CN106929931B - Viscose fiber containing isatis root extract and preparation method thereof - Google Patents
Viscose fiber containing isatis root extract and preparation method thereof Download PDFInfo
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- CN106929931B CN106929931B CN201710183744.5A CN201710183744A CN106929931B CN 106929931 B CN106929931 B CN 106929931B CN 201710183744 A CN201710183744 A CN 201710183744A CN 106929931 B CN106929931 B CN 106929931B
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08G12/30—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with substituted triazines
- C08G12/32—Melamines
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention provides a viscose fiber containing an isatis root extract, wherein the content of isatis root microcapsules is 9.1-9.79%, the dry breaking strength of the fiber is 2.70-2.75cN/dtex, the wet breaking strength is 1.70-1.75cN/dtex, the elongation at break is 22-23%, the bacteriostasis rate to staphylococcus aureus is 99.0-99.8%, the bacteriostasis rate to candida albicans is 96.6-98.8%, the bacteriostasis rate to typhoid bacillus is 97.2-99.1%, and the viscose fiber has strong inhibiting and killing effects on influenza A virus and influenza B virus; the invention also provides a preparation method of the viscose fiber containing the isatis root extract, which comprises the modification of isatis root microcapsules; the method reduces the loss of the radix isatidis microcapsules in the fiber preparation process, and reduces the bench-dismantling backwashing rate of the coagulation bath filter; improve the distribution uniformity of the isatis root microcapsules in the fiber.
Description
Technical Field
The invention relates to a viscose fiber, in particular to a viscose fiber containing an isatis root extract and a preparation method thereof, belonging to the technical field of spinning.
Background
The development of functional fibers is an indicator of the scientific progress of modern fibers. The development of functional fibers, differential fibers and high-performance fibers is a technical innovation of the traditional textile industry, creates favorable conditions for the transformation of the high-tech industry, and makes a contribution to the improvement of the living standard of human beings. The functional fiber is a novel fiber having a specific function in addition to the physical and mechanical properties of general fibers.
The isatis root is an excellent Chinese medicinal material and has the effects of resisting bacteria, viruses and tumors and improving the immunologic function; the isatis root extract is added into viscose fiber to prepare the textile with health care functions of resisting virus, improving immunity and the like, and the textile meets the requirement of the public on products with health care functions at present.
Chinese patent CN105381766A (publication number) discloses a preparation method and application of radix isatidis extract vitamin protein composite microcapsules, wherein the preparation method comprises the steps of firstly preparing radix isatidis extract vitamin protein composite microcapsules, then adding the composite microcapsules into a viscose stock solution, preparing a blended spinning solution, and spinning through an adjusted coagulation bath; the viscose fiber with the functions of antivirus, skin care and health care is prepared by microencapsulation and crosslinking curing.
Chinese patent CN106192045A (publication number) discloses an isatis root cellulose fiber and a preparation method thereof, wherein isatis roots are made into microcapsules, then the microcapsules are blended with spinning stock solution, and the fibers are prepared through spinning, so that the prepared isatis root cellulose fiber has long effective component slow-release period and good effects of inhibiting bacteria, clearing heat and cooling blood, resisting viruses and improving immunity.
The above patents suffer from the following drawbacks:
(1) in the process of preparing the fiber, if microcapsule coating is not adopted, the isatis root extract is very soluble in water, on one hand, the effective substances of the isatis root are easily damaged by acid and alkali, and on the other hand, most of the effective substances are lost due to very high solubility.
(2) If the radix isatidis microcapsule is coated by the microcapsule, the radix isatidis microcapsule is easy to run off.
The specific process of the loss is as follows: in the viscose spinning solution, the content of the alpha fibers is between 8.2 and 9.2 percent, and about 90 percent of the viscose spinning solution is water, soluble salt and other substances, wherein only the alpha fibers can be solidified and formed in the spinning process to form fibers.
In the spinning process, when the blended solution of the viscose spinning solution and the radix isatidis microcapsules is sprayed into the coagulating bath, the alpha fibers begin to be formed and then coat the added microcapsules, but substances capable of being solidified and formed in the viscose spinning solution, namely the content of the alpha fibers is less than 10%, the microcapsules capable of being coated by the alpha fibers in the forming process are few, and a large amount of microcapsules can be lost along with 90% of substances such as water, soluble salts and the like in the spinning viscose spinning solution, so that the radix isatidis microcapsules are greatly lost.
In practical experiments, when the addition of the microcapsule solid dry powder to the alpha-fibers is 10%, the content of the microcapsules in finished fibers is less than 5%, a large amount of microcapsule materials enter a coagulating bath after flowing away, and the backwashing rate of a filter dismounting of the coagulating bath is increased by 75%.
(3) Because the radix isatidis is easy to run off, the radix isatidis component on the surface of the fiber is easier to run off than that in the fiber during the preparation process of the fiber, so that the surface radix isatidis is less in the finished fiber, and the surface radix isatidis is relatively more towards the interior of the fiber.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a viscose fiber containing isatis root extract and a preparation method thereof, so as to realize the following purposes:
(1) the loss of radix isatidis microcapsules in the fiber preparation process is reduced, and the platform removal backwashing rate of a coagulation bath filter is reduced;
(2) improve the distribution uniformity of the isatis root microcapsules in the fiber.
In order to achieve the purpose of the invention, the invention adopts the technical scheme that:
a viscose fiber containing radix Isatidis extract contains radix Isatidis microcapsule 9.1-9.79%, dry breaking strength of fiber 2.70-2.75cN/dtex, wet breaking strength of fiber 1.70-1.75cN/dtex, and elongation at break of 22-23%. The bacteriostatic rate of the compound preparation on staphylococcus aureus is 99.0-99.8%, the bacteriostatic rate on candida albicans is 96.6-98.8%, the bacteriostatic rate on typhoid bacillus is 97.2-99.1%, and the compound preparation has strong inhibiting and killing effects on influenza A virus and influenza B virus;
the following is a further improvement of the above technical solution:
a preparation method of viscose fiber containing radix Isatidis extract comprises modifying radix Isatidis microcapsule; modifying the isatis root microcapsules by using a modifier solution; the modifier solution comprises, by weight, 3 parts of guar gum, 5 parts of chitosan, 1 part of polyvinyl alcohol, 30 parts of purified water and 100 parts of acetic acid.
The preparation method comprises the steps of spinning and forming; the spinning forming is carried out in an acid bath, and 3-5% of acid bath auxiliary agent solution is added into the acid bath; the acid bath assistant solution comprises the following raw material components in parts by weight: 6 parts of starch tertiary amino alkyl ether, 5 parts of quaternary ammonium starch ether, 10 parts of polyquaternary ammonium salt, 3 parts of octadecyl dimethyl benzyl ammonium chloride, 4 parts of dodecyl dimethyl benzyl ammonium chloride and 100 parts of purified water.
The polyquaternary ammonium salt is polyquaternary ammonium salt 10;
the preparation of the modifier solution comprises the following steps:
A. preparation of polyvinyl alcohol solution
Weighing the raw material components according to the formula of the modifier, putting the purified water into a stirring tank, starting stirring at the stirring speed of 1200 plus 1300r/min, simultaneously adding the polyvinyl alcohol flaky solid, heating the polyvinyl alcohol flaky solid to 95 ℃ from 25 ℃ at the speed of 5 ℃ per minute, keeping the temperature for 30min until the polyvinyl alcohol is completely dissolved, starting stirring all the time to prevent crystallization, and preparing the polyvinyl alcohol solution.
B. Preparation of Chitosan solution
Mixing chitosan and acetic acid, dissolving, and preparing to obtain 5% chitosan acetic acid solution.
C. Mixing
Placing the chitosan solution prepared in the step B into a mixing container for later use;
and (3) adding the guar gum into the polyvinyl alcohol solution prepared in the step (A), stirring and dissolving at the speed of 900-.
The preparation method of the acid bath auxiliary agent solution comprises the steps of adding purified water into a mixing tank, starting stirring at the rotation speed of 500-550r/min, then adding a mixture of starch tertiary amino alkyl ether and quaternary ammonium starch ether, wherein the feeding speed is 1-1.5 parts/min, after the feeding is finished, heating the temperature from 25 ℃ to 95 ℃ at the speed of 5 ℃ per minute, preserving the temperature for 15 minutes, cooling to 60-65 ℃, adding polyquaternary ammonium salt, octadecyl dimethyl benzyl ammonium chloride and dodecyl dimethyl benzyl ammonium chloride, uniformly stirring, cooling to 25 ℃, filtering and taking filtrate to obtain the acid bath auxiliary agent solution.
The acid bath has sulfuric acid concentration of 130-: 50-53 ℃.
Spinning and forming, and soaking and growing: 420- & lt480 mm, stretching of the nozzle: 75-85%; disc drafting of 16-21%, three-bath drafting of-2-8%, four-bath drafting of 5-11%, and spinning speed of 27-32 m/min.
The soaking is preferably: 450-: 77-83 percent; the acid bath temperature is preferably 50-52 ℃; further preferred is the immersion: 460 mm, nozzle draft: 77%; temperature of the acid bath: at 50 ℃.
The special soaking length and the nozzle drafting adopted by the invention can improve the yarn guiding speed, so that the stay time of the yarn strips in the acid bath is short; the loss of the isatis root microcapsules is reduced;
the special concentration of sulfuric acid and sodium sulfate and higher acid bath temperature are combined, so that the forming defect can be made up, and the uniformity of the distribution of the isatis root microcapsules in the fibers is ensured;
by further matching with specific inter-disc drafting, three-bath drafting, four-bath drafting and spinning speed, the effects can be realized, meanwhile, the influence of the addition of the radix isatidis on the mechanical properties of the fibers is reduced, and the prepared fibers have better mechanical properties.
When the blended spinning solution of the spinning solution and the modified isatis root microcapsule emulsion is sprayed into a coagulating bath, the methyl fiber begins to be formed and solidified.
The acid bath auxiliary agent is uniformly dispersed in the coagulating bath, and the coagulating bath uniformly repels the modified isatis root microcapsules in the blended spinning solution in the spinning forming process, so that the modified isatis root microcapsules are firmly attached to the inside or the surface of the just-formed cellulose and are uniformly distributed.
The preparation method also comprises the step of preparing the isatis root microcapsule; the preparation of the isatis root microcapsule comprises the steps of preparing a prepolymer of a melamine formaldehyde resin capsule wall material; the preparation method comprises the steps of preparing a prepolymer of the melamine formaldehyde resin capsule wall material, putting 37% of formaldehyde solution into a reaction kettle, stirring, adjusting the pH value to 7.8-8.0, and mixing the materials according to the proportion that the 37% of formaldehyde solution: adding melamine into melamine at a ratio of 4:1, heating to 65-70 ℃, stirring at 900r/min for reaction for 0.8-1.2 hours under the constant temperature condition, and preparing the melamine formaldehyde resin capsule wall material prepolymer.
In practical application, the melamine formaldehyde resin capsule wall material prepolymer enables the combination of the isatis root microcapsules and the fibers to be firmer, and can prevent the isatis root active substances on the surfaces of the fibers from losing along with water washing or friction.
The preparation of the isatis root microcapsule also comprises the preparation of isatis root emulsion; the preparation method is characterized in that the isatis root emulsion is prepared,
adding the radix Isatidis extract into a mixing container, adding emulsifier, initiator and distilled water, controlling the temperature of the mixing container at 40-45 deg.C, stirring at 1800-; wherein the mass ratio of the isatis root extract to the emulsifier to the initiator to the distilled water is 100: 5-7:1.8-2.0: 350-;
the emulsifier is Tween-20; the initiator is benzoyl peroxide.
The preparation of the isatis root microcapsule also comprises a polymerization reaction; and (2) dropwise adding the melamine formaldehyde resin capsule wall material prepolymer into the radix isatidis emulsion, stirring in a water bath at 65-70 ℃ at a rotating speed of 1500-1800r/min, dropwise adding citric acid to reduce the pH value to 3.5-4.0, acidifying for 0.5-0.8 h, heating to 80-82 ℃, reacting for 1.5-2 h, heating to 88-90 ℃, curing for 45-60 min, standing, performing suction filtration on the obtained reaction liquid, washing with ethanol and suction filtration to obtain a solid substance after the reaction is finished, washing with petroleum ether and distilled water for 1 time respectively, performing centrifugal separation, taking a precipitate, and drying at 40 ℃ to obtain the radix isatidis microcapsule.
The particle size D97 of the isatis root microcapsule is 1-2 μm.
The mass ratio of the melamine formaldehyde resin capsule wall material prepolymer to the isatis root extract is 2: 1.
And the modification of the isatis root microcapsule comprises the steps of adding the isatis root microcapsule into a modifier solution, dispersing the isatis root microcapsule into the modifier solution under the stirring state of 700-800r/min, standing for 60-80 minutes, stirring for 5-7 minutes under the condition of 300-400r/min, carrying out spray drying, and adjusting the pH value to be neutral to obtain the modified isatis root microcapsule.
The preparation method also comprises the steps of preparing the modified microcapsule emulsion; the preparation of the modified isatis root microcapsule emulsion comprises the steps of adding the modified isatis root microcapsule into ionic liquid, stirring and dispersing for 30-35 minutes at the rotating speed of 400-450r/min at the temperature of 50-53 ℃ and the pressure of-0.012-0.014 MPa, and preparing the modified isatis root microcapsule emulsion.
The ionic liquid is 1-ethyl-3-methylimidazole acetate.
The preparation method also comprises the steps of preparing the blended spinning solution; the mass ratio of the isatis root microcapsules to the alpha cellulose in the viscose stock solution in the modified isatis root microcapsule emulsion is 0.098-0.10: 1; the viscose stock solution contains 9.5-9.8% of alpha cellulose, 3.0-3.3% of total alkali, 45-50s of viscosity and 15-17ml of ripening degree.
Due to the adoption of the technical scheme, the invention achieves the technical effects that:
(1) the content of the isatis root microcapsules in the isatis root viscose fiber prepared by the invention is 9.1-9.79%, the backwashing rate of the coagulation bath filter in detaching the platform is reduced by 50-55%, the water consumption is reduced by 520 formula/day, and the isatis root in the coagulation bath crystallization product sodium sulfate decahydrate is reduced to below 110 ppm.
(2) The isatis root viscose fiber prepared by the invention has the advantages that the isatis root is uniformly distributed in the fiber; the combination of the isatis root microcapsules and the fibers is firm, so that the loss of the effective substances of the isatis root on the surfaces of the fibers along with washing or friction can be avoided; tests show that after 50 times of water washing, the loss rate of the radix isatidis on the surface of the fiber is only 2.0-2.5%.
(3) The isatis root viscose fiber prepared by the invention has the dry breaking strength of 2.70-2.75cN/dtex, the wet breaking strength of 1.70-1.75cN/dtex, the elongation at break of 22-23%, good hygroscopicity, the moisture regain of the fiber of 14-15%, and can improve the wear resistance of common viscose fiber, and the fiber density is 1.42-1.45g/cm 3.
(4) The isatis root viscose fiber prepared by the invention can effectively resist influenza A virus and influenza B virus, has higher inhibition rate on staphylococcus aureus, candida albicans and typhoid bacillus, has the inhibition rate on staphylococcus aureus of 99.0-99.8%, candida albicans of 96.6-98.8% and typhoid bacillus of 97.2-99.1%, and has strong inhibition and killing effects on influenza A virus and influenza B virus.
Detailed Description
The present invention will be described in detail with reference to examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be apparent to those skilled in the art that several modifications and improvements can be made without departing from the inventive concept. All falling within the scope of the present invention.
Example 1A method for preparing viscose fiber containing Isatis root extract
The method comprises the following steps:
(1) preparation of isatis root microcapsule
A. Preparation of isatis root emulsion
Adding the radix Isatidis extract into a mixing container, adding emulsifier, initiator and distilled water, controlling the temperature of the mixing container at 40 deg.C, stirring at 1800r/min, and stirring for 0.5 hr to form stable radix Isatidis emulsion;
wherein the mass ratio of the isatis root extract to the emulsifier to the initiator to the distilled water is 100: 5:1.8: 350;
the emulsifier is Tween-20; the initiator is benzoyl peroxide.
Preparing the melamine formaldehyde resin capsule wall material prepolymer
Adding a 37% formaldehyde solution into a reaction kettle, stirring, adjusting the pH value to 7.8, and mixing the raw materials in a proportion of the 37% formaldehyde solution: adding melamine into melamine at a ratio of 4:1, heating to 65 ℃, stirring at a constant temperature of 800r/min for reaction for 0.8 hour, and preparing the melamine formaldehyde resin capsule wall material prepolymer.
And polymerization reaction
Dropwise adding the melamine formaldehyde resin capsule wall material prepolymer into the radix isatidis emulsion, stirring at a rotating speed of 1500r/min in a 65 ℃ water bath, dropwise adding citric acid to reduce the pH to 3.5, acidifying, wherein the acidification time is 0.5 hour, heating to 80 ℃, reacting for 1.5 hours, heating to 88 ℃, solidifying for 45 minutes, standing the obtained reaction solution after the reaction is finished, carrying out suction filtration, washing with ethanol, carrying out suction filtration to obtain a solid substance, washing with petroleum ether and distilled water for 1 time respectively, carrying out centrifugal separation, taking out a precipitate, and drying at 40 ℃ to obtain the radix isatidis microcapsule.
The particle size D97 of the isatis root microcapsule is 1-2 μm.
The mass ratio of the melamine formaldehyde resin capsule wall material prepolymer to the isatis root extract is 2: 1.
In practical application, the melamine formaldehyde resin capsule wall material prepolymer enables the combination of the isatis root microcapsules and the fibers to be firmer, and can prevent the isatis root active substances on the surfaces of the fibers from losing along with water washing or friction.
(2) Modification of isatis root microcapsule
Adding the isatis root microcapsules into a modifier solution, dispersing the isatis root microcapsules in the modifier solution under the stirring state of 700r/min, standing for 60 minutes, stirring for 5 minutes under the condition of 300r/min, carrying out spray drying, and adjusting the pH value to be neutral, so that the surfaces of the isatis root microcapsules are uniformly adsorbed with cationic polysaccharide-guar gum and chitosan in the modifier to be modified, and the modified isatis root microcapsules are obtained.
The modifier solution comprises, by weight, 3 parts of guar gum, 5 parts of chitosan, 1 part of polyvinyl alcohol, 30 parts of purified water and 100 parts of acetic acid.
The polyvinyl alcohol is a flaky solid;
the preparation of the modifier solution comprises the following steps:
A. preparation of polyvinyl alcohol solution
Weighing the raw material components according to the formula of the modifier, putting purified water into a stirring tank, starting stirring at the stirring speed of 1200r/min, simultaneously adding the polyvinyl alcohol flaky solid, heating to 95 ℃ from 25 ℃ at the speed of 5 ℃ per minute, keeping the temperature for 30min until the polyvinyl alcohol is completely dissolved, starting stirring all the time to prevent crystallization, and preparing the polyvinyl alcohol solution.
B. Preparation of Chitosan solution
Mixing chitosan and acetic acid, dissolving, and preparing to obtain 5% chitosan acetic acid solution.
C. Mixing
Placing the chitosan solution prepared in the step B into a mixing container for later use;
and B, adding guar gum into the polyvinyl alcohol solution prepared in the step A, stirring and dissolving at the speed of 800r/min, preparing a mixed solution of the polyvinyl alcohol and the guar gum, slowly dropwise adding the mixed solution into a mixing container containing a chitosan acetic acid solution at the speed of 0.5 part/min, controlling the temperature of the mixing container to be 40 ℃ and the stirring speed to be 900r/min, and preserving heat for 10 minutes after dropwise adding is finished, so as to prepare a modifier solution.
(3) Preparing modified isatis root microcapsule emulsion
Adding the modified isatis root microcapsule into ionic liquid, stirring and dispersing for 30 minutes at the rotating speed of 400r/min at the temperature of 50 ℃ and the pressure of-0.012 MPa, and preparing the modified isatis root microcapsule emulsion.
(4) Preparation of blended spinning solution
Cellulose pulp is used as a raw material, a viscose stock solution is prepared by a conventional viscose preparation process, the modified isatis root microcapsule emulsion is subjected to standing and defoaming, and the defoamed isatis root microcapsule emulsion is added into the viscose stock solution by using injection equipment before spinning to prepare a blended spinning solution;
the mass ratio of the isatis root microcapsules to the alpha cellulose in the viscose stock solution in the modified isatis root microcapsule emulsion is 0.099: 1.
The viscose stock solution contains 9.5-9.8% of alpha cellulose, 3.0-3.3% of total alkali, 45-50s of viscosity and 15-17ml of ripening degree (10% of ammonium chloride value).
(5) Spinning formation
Adding the blended spinning solution into an adjusted coagulating bath for spinning, adding a 3% acid bath auxiliary agent solution into an acid bath, and uniformly stirring, wherein in the acid bath, the sulfuric acid concentration is 130g/l, the sodium sulfate concentration is 130g/l, the zinc sulfate concentration is 4g/l, and the temperature of the acid bath is as follows: 50 ℃; soaking and growing: 450 mm, nozzle draft: 77%; inter-plate drafting of 16%, three-bath drafting of-2%, four-bath drafting of 5% and spinning speed of 27 m/min.
The acid bath assistant solution comprises the following raw material components in parts by weight:
6 parts of starch tertiary amino alkyl ether, 5 parts of quaternary ammonium starch ether, 10 parts of polyquaternary ammonium salt, 3 parts of octadecyl dimethyl benzyl ammonium chloride, 4 parts of dodecyl dimethyl benzyl ammonium chloride and 100 parts of purified water.
The polyquaternary ammonium salt is polyquaternary ammonium salt 10;
the preparation method of the acid bath assistant solution comprises the following steps:
adding purified water into a mixing tank, starting stirring at the rotating speed of 500r/min, then adding a mixture of starch tertiary amino alkyl ether and quaternary ammonium starch ether at the feeding speed of 1 part/min, raising the temperature from 25 ℃ to 95 ℃ at the speed of 5 ℃ per minute after feeding, preserving the heat for 15 minutes, then cooling to 60 ℃ by using circulating cooling water, adding polyquaternary ammonium salt, octadecyl dimethyl benzyl ammonium chloride and dodecyl dimethyl benzyl ammonium chloride, uniformly stirring, cooling to 25 ℃, filtering and taking filtrate to obtain the acid bath auxiliary solution.
When the blended spinning solution of the spinning solution and the modified isatis root microcapsule emulsion is sprayed into a coagulating bath, the methyl fiber begins to be formed and solidified.
The acid bath auxiliary agent and the modified isatis root microcapsule interact with each other, so that the modified isatis root microcapsule can flow to the fibers formed by the methyl cellulose and further be uniformly attached to the surfaces of the fibers which are just formed.
(6) Post-treatment
The obtained tows are subjected to cutting, mild desulfurization process, oil bath and water washing for refining and drying to obtain the isatis root viscose fiber.
In the isatis root viscose fiber prepared in the embodiment 1 of the invention, the content of isatis root microcapsules in the fiber is 9.3%, the loss rate of the isatis root microcapsules in the preparation process is 50% lower than the bench-dismantling backwashing rate of a coagulation bath filter in the same ratio, the water consumption is reduced by 500 square/day, and the isatis root in a coagulation bath crystallization product sodium sulfate decahydrate is reduced to be less than 100 ppm.
In the isatis root viscose fiber prepared in the embodiment 1 of the invention, the isatis root is uniformly distributed in the fiber; the combination of the isatis root microcapsules and the fibers is firm, so that the loss of the effective substances of the isatis root on the surfaces of the fibers along with washing or friction can be avoided; tests show that the loss rate of the radix isatidis on the surface of the fiber is only 2.0% after 50 times of water washing.
The isatis root viscose fiber prepared in the embodiment 1 of the invention has the dry breaking strength of 2.75cN/dtex, the wet breaking strength of 1.75cN/dtex, the elongation at break of 22 percent, good hygroscopicity and the moisture regain of 15 percent, and can improve the wear resistance of common viscose fiber, and the fiber density is 1.42g/cm 3. The bacteriostatic rate of the compound preparation on staphylococcus aureus is 99.1 percent, the bacteriostatic rate on candida albicans is 96.6 percent, the bacteriostatic rate on typhoid bacillus is 97.3 percent, and the potency of the compound preparation on influenza A virus and influenza B virus is 8 by adopting an erythrocyte agglutination method for detection.
Example 2 a method for preparing viscose fiber containing isatis root extract, comprising the following steps:
(1) preparation of isatis root microcapsule
A. Preparation of isatis root emulsion
Adding the radix Isatidis extract into a mixing container, adding emulsifier, initiator and distilled water, controlling the temperature of the mixing container at 45 deg.C, stirring at 2000r/min, and stirring for 0.7 hr to form stable radix Isatidis emulsion;
wherein the mass ratio of the isatis root extract to the emulsifier to the initiator to the distilled water is 100: 7: 2.0: 370;
the emulsifier is Tween-20; the initiator is benzoyl peroxide.
Preparing the melamine formaldehyde resin capsule wall material prepolymer
Adding a 37% formaldehyde solution into a reaction kettle, stirring, adjusting the pH value to 8.0, and mixing the formaldehyde solution: adding melamine into melamine at a ratio of 4:1, heating to 70 ℃, stirring at a constant temperature of 900r/min, and reacting for 1.2 hours to prepare the melamine formaldehyde resin capsule wall material prepolymer.
And polymerization reaction
Dropwise adding the melamine formaldehyde resin capsule wall material prepolymer into the radix isatidis emulsion, stirring at a rotating speed of 1800r/min in a 70 ℃ water bath, dropwise adding citric acid to reduce the pH to 4.0, acidifying, wherein the acidification time is 0.8 h, heating to 82 ℃, reacting for 2 h, heating to 90 ℃, solidifying for 60 min, standing the obtained reaction solution after the reaction is finished, carrying out suction filtration, washing with ethanol, carrying out suction filtration to obtain a solid substance, washing with petroleum ether and distilled water for 1 time respectively, carrying out centrifugal separation, taking out the precipitate, and drying at 40 ℃ to obtain the radix isatidis microcapsule.
The particle size D97 of the isatis root microcapsule is 1-2 μm.
The mass ratio of the melamine formaldehyde resin capsule wall material prepolymer to the isatis root extract is 2: 1.
In practical application, the melamine formaldehyde resin capsule wall material prepolymer enables the combination of the isatis root microcapsules and the fibers to be firmer, and can prevent the isatis root active substances on the surfaces of the fibers from losing along with water washing or friction.
(2) Modification of isatis root microcapsule
Adding the isatis root microcapsules into a modifier solution, dispersing the isatis root microcapsules in the modifier solution under the stirring state of 800r/min, standing for 80 minutes, stirring for 7 minutes under the condition of 400r/min, carrying out spray drying, and adjusting the pH value to be neutral, so that the surfaces of the isatis root microcapsules are uniformly adsorbed with cationic polysaccharide-guar gum and chitosan in the modifier to be modified, and the modified isatis root microcapsules are obtained.
The modifier solution comprises, by weight, 3 parts of guar gum, 5 parts of chitosan, 1 part of polyvinyl alcohol, 30 parts of purified water and 100 parts of acetic acid.
The polyvinyl alcohol is a flaky solid;
the preparation of the modifier solution comprises the following steps:
A. preparation of polyvinyl alcohol solution
Weighing the raw material components according to the formula of the modifier, putting the purified water into a stirring tank, starting stirring at the stirring speed of 1300r/min, simultaneously adding the polyvinyl alcohol flaky solid, heating to 95 ℃ from 25 ℃ at the speed of 5 ℃ per minute, keeping the temperature for 30min until the polyvinyl alcohol is completely dissolved, starting stirring all the time to prevent crystallization, and preparing the polyvinyl alcohol solution.
B. Preparation of Chitosan solution
Mixing chitosan and acetic acid, dissolving, and preparing to obtain 5% chitosan acetic acid solution.
C. Mixing
Placing the chitosan solution prepared in the step B into a mixing container for later use;
and (2) adding guar gum into the polyvinyl alcohol solution prepared in the step (A), stirring and dissolving at 900r/min, preparing a mixed solution of the polyvinyl alcohol and the guar gum, slowly dropwise adding the mixed solution into a mixing container containing a chitosan acetic acid solution at the speed of 0.7 part/min, controlling the temperature of the mixing container to be 45 ℃ and the stirring speed to be 1000r/min, and preserving heat for 15 minutes after dropwise adding is finished, thus preparing the modifier solution.
(3) Preparation of modified microcapsule emulsion
Adding the modified isatis root microcapsules into ionic liquid, stirring and dispersing for 35 minutes at the rotating speed of 450r/min at the temperature of 53 ℃ and the pressure of-0.014 MPa, and preparing the modified isatis root microcapsule emulsion.
(4) Preparation of blended spinning solution
Cellulose pulp is used as a raw material, a viscose stock solution is prepared by a conventional viscose preparation process, the modified isatis root microcapsule emulsion is subjected to standing and defoaming, and the defoamed isatis root microcapsule emulsion is added into the viscose stock solution by using injection equipment before spinning to prepare a blended spinning solution;
the mass ratio of the isatis root microcapsules to the alpha cellulose in the viscose stock solution in the modified isatis root microcapsule emulsion is 0.10: 1.
The viscose stock solution contains 9.5-9.8% of alpha cellulose, 3.0-3.3% of total alkali, 45-50s of viscosity and 15-17ml of ripening degree (10% of ammonium chloride value).
(5) Spinning formation
Adding the blended spinning solution into an adjusted coagulating bath for spinning, adding a 5% acid bath auxiliary agent solution into an acid bath, and uniformly stirring, wherein in the acid bath, the sulfuric acid concentration is 137g/l, the sodium sulfate concentration is 150g/l, the zinc sulfate concentration is 6g/l, and the temperature of the acid bath is as follows: 52 ℃; soaking and growing: 470 mm, nozzle draft: 83 percent; inter-plate drafting of 21 percent, three-bath drafting of 8 percent, four-bath drafting of 11 percent and spinning speed of 32 m/min.
The special soaking length and the nozzle drafting adopted by the invention can improve the yarn guiding speed, so that the stay time of the yarn strips in the acid bath is short; reduces the loss of the isatis root microcapsules.
The invention adopts the specific concentration of the sulfuric acid and the sodium sulfate and the higher acid bath temperature, can make up the molding deficiency and ensure the uniformity of the distribution of the isatis root microcapsules in the fiber.
The acid bath assistant solution comprises the following raw material components in parts by weight:
6 parts of starch tertiary amino alkyl ether, 5 parts of quaternary ammonium starch ether, 10 parts of polyquaternary ammonium salt, 3 parts of octadecyl dimethyl benzyl ammonium chloride, 4 parts of dodecyl dimethyl benzyl ammonium chloride and 100 parts of purified water.
The polyquaternary ammonium salt is polyquaternary ammonium salt 10;
the preparation method of the acid bath assistant solution comprises the following steps:
adding purified water into a mixing tank, starting stirring at the rotation speed of 550r/min, then adding a mixture of starch tertiary amino alkyl ether and quaternary ammonium starch ether at the feeding speed of 1.5 parts/min, raising the temperature from 25 ℃ to 95 ℃ at the speed of 5 ℃ per minute after feeding, preserving the temperature for 15 minutes, then cooling to 65 ℃ by using circulating cooling water, adding polyquaternary ammonium salt, octadecyl dimethyl benzyl ammonium chloride and dodecyl dimethyl benzyl ammonium chloride, uniformly stirring, cooling to 25 ℃, filtering and taking filtrate to obtain the acid bath auxiliary agent solution.
When the blended spinning solution of the spinning solution and the modified isatis root microcapsule emulsion is sprayed into a coagulating bath, the methyl fiber begins to be formed and solidified.
The acid bath auxiliary agent is uniformly dispersed in the coagulating bath, and the coagulating bath uniformly repels the modified isatis root microcapsules in the blended spinning solution in the spinning forming process, so that the modified isatis root microcapsules are firmly attached to the inside or the surface of the just-formed cellulose and are uniformly distributed.
(6) Post-treatment
The obtained tows are subjected to cutting, mild desulfurization process, oil bath and water washing for refining and drying to obtain the isatis root viscose fiber.
The isatis root viscose fiber prepared in the embodiment 2 of the invention has the isatis root microcapsule content of 9.5 percent, the backwashing rate of the coagulation bath filter detaching table is reduced by 55 percent, the water consumption is reduced by 520 square/day, and the isatis root in the coagulation bath crystallization product sodium sulfate decahydrate is reduced to be below 110 ppm.
In the isatis root viscose fiber prepared in the embodiment 2 of the invention, the isatis root is uniformly distributed in the fiber; the combination of the isatis root microcapsules and the fibers is firm, so that the loss of the effective substances of the isatis root on the surfaces of the fibers along with washing or friction can be avoided; tests show that the loss rate of the radix isatidis on the surface of the fiber is only 2.5 percent after 50 times of water washing.
The isatis root viscose fiber prepared in the embodiment 2 of the invention has the dry breaking strength of 2.70cN/dtex, the wet breaking strength of 1.70cN/dtex, the elongation at break of 23 percent, good hygroscopicity and the moisture regain of 14 percent, and can improve the wear resistance of common viscose fiber, and the fiber density is 1.45g/cm 3. The bacteriostatic rate of staphylococcus aureus is 99.7%, the bacteriostatic rate of candida albicans is 98.5%, the bacteriostatic rate of typhoid bacillus is 98.9%, and the potency of influenza A virus and influenza B virus is 9 by adopting an erythrocyte agglutination method for detection.
EXAMPLE 3 microcapsule wall Material selection
By adopting the preparation method of the isatis root viscose fiber described in example 1, only the category of the capsule wall material in the isatis root microcapsule prepared in step (1) is changed, the viscose fibers are respectively prepared by adopting the capsule wall materials described in the following table 1, and the loss rate of the isatis root on the fiber surface after washing each group of prepared viscose fibers for 50 times is measured.
Table 1 microcapsule wall material selection
The urea-formaldehyde resin, the polystyrene, the polyisocyanate, the arabic gum and the polycarbonate are all purchased from the market, and the melamine formaldehyde resin capsule wall material prepolymer is prepared by the preparation method of the embodiment 1.
As can be seen from the results in table 1, group 3 is the most preferable choice, i.e. the melamine formaldehyde resin capsule wall material prepolymer prepared by the present invention is the most preferable capsule wall material, which makes the combination of the isatis root microcapsule and the fiber more firm, and can reduce the loss rate of the isatis root effective substance on the fiber surface with water washing or friction.
EXAMPLE 4 spin-Forming Process optimization
By adopting the preparation method of the isatis root viscose fiber described in the embodiment 1, viscose fibers are respectively prepared only by changing the immersion length, the nozzle drafting and the acid bath temperature in the spinning and forming in the step (5), the content of the isatis root microcapsules in the viscose fiber prepared by each group and the distribution of the isatis root microcapsules in the fiber are measured, the more uniform the distribution is, the higher the score is, the full score is 10, and the specific table is shown in table 2.
TABLE 2 spin-forming Process preferences
Adding the blended spinning solution into an adjusted coagulation bath for spinning, adding 3-5% of acid bath auxiliary agent solution into an acid bath, and uniformly stirring, wherein in the acid bath, the sulfuric acid concentration is 130-137g/l, the sodium sulfate concentration is 130-150g/l, the zinc sulfate concentration is 4-6g/l, and the temperature of the acid bath is as follows: 50-53 ℃; soaking and growing: 420- & lt480 mm, stretching of the nozzle: 75-85%; disc drafting of 16-21%, three-bath drafting of-2-8%, four-bath drafting of 5-11%, and spinning speed of 27-32 m/min.
TABLE 2 spin-forming Process preferences
As can be seen from the results in table 2, group 10 is most preferred, i.e. soaking: 460 mm, nozzle draft: 77%;
temperature of the acid bath: 50 ℃ is the most preferred condition.
The content of the isatis root in the viscose fiber prepared by the invention is calculated relative to the alpha fiber;
the coagulating bath is an acid bath.
Unless otherwise stated, the percentages used in the present invention are percentages by weight, and the proportions described in the present invention are proportions by mass.
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 (1)
1. A preparation method of viscose fiber containing isatis root extract is characterized by comprising the following steps: the content of the isatis root microcapsules in the viscose fibers is 9.1-9.79%, the dry breaking strength of the fibers is 2.70-2.75cN/dtex, the wet breaking strength is 1.70-1.75cN/dtex, and the elongation at break is 22-23%;
the preparation method comprises the modification of the isatis root microcapsule; modifying the isatis root microcapsules by using a modifier solution; the modifier solution comprises, by weight, 3 parts of guar gum, 5 parts of chitosan, 1 part of polyvinyl alcohol, 30 parts of purified water and 100 parts of acetic acid;
modifying the isatis root microcapsules, namely adding the isatis root microcapsules into a modifier solution, dispersing the isatis root microcapsules in the modifier solution under the stirring state of 700-800r/min, standing for 60-80 minutes, stirring for 5-7 minutes under the condition of 300-400r/min, performing spray drying, and adjusting the pH value to be neutral to obtain the modified isatis root microcapsules;
the preparation method comprises the steps of spinning and forming; the spinning forming is carried out in an acid bath, and 3-5% of acid bath auxiliary agent solution is added into the acid bath; the acid bath assistant solution comprises the following raw material components in parts by weight: 6 parts of starch tertiary amino alkyl ether, 5 parts of quaternary ammonium starch ether, 10 parts of polyquaternary ammonium salt, 3 parts of octadecyl dimethyl benzyl ammonium chloride, 4 parts of dodecyl dimethyl benzyl ammonium chloride and 100 parts of purified water;
the preparation method of the acid bath auxiliary agent solution comprises the steps of adding purified water into a mixing tank, starting stirring at the rotation speed of 500-550r/min, then adding a mixture of starch tertiary amino alkyl ether and quaternary ammonium starch ether, wherein the feeding speed is 1-1.5 parts/min, after the feeding is finished, heating the temperature from 25 ℃ to 95 ℃ at the speed of 5 ℃ per minute, preserving the temperature for 15 minutes, cooling to 60-65 ℃, adding polyquaternary ammonium salt, octadecyl dimethyl benzyl ammonium chloride and dodecyl dimethyl benzyl ammonium chloride, uniformly stirring, cooling to 25 ℃, filtering and taking filtrate to obtain the acid bath auxiliary agent solution;
the acid bath has sulfuric acid concentration of 130-: 50-53 ℃;
spinning and forming, and soaking and growing: 420- & lt480 mm, stretching of the nozzle: 75-85%; inter-disc drafting of 16-21%, three-bath drafting of-2-8%, four-bath drafting of 5-11%, and spinning speed of 27-32 m/min;
the preparation method also comprises the step of preparing the isatis root microcapsule; the preparation of the isatis root microcapsule comprises the steps of preparing a prepolymer of a melamine formaldehyde resin capsule wall material; the preparation method comprises the steps of preparing a prepolymer of the melamine formaldehyde resin capsule wall material, putting 37% of formaldehyde solution into a reaction kettle, stirring, adjusting the pH value to 7.8-8.0, and mixing the materials according to the proportion that the 37% of formaldehyde solution: adding melamine into melamine at a ratio of 4:1, heating to 65-70 ℃, stirring at 900r/min for reaction for 0.8-1.2 hours under the constant temperature condition to prepare a melamine formaldehyde resin capsule wall material prepolymer; the preparation method also comprises the steps of preparing the modified microcapsule emulsion; the preparation of the modified microcapsule emulsion comprises the steps of adding the modified radix isatidis microcapsule into ionic liquid, stirring and dispersing for 30-35 minutes at the rotating speed of 400-450r/min at the temperature of 50-53 ℃ and the pressure of-0.012-0.014 MPa to prepare the modified radix isatidis microcapsule emulsion;
the preparation method also comprises the steps of preparing the blended spinning solution; the mass ratio of the isatis root microcapsules to the alpha cellulose in the viscose stock solution in the modified isatis root microcapsule emulsion is 0.098-0.10: 1; the viscose stock solution contains 9.5-9.8% of alpha cellulose, 3.0-3.3% of total alkali, 45-50s of viscosity and 15-17ml of ripening degree.
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| CN111909507A (en) * | 2020-07-02 | 2020-11-10 | 青岛百草新材料股份有限公司 | Radix isatidis modified polyamide masterbatch for superfine fibers |
| CN111621871A (en) * | 2020-07-02 | 2020-09-04 | 中科纺织研究院（青岛）有限公司 | Radix isatidis extract modified polyamide fiber and preparation method thereof |
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