process to 40-50 breaks per 100 spindles per hour, which is associated with a decrease in the removal of hemicellulose compounds to 30-35% against 65% of the prototype. This preservation of hemicellulose compounds allowed to increase the breaking load of the yarn to 1327 cN (1147 cN according to the prototype), the specific breaking load to 25.0 cN / Tex (20.3 cN / Tex according to the prototype), the work break to 42.6-43.7 kgf · cm / g (40.4 kgf · cm / g according to the prototype) and a twist to 550-562 cr./m (524 cr./m according to the prototype) while reducing the variation coefficients for the gap to 5.1-5 , 9% (7.9% of the prototype) and twist to 7.2-7.9% (9.4% of the prototype). The share of slowly reversible relaxation in the total elongation during single-cycle testing of the yarn increased to 23-25% (18% of the prototype), and the endurance of the yarn to repeated bending and abrasion increased to 6745-6897 cycles (versus 5432 cycles of the prototype);

- to improve the aesthetics of the appearance of the formed woven fabrics by reducing the number of yarn defects in the form of thickenings exceeding 1.5 times the average diameter of the yarn to 1920 pcs / km (versus 3570 pcs / km for the prototype) and thinning with a diameter less than 0.7 average diameter up to 970-1171 pcs./km (3960 pcs./km for the prototype).

Information confirming the possibility of carrying out the invention

According to the claimed method, it is possible to process the rovings of stanchian or urinary technical fibers of coarse or medium softness from domestic varieties of flax raw materials, as well as from coarse fiber.

To implement the method using the following reagents.

- As a multienzyme preparation, cultivation products of microbiological producers can be used that provide simultaneous biosynthesis of a complex of technologically necessary enzymes:

- endopoligalacturonase (has a different trivial name for pectinase, as well as the classification number KF 3.2.1.15 and the scientific name poly [1,4-α-D-galacturonide] glycanohydrolase established by the current International Classification of Enzymes 1961),

- pectin esterase (EC 3.1.1.11, pectin pectyl hydrolase),

- proteases of two varieties of serine proteinases (subclass KF 3.4.21) and / or metalloproteinases (subclass KF 3.4.24);

- exopoligalacturonase (EC 3.2.1.67 poly [1,4-α-D-galacturonide] galacturonhydrolase) and / or exopolygalacturonosidase (EC 3.2.1.82 poly [1,4-α-D-galactosiduronate] digalacturonhydrolase);

- exogalactosidase (K.F. 3.2.1.23, β-D-galactoside-galactohydrolase);

- exoxylosidase (K.F. 3.2.1.37, 1,4-β-D-xylan-xylhydrolase and / or K.F. 3.2.1.72, 7,3-β-xylan-xylhydrolase);

- exoglucanase (EC 3.2.1.74, exo-1,4-β-glucosidase).

A multienzyme preparation can be obtained, for example, by mixing cultivation products of non-pathogenic bacterial strains from the Museum of the State Research Institute of Genetics, registered under the numbers of the All-Russian Collection of Industrial Microorganisms (VKPM) V. circulans VKPM B-1741, B. subtilis VKPM B-1093, Erw. carotovora VKPM B-1358, you. mesentericus VKPM B-1559 or B-2466. You can use the composition of the products of cultivation of fungal producers Penicillium lanosum F-387, Asp. awamori 22 and Asp. flavus VKPM F-591.

Measurement of the number of enzymes with an expression in conventional weight or volume units is difficult, since enzymes are substances of protein nature, and it is impossible to determine their amount in a mixture with other proteins. In addition, the catalytic properties of enzymes are unstable and can vary significantly depending on the temperature, acid-base properties of the medium or completely lost under adverse conditions of storage and use of drugs. In accordance with the recommendations of the Commission on Enzymes of the International Biochemical Union, a quantitative assessment of the content of a particular enzyme in a preparation is expressed in units of activity according to the results of the reaction that it catalyzes, that is, by the amount of the reaction product formed or a decrease in the initial substrate. A unit of activity for any enzyme is understood to be such an amount that catalyzes the conversion of 1 μmol of a certain type of substance in 1 min under given, regulated conditions of a test experiment.

The ratio of individual types of enzymes is regulated by the selection of the composition of nutrient media, the conditions for the cultivation of microorganisms and the biosynthesis of enzymes, as well as methods for their subsequent isolation. The multienzyme preparation can be used in powder form after isolation and freeze drying in the form of stabilized liquid products or fresh filtrates of culture liquids. The method can be implemented with any ratio of the components of the multienzyme preparation within the specified ranges of activity.

- As an alkaline agent in the treatment with an alkaline peroxide solution, you can use the traditionally used compounds tripolyphosphate, bicarbonate, sodium metasilicate, which performs primarily the function of a stabilizer of hydrogen peroxide, as well as soda ash, the concentration of which is determined taking into account the content of other agents to a set value of the total the alkalinity of the solution in terms of sodium hydroxide.

- Hydrogen peroxide is used as an oxidizing agent during treatment with an alkaline peroxide solution, the dosage of which is carried out taking into account its concentration in commercial exhaust forms in terms of active oxygen.

- As a detergent when washing the rovings after treatment with an alkaline peroxide solution, it is possible to use surfactants with a wetting and emulsifying effect, for example, neonol 9-12, EM-3P, XT-detergent.

- Organic acids, mainly acetic or oxalic, can be used as an agent for antimicrobial treatment.

- As additional components, if necessary, the enzyme treatment solution and alkaline peroxide solution may contain wetting agents, complexing agents, antifoams, neutral electrolytes.

- For the preparation of solutions, distilled, industrial or softened water can be used.

The method can be implemented on standard equipment for preparing flax rovings, in particular in autoclave devices of the OB-500-L, AKD-U-6 type or on laboratory equipment of the brand AL 210/1.

The method is implemented by sequentially carrying out the following operations:

- Deoxidation - designed to remove acidic degradation products of plant tissue of the flax stem in the primary processing of flax straw. The operation prevents the loss of enzyme activity upon impregnation of the severe rovings without introducing special buffering additives into the solution of the multienzyme preparation. Depending on the degree of acidification of raw materials, determined by the level of acid-base properties of aqueous extracts, deoxidation can be carried out by washing with technical or softened water, or by impregnating a soda solution of the required concentration. The processing is carried out at a temperature of 20-50 ° C, mainly at 40-45 ° C for 10-15 minutes.

- Enzymatic treatment with a solution of a multienzyme preparation with indicators of enzyme activity, units / ml:

- endopolygalacturonase - 20-25;

- pectin esterase - 2.5-4.7;

- protease - 0.2-0.3;

- exopoligalacturonase - 0.6-1.0;

- exogalactosidase - 0.2-0.4;

- exoxylosidase - 0.3-0.5;

- exoglucanase - 0.6-0.8.

The operation is carried out according to the variant of single-stage two-stage processing. At the first stage, the temperature and pH of the solution are selected based on a compromise combination of optimums on the dependences of the activity of each type of enzyme on the temperature and acidity of the medium, specific for different microbiological sources of their production. For most of the above mesophilic (medium-loving) microorganisms, the optimum temperature of enzyme activity is 40-50 ° C, the working pH range is neutral values and adjacent areas. Bath module 1: 10-1: 50. The processing time is 90-95 minutes. In the second stage, the solution is heated to boiling and kept “on a bale” with a total duration of 20-25 minutes.

- Rinsing with water is carried out at a temperature of 65-70 ° C for 10 min with a three-time change of water. It is possible to use non-ionic detergents at the first stage with a temperature increase of up to 80-85 ° С for more efficient removal of waxy impurities.

- Treatment with an alkaline-peroxide solution containing hydrogen peroxide at a concentration of 0.6-0.8 g / l in terms of active oxygen, a peroxide stabilizer (for example, MgSO ₄ or MgCl ₂ , polycarboxylic or oleic carboxylic acids, sodium silicate or metasilicate), alkaline agents (for example, tripolyphosphate, soda ash) to a total alkalinity of 6.5-7.0 g / l in terms of NaOH. If necessary, the solution may include wetting agents, complexing agents, neutral electrolytes. The bath module is predominantly 1:10. Processing is carried out with heating the solution to a boil and holding it “to a bale”. The total duration of 90-95 minutes

- Flushing in three stages. At the first stage, the treatment is carried out at a temperature of 70 ° C for 10 min with a detergent solution, mainly nonionic surfactants with an emulsifying effect, for example, neonol 9-12, EM-ZP, XT-detergent in quantities recommended by manufacturers. Next, the roving is washed twice with hot water at 70 ° C and 65 ° C for 10 minutes.

- Antimicrobial treatment with a solution of an organic quota, for example acetic, with a concentration of 1 g / l at 45-50 ° C for 15 minutes.

Evaluation of the effectiveness of the proposed method for preparing flax rovings for spinning and the prototype was carried out identically in terms of fiber properties in rovings (pok.1-8) and a set of indicators of the properties of the formed yarn (pok.9-22):

1 - fiber mass loss after processing the roving (ΔM,%); determined by the change in mass of the samples before and after processing [Friedman B.N. and others. A guide to spinning flax. - M .: 1979.];

2 - lignin content (L, wt.%) [Krichevsky G.E., Nikitkov V.A. Theory and practice of preparing textile materials from cellulose fibers. - M .: 1989. - 207 p.];

3 - the content of pectin substances (P, wt.%) [Krichevsky G.E., Nikitkov V.A. Theory and practice of preparing textile materials from cellulose fibers. - M .: 1989. - 207 p.];

4 - the degree of removal of pectin substances (ΔP,%) [Krichevsky G.E., Nikitkov V.A. Theory and practice of preparing textile materials from cellulose fibers. - M .: 1989. - 207 p.];

5 - the content of hemicelluloses, (HC, wt.%) [Krichevsky G.E., Nikitkov V.A. Theory and practice of preparing textile materials from cellulose fibers. - M .: 1989. - 207 p.];

6 - the degree of removal of hemicelluloses, (ΔHZ,%) [Krichevsky G.E., Nikitkov V.A. Theory and practice of preparing textile materials from cellulose fibers. - M .: 1989. - 207 p.];

7 - reduction of the breaking load in the wet state to the level of untreated roving (ΔР _M ,%) [Test of bast-fiber materials / VV Gorodov et al. - M .: 1969];

8 - whiteness, (B,%) [GOST 18054-72] the accuracy of the method is 0.1%;

9 - linear density of yarn (T, Tex) [GOST 6611.1-73];

10 - coefficient of variation in linear density (C _T ,%) [GOST 11.004-74];

11 - the number of defects per 1000 m of yarn:

- thickenings exceeding 1.5d _SR (U _1.5, units / km);

- thinning, less than 0.7d _SR (Y _0.7 , units / km).

The indicators are evaluated using a monocular optical light microscope Biolam R-11 at a 70-fold increase;

12 - twist yarn (K _f , torsion per 1 m length) [Laboratory workshop on materials science of sewing production: Textbook. manual for universities / B.A. Buzov et al. - M .: Legprombytizdat, 1991. - P.57-60];

13 - coefficient of variation in twist (C _K ,%) [GOST 11.004-74];

14 - breaking load (P _r , SN) [GOST 6611.2-73];

15 - specific breaking load (P _y , cN / Tex) [GOST 6611.2-73];

16 - coefficient of variation in breaking load (C _P ,%) [GOST 11.004-74];

17 - specific work of the gap (r, kgf · cm / g) [GOST 6611.2-73];

18 - coefficient of variation in the work of the gap (C _r ,%) [GOST 11.004-74];

19 - the proportion of elongation components in single-cycle tests [Laboratory workshop on materials science of sewing production: Textbook. manual for universities / B.A. Buzov et al. - M.: Legprombytizdat, 1991. - S.166-172]:

- reversible elongation (Δ _bo ) - characterizes the amount of elastic deformation under tension;

- slow reversible elongation (Δ _mo ) - characterizes the elastic component of tensile deformation;

- residual elongation (Δ _ost ) - characterizes the irreversible deformation under tension;

20 - endurance to repeated bending and abrasion (n _and , cycles). Tests are carried out on a TKI brand instrument with an angle of passage of yarn through the eyes of a galey heel ring 10 °, stroke length 40 mm, load 15% of breaking load, vibration frequency

600 min ^-1 ;

21 - breakage of yarn (N, arr. / 100 ver · h). The assessment is carried out by statistical calculation of the number of breaks in the processing of yarn on weaving machines;

22 - grade of yarn [GOST 10078-85].

The invention is illustrated by the following examples.

Example 1

The roving No. 16 of coarse, fibrous Kaluga linen fiber was prepared for yarn production with a nominal linear density of 56 Tex. Processing rovings was carried out on the apparatus of the brand OB-500-L according to the following technological regime:

1 - deoxidation with water at 40 ° C for 10 min;

2 - enzymatic treatment with a solution of a multienzyme preparation obtained from the cultivation products of bacterial strains B. circulans VKPM B-1741, B. subtilis VKPM B-1093, Erw. carotovora VKPM B-1358, you. mesentericus VKPM B-2466, with indicators of enzyme activity, units / ml:

- endopoligalacturonase - 20;

- pectin esterase - 3.2;

- protease - 0.3;

- exopoligalacturonase - 0.8;

- exogalactosidase - 0.2;

- exoxylosidase - 0.4;

- exoglucanase - 0.7,

with the addition of 1 g / l of neonol 9-12 and 2 g / l of trilon B, 20 g / l of triethanolamine; solution temperature 50 ° C, bath module 1:10, processing time 90 min; heating and holding "on a bale" for 20 minutes;

3 - washing with a solution of XT-detergent 0.5 g / l for 10 minutes and twice with hot water at 70 ° C for 10 minutes;

4 - treatment with an alkaline peroxide solution containing 0.8 g / L hydrogen peroxide (in terms of active oxygen), sodium metasilicate 8.0 g / L and soda ash to a total alkalinity of 7.0 g / L (in terms of NaOH ) with heating from 45 to 98 ° C for 45 min and holding at 98 ° C for 50 min;

5 - washing with a solution of neonol 9-12 with a concentration of 0.8 g / l at 70 ° C for 10 minutes and then twice with hot water at 70 and 65 ° C for 10 minutes;

6 - antimicrobial treatment with acetic acid 0.9 g / l at 50 ° C for 15 minutes

After preparation of the rovings, the spinning was carried out wet on a PM-88-L8 spinning machine.

A yarn was obtained that meets the set of standardized quality indicators in accordance with the requirements of grade “I tall”.

For comparison, the processing of rovings was carried out according to the prototype using at the stage of enzymatic processing a mixture of the drug Pectofoetidin P10x and the drug oxidoreductases [Kundiy S.A. Development of energy-saving environmentally friendly technologies for the preparation of flax materials based on bioprocesses // Diss ... Cand. tech. sciences. - Ivanovo, 1999. - S.114-119]. Wet spinning was carried out with the same filling parameters of the PM-88-L8 spinning machine.

The results of comparing the properties of roving and yarn in the aggregate of the analyzed indicators of semi-finished products for the proposed method for preparing linen roving and prototype are presented in the table.

Example 2

Flax rovings of medium softness No. 16 of the stanza Vologda flax fiber were prepared for yarn production with a nominal linear density of 56 Tex. Processing rovings was carried out on the apparatus of the brand AL 210/1 in the following technological mode:

1 - deoxidation with a solution of soda ash 0.2 g / l at 45 ° C for 10 min;

2 - enzymatic treatment with a solution of a multienzyme preparation obtained by mixing the products of the cultivation of strains of P. lanosum F-387, Asp. flavus VKPM F-591 and Asp. awamori 22, with indicators of enzyme activity, units / ml:

- endopoligalacturonase - 25;

- pectin esterase - 2.5;

- protease - 0.2;

- exopoligalacturonase - 0.6;

- exogalactosidase - 0.4;

- exoxylosidase - 0.3;

- exoglucanase - 0.6

with the addition of 1 g / l of neonol 9-12 and 2 g / l of trilon B, 25 g / l of sodium bicarbonate; bath module 1:10, solution temperature 40 ° C, processing time 90 min; then heating and holding "on a bale" for 20 minutes;

3 - three times washing with hot water at 65 ° C for 10 min;

4 - treatment with an alkaline peroxide solution containing sodium metasilicate 7.8 g / l and soda ash calcined to a total alkalinity of 6.5 g / l (in terms of sodium hydroxide) and hydrogen peroxide of 0.6 g / l (in terms of active oxygen), with heating from 45 to 98 ° C for 45 min and holding at 98 ° C for 45 min;

5 - washing with a neonol detergent solution 9-12 with a concentration of 0.5 g / l at 70 ° C for 10 minutes, then twice with water at 70 and 65 ° C for 10 minutes;

6 - antimicrobial treatment with acetic acid 1 g / l at 50 ° C for 15 minutes

After preparation of the rovings, the spinning was carried out wet on a PM-88-L8 spinning machine.

The yarn obtained, corresponding in terms of the set of standardized quality indicators to the requirements of the grade “1 high-yielded”.

The test results of roving and yarn in the aggregate of the analyzed indicators of semi-finished products are presented in the table.

Example 3

Preparation was carried out for the osseous roving No. 16 of Kaluga linen fiber for yarn production with a nominal linear density of 56 Tex. Processing rovings was performed on the apparatus of the brand AKD-U-6 according to the following technological regime:

1 - deoxidation with a solution of soda ash 0.2 g / l at 45 ° C for 10 min;

2 - enzymatic treatment with a solution of a multienzyme preparation obtained from the cultivation products of bacterial strains B. circulans VKPM B-6747, B. subtilis VKPM B-1093, Erw. carotovora VKPM B-2970, B. mesentericus VKPM B-1559, with indicators of enzyme activity, units / ml:

- endopoligalacturonase (pectinase) - 25;

- pectin esterase - 4.7;

- protease - 0.3;

- exopoligalacturonase - 1.0;

- exogalactosidase - 0.3;

- exoxylosidase - 0.5;

- exoglucanase - 0.8

with the addition of 1 g / l of neonol 9-12 and 2 g / l of trilon B, 25 g / l of sodium bicarbonate; module 1:10, solution temperature 50 ° C, processing time 95 min; subsequent heating to a boil and holding "to a bale" for 25 minutes;

3 - washing with an XT-detergent solution of 0.5 g / l for 10 minutes and twice with hot water at 70 ° C for 10 minutes;

4 - treatment with an alkaline peroxide solution containing sodium metasilicate 8.0 g / l and soda ash calcined to a total alkalinity of 7.0 g / l (in terms of sodium hydroxide) and hydrogen peroxide of 0.7 g / l (in terms of active oxygen) with heating from 45 to 98 ° C for 45 min and holding at 98 ° C for 50 min;

5 - washing with a detergent solution EM-3P 0.5 g / l at 70 ° C for 10 minutes and then twice with hot water at 70 and 65 ° C for 10 minutes;

6 - antimicrobial treatment with acetic acid 0.9 g / l at 50 ° C for 15 minutes

After preparation of the rovings, the spinning was carried out wet on a PM-88-L8 spinning machine.

The yarn obtained, corresponding in terms of the set of standardized quality indicators to the requirements of the grade “1 high-yarrow”.

The test results of roving and yarn in the aggregate of the analyzed indicators of semi-finished products are presented in the table.

These tables show that the claimed method is applicable for preparing for spinning rovings from domestic high-lignified varieties of medium-soft flaxseed, coarse and hairy fiber with a significant increase in the spinning properties of the fiber and the quality of the yarn obtained.

Thus, the fiber whiteness in the prepared roving is increased by 2.5 times, which is the result of deliberately controlled destruction of impurities, carried out within the acceptable values of fiber mass loss, and achieving a 70-75% degree of lignin removal, i.e. 1.56 times higher than in the prototype method.

As a result of increasing the degree of removal of pectins by 1.6-1.7 times and improving the preparedness of the complex fiber for uniform crushing, characterized by a 1.58-fold increase in the reduction of the breaking load of the rovings in the wet state relative to the level of the indicator for the untreated roving, a finer yarn was obtained, satisfying the requirements of GOST 10078-85 for grades “1 high-rooted” or “1 high-roasted”. The coefficient of variation in linear density is reduced by 2.1-2.8 times, the coefficient of variation in breaking load is 1.7-2.1 times.

The breakage of the yarn in the weaving process is reduced by 1.6-2 times due to the fact that the removal of technologically necessary hemicelluloses is reduced by 1.9-2.2 times. The dried yarn obtained by the proposed method for preparing rovings has:

• higher strength:

- breaking load increases in comparison with the known method 1.13-1.16 times;

- specific breaking load increases 1.14-1.23 times;

- the work of the gap increases by 1.05-1.08 times;

- the coefficient of variation in the work of the gap decreases 1.34-1.55 times;

• improved deformation and elastic properties of yarn:

- twist rate increased by 5-7%;

- the coefficient of variation in twist is reduced by 1.2-1.3 times;

- the proportion of slowly reversible relaxation in the total elongation in single-cycle tests is increased 1.28-1.39 times;

- resistance to repeated bending and abrasion increased by 21-27%.

Improved aesthetics of textile products, as reduced the number of worsening the appearance of woven fabrics of defects in yarn with thickenings _1,5

1.8-2 times and with thinning U _0.7 3.4-4.1 times.

According to the total set of standardized indicators, the yarn obtained by the proposed method of enzymatic-peroxide preparation of highly lignified linen rovings is characterized by a higher grade.

Comparative results of the quality of prepared rovings and obtained yarn according to the proposed method Semi-finished product quality indicators The value of the indicators in the preparation of rovings according to the proposed and known methods example number 1 example number 2 example number 3 proposed prototype proposed proposed ΔM,% 13 8.3 fourteen eleven L, wt.% 8.4 / 2.15 8.4 / 3.36 6.3 / 1.89 10.1 / 3.05 P, wt.% 2.7 / 0.39 2.7 / 1.49 3.3 / 0.50 3.6 / 0.54 ΔP,% 85 45 85 85 GC, wt.% 10.5 / 7.35 10.5 / 3.67 13.5 / 8.75 12.8 / 8.41 ΔHZ,% thirty 65 35 34 ? P _M,% 68 43 70 65 B% 55.0 22.8 56.1 54.8 T, Tex 53.3 56.6 53.0 56.2 C _T % 2.2 5,4 1.9 2.6 _1.5 , pcs / km 1920 3570 1780 1940 At _0.7 , pcs./km 1171 3960 970 1050 K _f , cr. / M 550 524 562 547 _P C% 7.9 9,4 7.2 8.1 R _p , SN 1327 1147 1306 1298 R _y , cN / Tex 25.0 20.3 24.6 23.1 C _P % 11.3 21.5 10,2 12,4 r, kgfcm / g 42.6 40,4 43,4 43.7 C _r ,% 5,4 7.9 5.1 5.9 Δ _bo 0.38 0.39 0.37 0.39 Δ _mo 0.25 0.18 0.25 0.23 Δ _ost 0.37 0.43 0.38 0.38 n _And , cycles 6745 5432 6897 6589 N, Sample / 100 verh 45 80 40 fifty Grade 1 VL 1 Srl 1 VL 1 VO Notes: 1) in the numerator and denominator of the conditional fraction, the values of the impurity content are given, respectively, in the severe roving and after preparation; 2) the grade of yarn: VL and VO - vysokolnyaya and vysokoechnical; Srl - median.

Claims (1)

A method of enzymatic-peroxide preparation for spinning a highly lignified flax rove, comprising enzymatic treatment with a solution of a multienzyme preparation, including endopoligalacturonase, pectin esterase, protease and exopoligalacturonase, washing with water, alkaline peroxide solution, washing with a mild detergent and water and by enzymatic treatment with a polyenzyme preparation, the roving is deoxidized; a solution is used as a polyenzyme preparation . ADDITIONAL comprising ekzogalaktozidazu, ekzoksilozidazu ekzoglyukanazu and with measures of enzyme activity U / ml:
endopolygalacturonase 20-25 pectin esterase 2.5-4.7 protease 0.2-0.3 exopoligalacturonase 0.6-1.0 exogalactosidase 0.2-0.4 exoxylosidase 0.3-0.5 exoglucanase 0.6-0.8
enzyme treatment is carried out at a temperature of 40-50 ° C for 90-95 minutes, followed by heating to a boil and holding for 20-25 minutes, and treatment with an alkaline peroxide solution is carried out at a concentration of hydrogen peroxide of 0.6-0.8 g / l (active oxygen) and total alkalinity of 6.5-7.0 g / l (in terms of caustic soda) for 90-95 minutes