CN111020722B - Regenerated cellulose fiber of centella asiatica viscose carrier and preparation method thereof - Google Patents
Regenerated cellulose fiber of centella asiatica viscose carrier and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
- D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
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- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/65—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing epoxy groups
- D06M15/652—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing epoxy groups comprising amino groups
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
- D10B2201/20—Cellulose-derived artificial fibres
- D10B2201/22—Cellulose-derived artificial fibres made from cellulose solutions
- D10B2201/24—Viscose
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- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/06—Load-responsive characteristics
- D10B2401/061—Load-responsive characteristics elastic
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/06—Load-responsive characteristics
- D10B2401/063—Load-responsive characteristics high strength
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- D10B2401/13—Physical properties anti-allergenic or anti-bacterial
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Abstract
The invention provides regenerated cellulose fibers of a centella asiatica viscose carrier, belonging to the technical field of fiber materials, wherein the fibers contain a centella asiatica extract, and the content of the fibers is 0.2-12%; the invention also provides a preparation method of the regenerated cellulose fiber of the centella asiatica viscose carrier, which comprises pretreatment, enzyme bath, ozone-electric field treatment, premixing, wet spinning, protection and washing; the regenerated cellulose fiber of the centella asiatica viscose carrier has stable mechanical performance indexes, and the dry heat shrinkage rate is 0.001-0.003%; has excellent moisture absorption performance, and the moisture regain is 13.1-16.2%; the cotton gauze has excellent air permeability and moisture absorption, wherein the moisture absorption hysteresis value is 20 percent higher than that of the common commercial pure cotton gauze, and the maximum value can reach 27.1 percent; the moisture-dissipating function of the gauze is 15.7 percent higher than that of the common pure cotton gauze sold in the market, and the maximum moisture-dissipating function can reach 22.6 percent.
Description
Technical Field
The invention belongs to the technical field of fiber materials, relates to a cellulose fiber product, and particularly relates to a regenerated cellulose fiber of a centella asiatica viscose carrier and a preparation method thereof.
Background
Regenerated cellulose fiber is an abbreviation of English cellulose fiber, has a structure and a composition similar to cotton, is different from cotton fiber in that the moisture absorption and the air permeability are better than those of the cotton fiber, is one of all chemical fibers with the best moisture absorption and air permeability, and is known as breathable fabric. The raw material is natural cellulose (cotton, hemp, bamboo, tree and shrub), the chemical structure of which is not changed, and the regenerated cellulose fiber with better performance is manufactured only by changing the physical structure of the natural cellulose.
The invention patent application with the Chinese patent application number of CN106757454A provides a preparation method of enteromorpha regenerated cellulose fiber, which comprises the steps of firstly preparing enteromorpha pulp, bleaching to obtain an enteromorpha regenerated fiber stock solution, adding dimethyl sulfoxide and N, N-dimethylformamide into the enteromorpha regenerated fiber stock solution to obtain an enteromorpha regenerated cellulose fiber spinning stock solution, feeding the enteromorpha regenerated cellulose fiber spinning stock solution into spinning equipment for extrusion, concentration and solidification, winding, elongation and thinning to obtain the enteromorpha regenerated cellulose fiber. The preparation method only extracts cellulose in the enteromorpha, active ingredients in the plants are almost lost and wasted, and the enteromorpha is only a gimmick name and cannot actually have plant functional characteristics.
The patent of publication No. CN102605462B provides a high-strength viscose fiber, which is obtained by uniformly mixing aromatic polyamide and viscose stock solution according to the mass ratio of 1:20 at 90-150 ℃ under the condition of gaseous NH3 to obtain a mixed solution and then spinning the mixed solution to obtain the viscose fiber, thereby solving the technical problem of low strength of the existing viscose fiber and greatly improving the wet strength performance of the viscose fiber.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a modified fiber master batch and a preparation method thereof, so as to realize the following purposes:
(1) the regenerated cellulose fiber of the asiatic centella adhesive carrier has stable basic mechanical performance indexes, higher strength and higher breaking elongation, uniform strength and good dry heat shrinkage;
(2) the regenerated cellulose fiber of the asiatic pennywort herb viscose carrier has excellent moisture absorption performance;
(3) the regenerated cellulose fiber of the centella asiatica viscose carrier has excellent antibacterial effect;
(4) the anti-pilling performance of the fabric made of the regenerated cellulose fiber of the centella asiatica viscose carrier is improved by 7.5-12.4% on the premise that other excellent performances are not changed.
In order to solve the technical problems, the following technical scheme is adopted:
the regenerated cellulose fiber of the centella asiatica viscose carrier is characterized in that:
the regenerated cellulose fiber of the centella asiatica viscose carrier contains a centella asiatica extract.
The technical scheme of the invention is further defined as follows:
the content of centella asiatica extract is 0.2-2.0%.
The regenerated cellulose fiber of the asiatic pennywort herb viscose carrier has the wet breaking strength of 3.6-3.9CN/tex and the strength unevenness of 0.0-0.001%.
A preparation method of regenerated cellulose fibers of a centella asiatica viscose carrier comprises the steps of pretreatment, enzyme bath, ozone-electric field treatment, premixing, wet spinning, protection and washing.
In the pretreatment, the addition amount of 95% ethanol-water solution is 150%, and the addition amount of L-cysteine is 5%.
The enzyme bath temperature is 37-45 ℃, the pH is controlled at 5.2-7.6, after the enzyme bath is carried out for 5-8min, 3 percent glacial acetic acid is added, the pH is adjusted to 4.8-7.2, the stirring is carried out, and the enzyme bath is continued for 15-18 mi.
The composite active enzyme is GDSL esterase, xylanase, papain and catalase in a mass ratio of 2:5-8:18: 1.
The enzyme activity of the GDSL esterase is more than or equal to 5.5 wu/g, the enzyme activity of the xylanase is more than or equal to 10 wu/g, the enzyme activity of the papain is more than or equal to 10 wu/g, and the enzyme activity of the catalase is 6-8 wu/g.
The ozone-electric field treatment is carried out, the flow rate of the mixed solution of the asiatic pennywort herb pulp is 5-17mL/min, and the treatment time is 15-30 min.
The ozone-electric field treatment is to introduce 0.8-22mg/L ozone into the asiatic pennywort herb plant pulp at a speed of 25-42L/min, and keep the temperature at 22-36 ℃.
The ozone-electric field treatment has the electric field intensity of 80-120kV/cm, the pulse width of 0.05-1ms, the pulse frequency of 5-5000Hz and the current peak value of 10-5000A.
And pre-mixing, namely naturally drying the centella extract until the water content is 6-10%, adding the centella extract into the viscose stock solution, uniformly stirring, sequentially adding the penetrating agent, the cross-linking agent and the retention aid, uniformly stirring, and defoaming to obtain the pre-mixed spinning solution.
The mass ratio of the viscose stock solution to the penetrating agent to the cross-linking agent to the retention aid is 25:2-16:6-8: 1.
The addition amount of the centella asiatica extract is 0.2-2% of the total amount.
The viscose stock solution has the indexes of 38-60s of viscosity (falling ball method) and 10% NH of maturity4CI value) 12-25ml, alpha cellulose content 8.2-10.5% and NaOH content 2.0-8.5%.
The penetrating agent is Triton X-100, the molecular formula is (C2H4O) N.C14H22O, the CAS number is 9002-93-1, and the EINECS number is 255-695-5.
The cross-linking agent is prepared from the following components in a mass ratio of 0.1: 1:20 adipic acid dihydrazide, acetaldehyde and glyoxal.
The retention aid is a mixture of beryllium chloride and Cpma in a mass ratio of 7: 1.
And defoaming, wherein the content of air bubbles is less than 0.001%.
And in the wet spinning, the premixed spinning solution is injected into a spinning nozzle through a meter, enters a coagulating bath, and is subjected to drafting, forming and cutting to obtain the fiber tows.
Wherein, the coagulating bath formula is as follows: 66-105g/l of sulfuric acid, 22-65g/l of zinc sulfate, 110g/l of sodium sulfate and 250g/l of sodium sulfate, and the temperature of a coagulation bath is 45-52 ℃. The spinning speed is 45-74 m/min.
And the protection comprises the steps of adding 7-10 times of epoxy quaternized modified amino silicone oil by weight into the fiber tow, soaking for 25-40min, adding 2-5% ferrous sulfate solution, controlling the temperature at 2-9 ℃, and slowly stirring for 5-15 min.
And (3) washing, namely washing the product for 2-3 times by using 0.01-0.03mol/L ethanol, washing the product to a neutral pH value by using deionized water, and naturally airing to obtain the regenerated cellulose fiber of the centella asiatica viscose carrier.
The regenerated cellulose fiber of the centella asiatica viscose carrier is subjected to an antibacterial experiment by adopting a GB/T20944.3-2008 oscillation method, the washing procedure is 7B, the washing times are 50 times, and the regenerated cellulose fiber is rolled and dried, and the result is that: the bacteriostasis rate of staphylococcus aureus ATCC6538 is 92.2-99.2%, the bacteriostasis rate of escherichia coli 8099 is 99.2-99.6%, and the bacteriostasis rate of candida albicans ATCC10231 is 91.2-94.7%.
The anti-pilling performance of the fabric made of the regenerated cellulose fiber of the centella asiatica viscose carrier is improved by 7.5-12.4% on the premise that other excellent performances are not changed.
By adopting the technical scheme, compared with the prior art, the invention has the following advantages:
(1) the regenerated cellulose fiber of the asiatic centella viscose carrier is stable in basic mechanical performance index, has high strength and high elongation at break, and has the dry breaking strength of 4.1-4.2CN/tex, the wet breaking strength of 3.6-3.9CN/tex, the elongation at break of 18.4-20.6%, the strength irregularity of 0.0-0.001% and the dry heat shrinkage rate (177 ℃ C. 10min. 0.05CN/dtex) of 0.001-0.003%;
(2) the regenerated cellulose fiber of the asiatic pennywort herb viscose carrier has excellent moisture absorption performance, and the moisture regain is 13.1-16.2%;
(3) the regenerated cellulose fiber of the asiatic pennywort herb viscose carrier has obvious activation effect on the skin in direct contact, can improve the microcirculation of a human body, activate histiocyte, promote metabolism and enhance immunity: can emit far infrared light waves of 7-10 μm;
(4) the regenerated cellulose fiber of the centella asiatica viscose carrier disclosed by the invention is subjected to an antibacterial experiment by adopting a GB/T20944.3-2008 oscillation method, the washing procedure is 7B, the washing times are 50 times, and the regenerated cellulose fiber is rolled and dried, and the result is that: the bacteriostasis rate of staphylococcus aureus ATCC6538 is 92.2 percent, the bacteriostasis rate of escherichia coli 8099 is 99.2 percent, and the bacteriostasis rate of candida albicans ATCC10231 is 91.2 percent;
(5) the anti-pilling performance of the fabric made of the regenerated cellulose fiber of the asiatic pennywort herb viscose carrier is improved by 7.5-12.4% on the premise that other excellent performances are not changed;
(6) the gauze prepared from the regenerated cellulose fibers of the viscose carrier prepared by the method has excellent air permeability and moisture absorption, wherein the moisture absorption hysteresis value is 20 percent higher than that of the common commercially available pure cotton gauze, and can reach 27.1 percent at most; the moisture-dissipating function of the gauze is 15.7 percent higher than that of the common pure cotton gauze sold in the market, and the maximum moisture-dissipating function can reach 22.6 percent.
Detailed Description
Example 1 regenerated cellulose fiber of centella asiatica viscose carrier and preparation method thereof
The preparation method of the regenerated cellulose fiber of the centella asiatica viscose carrier specifically comprises the following steps:
(1) pretreatment of
Weighing tender leaves of centella asiatica, cleaning, adding 150% of 95% ethanol-water solution and 5% of L-cysteine, stirring, crushing the tender leaves of centella asiatica with a crusher to prepare pulp, filtering to remove impurities, drying to remove water, wherein the water content is less than or equal to 18%.
(2) Enzyme bath
Adding the above herba Centellae pulp into composite active enzyme, performing enzyme bath treatment at 37 deg.C and pH 7.6, adding 3% glacial acetic acid after enzyme bath for 5min, adjusting pH to 7.2, stirring, and continuing enzyme bath for 15 min.
The composite active enzyme is GDSL esterase, xylanase, papain and catalase in a mass ratio of 2:8: 18: 1;
the enzyme activity of GDSL esterase is 5.5 wu/g, the enzyme activity of xylanase is 10 wu/g, the enzyme activity of papain is 10 wu/g, and the enzyme activity of catalase is 6.8 wu/g.
(3) Ozone-electric field treatment
Starting an ozone generator, introducing ozone with concentration of 0.8mg/L into the above herba Centellae plant pulp at a rate of 42L/min to obtain herba Centellae pulp mixed solution. And meanwhile, opening the thermostat, controlling the temperature of the mixed solution of the asiatic pennywort herb pulp to be kept within the range of 22 ℃, pumping the mixed solution of the asiatic pennywort herb pulp into a pulse electric field for pulse treatment, stopping the ozone-electric field treatment after 30min of treatment, filtering, removing enzyme, and drying to obtain the asiatic pennywort herb extract.
The pulse treatment has the field intensity of 80kV/cm, the pulse width of 1ms, the pulse frequency of 5-5000Hz, the current peak value of 10-5000A and the flow rate of the mixed solution of the asiatic pennywort herb pulp of 5 mL/min.
(4) Premixing
Naturally drying the centella asiatica extract until the water content is 6%, adding the centella asiatica extract into the viscose stock solution, uniformly stirring, sequentially adding the penetrating agent, the cross-linking agent and the retention aid, uniformly stirring, and defoaming to obtain the premixed spinning solution.
The mass ratio of the viscose stock solution to the penetrating agent to the cross-linking agent to the retention aid is 25:16:6: 1;
the addition amount of the centella asiatica extract is 2% of the total amount;
the viscose stock solution has the indexes of 38s of viscosity (falling ball method) and 10 percent of NH4CI value) 25ml, alpha cellulose content 8.2 percent and NaOH content 8.5 percent;
the penetrating agent is Triton X-100, the molecular formula is (C2H4O) N.C14H22O, the CAS number is 9002-93-1, the EINECS number is 255-695-5;
the cross-linking agent is prepared from the following components in a mass ratio of 0.1: 1:20 of adipic acid dihydrazide, acetaldehyde and glyoxal;
the retention aid is a mixture of beryllium chloride and Cpma in a mass ratio of 7: 1;
and defoaming, wherein the content of air bubbles is less than 0.001%.
(5) Wet spinning
And (3) pumping the premixed spinning solution into a spinning nozzle through a metering device, entering a coagulating bath, and obtaining fiber tows through drafting, forming and cutting.
Wherein, the coagulating bath formula is as follows: 66g/l of sulfuric acid, 65g/l of zinc sulfate and 110g/l of sodium sulfate, and the coagulation bath temperature is 52 ℃. The spinning speed was 45 m/min.
(6) Protection of
Adding 7 times of epoxy quaternized modified amino silicone oil into the fiber tow, soaking for 40min, adding 2% ferrous sulfate solution, controlling the temperature at 9 ℃, and slowly stirring for 5 min.
(7) Washing machine
Washing the product with 0.01mol/L ethanol for 3 times, washing with deionized water until the pH value is neutral, and naturally airing to obtain the regenerated cellulose fiber of the centella asiatica viscose carrier.
The regenerated cellulose fiber of the viscose carrier of the embodiment is subjected to an antibacterial experiment by using a GB/T20944.3-2008 oscillation method, and the washing procedure is 7B, the washing times are 50 times, and the result is as follows: the bacteriostasis rate of staphylococcus aureus ATCC6538 is 92.2%, the bacteriostasis rate of escherichia coli 8099 is 99.2%, and the bacteriostasis rate of candida albicans ATCC10231 is 91.2%.
The anti-pilling performance of the fabric made of the regenerated cellulose fibers of the viscose carrier is improved by 7.7 percent on the premise that other excellent performances are not changed.
Example 2 regenerated cellulose fiber of centella asiatica viscose carrier and preparation method thereof
The preparation method of the regenerated cellulose fiber of the centella asiatica viscose carrier specifically comprises the following steps:
(1) pretreatment of
Weighing tender leaves of centella asiatica, cleaning, adding 150% of 95% ethanol-water solution and 5% of L-cysteine, stirring, crushing the tender leaves of centella asiatica with a crusher to prepare pulp, filtering to remove impurities, drying to remove water, wherein the water content is less than or equal to 18%.
(2) Enzyme bath
Adding the above herba Centellae pulp into composite active enzyme, performing enzyme bath treatment at 42 deg.C and pH 7.1, after enzyme bath for 8min, adding 3% glacial acetic acid, adjusting pH to 6.8, stirring, and continuing enzyme bath for 20 min.
The composite active enzyme is GDSL esterase, xylanase, papain and catalase in a mass ratio of 2:6:18: 1;
the enzyme activity of GDSL esterase is 5.7 wu/g, the enzyme activity of xylanase is 10 wu/g, the enzyme activity of papain is 10 wu/g, and the enzyme activity of catalase is 7 wu/g.
(3) Ozone-electric field treatment
Starting an ozone generator, introducing ozone with the concentration of 10mg/L into the asiatic pennywort herb plant pulp at the speed of 32L/min to obtain the asiatic pennywort herb pulp mixed solution. And meanwhile, opening the thermostat, controlling the temperature of the mixed solution of the asiatic pennywort herb pulp to be kept within the range of 22-30 ℃, pumping the mixed solution of the asiatic pennywort herb pulp into a pulse electric field for pulse treatment, stopping the ozone-electric field treatment after 22min of treatment, filtering, removing enzyme, and drying to obtain the asiatic pennywort herb extract.
The pulse treatment has the electric field intensity of 100kV/cm, the pulse width of 0.05-1ms, the pulse frequency of 5-5000Hz, the current peak value of 10-5000A and the flow rate of the mixed solution of the asiatic pennywort herb pulp of 13 mL/min.
(4) Premixing
Naturally drying the centella asiatica extract until the water content is 8%, adding the centella asiatica extract into the viscose stock solution, uniformly stirring, sequentially adding the penetrating agent, the cross-linking agent and the retention aid, uniformly stirring, and defoaming to obtain the premixed spinning solution.
The mass ratio of the viscose stock solution to the penetrating agent to the cross-linking agent to the retention aid is 25:8:7: 1;
the addition amount of the centella asiatica extract is 2.7 percent of the total amount;
the viscose stock solution has the indexes of 38-60s of viscosity (falling ball method) and 10% NH of maturity4CI value) 22ml, alpha cellulose content 9.4 percent and NaOH content 7.5 percent;
the penetrating agent is Triton X-100, the molecular formula is (C2H4O) N.C14H22O, the CAS number is 9002-93-1, the EINECS number is 255-695-5;
the cross-linking agent is prepared from the following components in a mass ratio of 0.1: 1:20 of adipic acid dihydrazide, acetaldehyde and glyoxal;
the retention aid is a mixture of beryllium chloride and Cpma in a mass ratio of 7: 1;
and defoaming, wherein the content of air bubbles is less than 0.001%.
(5) Wet spinning
And (3) pumping the premixed spinning solution into a spinning nozzle through a metering device, entering a coagulating bath, and obtaining fiber tows through drafting, forming and cutting.
Wherein, the coagulating bath formula is as follows: 100g/l of sulfuric acid, 55g/l of zinc sulfate and 1250g/l of sodium sulfate, and the coagulation bath temperature is 50 ℃. The spinning speed was 66 m/min.
(6) Protection of
Adding 8 times of epoxy quaternized modified amino silicone oil into the fiber tow, soaking for 33min, adding 3.5% ferrous sulfate solution, controlling the temperature at 5 ℃, and slowly stirring for 12 min.
(7) Washing machine
Washing the product with 0.02mol/L ethanol for 2-3 times, washing with deionized water until the pH value is neutral, and naturally airing to obtain the regenerated cellulose fiber of the centella asiatica viscose carrier.
The regenerated cellulose fiber of the viscose carrier of the embodiment is subjected to an antibacterial experiment by using a GB/T20944.3-2008 oscillation method, and the washing procedure is 7B, the washing times are 50 times, and the result is as follows: the bacteriostasis rate of staphylococcus aureus ATCC6538 is 99.2%, the bacteriostasis rate of escherichia coli 8099 is 99.6%, and the bacteriostasis rate of candida albicans ATCC10231 is 94.7%.
The anti-pilling performance of the fabric made of the regenerated cellulose fibers of the viscose carrier is improved by 12.4% on the premise that other excellent performances are not changed.
Example 3 regenerated cellulose fiber of centella asiatica viscose carrier and preparation method thereof
The preparation method of the regenerated cellulose fiber of the centella asiatica viscose carrier specifically comprises the following steps:
(1) pretreatment of
Weighing tender leaves of centella asiatica, cleaning, adding 150% of 95% ethanol-water solution and 5% of L-cysteine, stirring, crushing the tender leaves of centella asiatica with a crusher to prepare pulp, filtering to remove impurities, drying to remove water, wherein the water content is less than or equal to 18%.
(2) Enzyme bath
Adding the above herba Centellae pulp into composite active enzyme, performing enzyme bath treatment at 45 deg.C and pH 5.2, adding 3% glacial acetic acid after enzyme bath for 8min, adjusting pH to 4.8, stirring, and continuing enzyme bath for 18 min.
The composite active enzyme is GDSL esterase, xylanase, papain and catalase in a mass ratio of 2:5:18: 1;
the enzyme activity of GDSL esterase is 6.5 ten thousand u/g, the enzyme activity of xylanase is 10 ten thousand u/g, the enzyme activity of papain is 11.2 ten thousand u/g, and the enzyme activity of catalase is 8 ten thousand u/g.
(3) Ozone-electric field treatment
Starting an ozone generator, introducing ozone with concentration of 22mg/L into the above herba Centellae plant pulp at a rate of 25L/min to obtain herba Centellae pulp mixed solution. And meanwhile, opening the thermostat, controlling the temperature of the mixed solution of the asiatic pennywort herb pulp to be kept within the range of 36 ℃, pumping the mixed solution of the asiatic pennywort herb pulp into a pulse electric field for pulse treatment, stopping the ozone-electric field treatment after 15min of treatment, filtering, removing enzyme, and drying to obtain the asiatic pennywort herb extract.
The pulse treatment has the electric field intensity of 120kV/cm, the pulse width of 0.05-1ms, the pulse frequency of 5-5000Hz, the current peak value of 10-5000A and the flow rate of the mixed solution of the asiatic pennywort herb pulp of 17 mL/min.
(4) Premixing
Naturally drying the centella asiatica extract until the water content is 10%, adding the centella asiatica extract into the viscose stock solution, uniformly stirring, sequentially adding the penetrating agent, the cross-linking agent and the retention aid, uniformly stirring, and defoaming to obtain the premixed spinning solution.
The mass ratio of the viscose stock solution to the penetrating agent to the cross-linking agent to the retention aid is 25:2:8: 1;
the addition amount of the centella asiatica extract is 1.3 percent of the total amount;
the viscose stock solution has the indexes of 60s of viscosity (falling ball method) and 10% NH of maturity4CI value) 12ml, alpha cellulose content 10.5 percent and NaOH content 2.5 percent;
the penetrating agent is Triton X-100, the molecular formula is (C2H4O) N.C14H22O, the CAS number is 9002-93-1, the EINECS number is 255-695-5;
the cross-linking agent is prepared from the following components in a mass ratio of 0.1: 1:20 of adipic acid dihydrazide, acetaldehyde and glyoxal;
the retention aid is a mixture of beryllium chloride and Cpma in a mass ratio of 7: 1;
and defoaming, wherein the content of air bubbles is less than 0.001%.
(5) Wet spinning
And (3) pumping the premixed spinning solution into a spinning nozzle through a metering device, entering a coagulating bath, and obtaining fiber tows through drafting, forming and cutting.
Wherein, the coagulating bath formula is as follows: 105g/l of sulfuric acid, 60g/l of zinc sulfate and 110g/l of sodium sulfate, and the coagulation bath temperature is 52 ℃. The spinning speed was 74 m/min.
(6) Protection of
Adding 10 times of epoxy quaternized modified amino silicone oil into the fiber tow, soaking for 25min, adding 5% ferrous sulfate solution, controlling the temperature at 2 ℃, and slowly stirring for 15 min.
(7) Washing machine
Washing the product with 0.03mol/L ethanol for 2-3 times, washing with deionized water until the pH value is neutral, and naturally airing to obtain the regenerated cellulose fiber of the centella asiatica viscose carrier.
The regenerated cellulose fiber of the viscose carrier of the embodiment is subjected to an antibacterial experiment by using a GB/T20944.3-2008 oscillation method, and the washing procedure is 7B, the washing times are 50 times, and the result is as follows: the bacteriostasis rate of staphylococcus aureus ATCC6538 is 93.5%, the bacteriostasis rate of escherichia coli 8099 is 99.2%, and the bacteriostasis rate of candida albicans ATCC10231 is 92.6%.
The anti-pilling performance of the fabric made of the regenerated cellulose fibers of the viscose carrier is improved by 8.8% on the premise that other excellent performances are not changed.
The following are relevant tests for the regenerated cellulose fibers of the viscose carrier prepared according to the invention:
1. basic mechanical performance indexes:
2. the regenerated cellulose fiber of the viscose carrier prepared by the invention has excellent moisture absorption performance, and the moisture regain is 13.1-16.2%.
Table 2:
3. the regenerated cellulose fiber of the viscose carrier prepared by the invention has obvious activation effect on directly contacted skin, can improve human microcirculation, activate histiocyte, promote metabolism and enhance immunity: the regenerated cellulose fibers of the viscose support according to the invention were subjected to far infrared light wave trapping using an oscilloscope (brand: UNI-T, model: UTD2102 CEX) with the following results:
table 3:
4. the research and experiments of the applicant show that the gauze prepared from the regenerated cellulose fibers of the viscose carrier prepared by the invention has excellent air permeability and moisture absorption, and the moisture absorption hysteresis value of the gauze is 20 percent higher (average value) and can reach 27.1 percent higher (example 2) than that of the common commercial pure cotton gauze; the moisture-dispersing function of the cotton gauze is 15.7 percent (average value) higher than that of the common commercial pure cotton gauze, and the maximum value can reach 22.6 percent (example 2).
As is apparent from the above technical effects, the modified cellulose fiber of the present invention has the following advantages as compared with conventional cellulose fibers:
(1) the regenerated cellulose fiber of the asiatic centella viscose carrier is stable in basic mechanical performance index, has high strength and high elongation at break, and has the dry breaking strength of 4.1-4.2CN/tex, the wet breaking strength of 3.6-3.9CN/tex, the elongation at break of 18.4-20.6%, the strength irregularity of 0.0-0.001% and the dry heat shrinkage rate (177 ℃ C. 10min. 0.05CN/dtex) of 0.001-0.003%;
(2) the regenerated cellulose fiber of the asiatic pennywort herb viscose carrier has excellent moisture absorption performance, and the moisture regain is 13.1-16.2%;
(3) the regenerated cellulose fiber of the asiatic pennywort herb viscose carrier has obvious activation effect on the skin in direct contact, can improve the microcirculation of a human body, activate histiocyte, promote metabolism and enhance immunity: can emit far infrared light waves of 7-10 μm;
(4) the gauze prepared from the regenerated cellulose fiber of the viscose carrier prepared by the invention has excellent air permeability and moisture absorption, wherein the moisture absorption hysteresis value is 20 percent (average value) higher than that of the common commercial pure cotton gauze (purchased from Beiqi textile Co., Ltd., China Tung City, the cargo number: 16003A) and can reach 27.1 percent at most (example 2); the moisture-dispersing function of the cotton gauze is 15.7 percent (average value) higher than that of the common commercial pure cotton gauze, and the maximum value can reach 22.6 percent (example 2).
All percentages used herein are weight percentages and all ratios described herein are mass ratios, unless otherwise indicated.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. A preparation method of regenerated cellulose fiber of a centella asiatica viscose carrier is characterized by comprising the following steps: the regenerated cellulose fiber of herba Centellae viscose carrier contains herba Centellae extract;
the preparation method comprises the steps of pretreatment, enzyme bath, ozone-electric field treatment, premixing, wet spinning, protection and washing;
the enzyme bath is characterized in that asiatic centella pulp is added into the compound active enzyme for enzyme bath treatment, the temperature of the enzyme bath is 37-45 ℃, the pH value is controlled to be 5.2-7.6, 3% glacial acetic acid is added after the enzyme bath is carried out for 5-8min, the pH value is adjusted to be 4.8-7.2, the mixture is stirred, and the enzyme bath is continued for 15-18 min;
in the pretreatment, the addition amount of a 95% ethanol-water solution is 150%, and the addition amount of L-cysteine is 5%;
the composite active enzyme is GDSL esterase, xylanase, papain and catalase in a mass ratio of 2:5-8:18: 1;
the ozone-electric field treatment is carried out, the flow rate of the mixed solution of the asiatic pennywort herb pulp is 5-17mL/min, and the treatment time is 15-30 min;
the ozone-electric field treatment is carried out, wherein ozone with the concentration of 0.8-22mg/L is introduced into the asiatic pennywort herb plant pulp at the speed of 25-42L/min, and the temperature is kept at 22-36 ℃;
the ozone-electric field treatment is carried out, the field intensity of the electric field is 80-120kV/cm, the pulse width is 0.05-1ms, the pulse frequency is 5-5000Hz, and the current peak value is 10-5000A;
the preparation method comprises the steps of premixing, namely naturally drying the centella extract until the water content is 6-10%, adding the centella extract into a viscose stock solution, uniformly stirring, sequentially adding a penetrating agent, a cross-linking agent and a retention aid, uniformly stirring, and defoaming to obtain a premixed spinning solution;
the mass ratio of the viscose stock solution to the penetrating agent to the cross-linking agent to the retention aid is 25:2-16:6-8: 1;
the addition amount of the centella asiatica extract is 0.2-2% of the total amount;
and the protection comprises the steps of adding 7-10 times of epoxy quaternized modified amino silicone oil by weight into the fiber tow, soaking for 25-40min, adding 2-5% ferrous sulfate solution, controlling the temperature at 2-9 ℃, and slowly stirring for 5-15 min.
2. The method for preparing regenerated cellulose fiber of centella asiatica viscose carrier according to claim 1, wherein the method comprises the following steps: the content of centella asiatica extract is 0.2-2%.
3. The method for preparing regenerated cellulose fiber of centella asiatica viscose carrier according to claim 1, wherein the method comprises the following steps: the enzyme activity of the GDSL esterase is more than or equal to 5.5 wu/g, the enzyme activity of the xylanase is more than or equal to 10 wu/g, the enzyme activity of the papain is more than or equal to 10 wu/g, and the enzyme activity of the catalase is 6-8 wu/g.
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