CN112796003B - Intelligent temperature-adjusting acrylic fiber with high-sensitivity heat absorption and release functions and preparation method thereof - Google Patents
Intelligent temperature-adjusting acrylic fiber with high-sensitivity heat absorption and release functions and preparation method thereof Download PDFInfo
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- CN112796003B CN112796003B CN202110027003.4A CN202110027003A CN112796003B CN 112796003 B CN112796003 B CN 112796003B CN 202110027003 A CN202110027003 A CN 202110027003A CN 112796003 B CN112796003 B CN 112796003B
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/08—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyacrylonitrile as constituent
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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
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
Abstract
The invention provides intelligent thermoregulation acrylic fiber with high-sensitivity heat absorption and release functions, wherein polyacrylonitrile accounts for 61-63% of the absolute dry finished fiber, alpha cellulose accounts for 15-20%, phase change microcapsules account for 11-21%, and heat conduction powder accounts for 1.8-8%; the invention also provides a preparation method of the fiber, which comprises the steps of preparing cellulose composite powder, preparing cellulose solution, preparing polyacrylonitrile composite powder, preparing polyacrylonitrile phase-change microcapsule composite emulsion, preparing composite spinning solution stock solution and spinning. The polyacrylonitrile fiber prepared by the invention accounts for 61-63% of the absolute dry finished fiber, the alpha cellulose accounts for 15-20%, the phase change microcapsule accounts for 11-21%, and the heat conduction powder accounts for 1.8-8%, wherein the dry strength of the fiber is not less than 3.68cN/dtex, the wet strength is not less than 2.10 cN/dtex, and the coupling strength is not less than 0.94 cN/dtex.
Description
Technical Field
The invention relates to an intelligent temperature-adjusting acrylic fiber with high-sensitivity heat absorption and discharge functions and a preparation method thereof, belonging to the technical field of acrylic fibers.
Background
Acrylic is the trade name of polyacrylonitrile fiber (PAN) in China, and is known as rayon wool. The acrylic fiber has excellent properties, such as light weight, soft and warm hand feeling, bright and firm dyeing, and moth and mildew resistance of fiber, and the acrylic fiber has the best stability on sunlight and atmospheric action in all the current synthetic fibers produced on a large scale. After one year of sunlight and atmosphere action, most of the fibers lose about 95% of the original strength, while the strength of the acrylic fiber is reduced by about 20%, and the excellent light resistance and weather resistance of the acrylic fiber can be attributed to cyano groups on macromolecules. Carbon and nitrogen atoms in the cyano group are connected by a triple bond, and the structure can absorb photons with higher energy and convert the photons into heat energy, thereby protecting main valence bonds and avoiding the degradation of macromolecules.
However, acrylic fibers have the same disadvantages of poor moisture absorption and retention as other synthetic fibers, and the electrical resistivity of conventional acrylic fibers is as high as 10 under standard conditions13Omega cm, the clothing has strong stuffy and uncomfortable feeling, thereby limiting the application of the clothing in the fields of underwear, shirts, pajamas, clothing linings, close-fitting sportswear and the like. There is a certain internal relation among moisture absorption, antistatic property and anti-pollution property of the fiber, and one of the two can be improved.
In view of the defects of the acrylic fibers, a large number of scientific researchers and engineers make good use of the defects and avoid the defects, and the acrylic fibers are modified on the premise of fully utilizing the advantages of the acrylic fibers, so that the maximum use performance is strived for.
The Chinese patent with the application number of 201010521971.2 discloses phase-change microcapsule heat-storage and temperature-regulation polyacrylonitrile fiber and a wet spinning preparation method thereof. The prepared fiber has high thermal efficiency, and has good physical and mechanical properties, wearability, processability and dyeing property; the phase-change material is paraffin wax which is already industrially produced, and has the advantage of low cost. Chinese patent with application number 201310472662.4 discloses that aqueous phase-change material microcapsule suspension, NaSCN aqueous solution and a small amount of spinning stock solution are mixed according to a certain proportion to prepare a uniform phase-change material microcapsule-containing additive, and then the pH value of the additive is adjusted to 7.0-9.0; the additive is heated to 40-45 ℃, and is directly sent into a spinning machine for spinning after being mixed with spinning solution on line through a multistage static mixer, so that brand new heat-insulating fiber with comfortable microclimate environment can be provided for human bodies. The Chinese patent with application number of 201610440883.7 discloses a protein modified acrylic fiber with phase-change temperature-regulating function, spinning solution and a preparation method thereof, which are characterized in that the protein modified acrylic fiber with phase-change temperature-regulating function is prepared by blending and copolymerizing a prepared solution of two different components and a macromolecular bridging agent, and then filtering, defoaming and aging processes
And (4) silk liquid.
The three patents are all that add phase transition thermoregulation microcapsule to the spinning fluid, wet spinning that realizes through sodium thiocyanate aqueous solution as coagulant solution, make the fibre possess according to the change of external environment and reach the function of heat absorption and release, but the acrylon has the name of artificial wool, and the rate of keeping warm is the best among the synthetic fiber, is unfavorable for the conduction of heat, therefore even only use as the next to the skin surface fabric in autumn and winter, the heat that releases when the microcapsule takes place the phase transition in the fibre is lost, has increased the stuffy sense of feeling and the gathering of static of next to the skin clothing more greatly.
Chinese patent application No. 201510634124.X discloses a method for preparing moisture-absorbing acrylon, which comprises mixing dry polyacrylonitrile powder, pore-forming agent, hydrophilic substance, additive and organic solvent, and heating to form spinning solution; spinning the spinning solution into acrylic fibers in the air through hot air, and washing and drying the obtained fibers to finally obtain the moisture absorption acrylic fibers; the Chinese patent with application number 201710105696.8 discloses a super absorbent acrylic fiber and a preparation method thereof, wherein the outer layer of the super absorbent acrylic fiber is obtained by mixing polyacrylonitrile, polyvinyl alcohol and a cross-linking agent and performing cross-linking, and the preparation steps are as follows: 1) preparing an acrylic fiber spinning solution; 2) spinning; 3) and (4) crosslinking and collecting. The patent utilizes the cross-linking effect of the cross-linking agent to form a water absorption layer which takes polyacrylonitrile and polyvinyl alcohol as main components on the surface layer of the acrylic fiber, so that the water absorption performance of the prepared acrylic fiber is greatly improved, and the water absorption capacity of the high-water-absorption acrylic fiber prepared per gram reaches more than 11.3 grams. The application number 201811186274.9 discloses an antistatic acrylic fiber and a preparation method thereof, wherein 15% of carbon nano tube, 10% of carbon black and 75% of polyacrylonitrile are mixed according to the mass ratio, and the mixture is sequentially subjected to the procedures of pre-drawing, acrylic fiber pre-drawing, roving, spinning, dipping, drying, spooling and the like, so that the produced acrylic fiber has strong antistatic performance.
The three patents improve the moisture absorption performance of the acrylic fibers or add the conductive auxiliary agent to improve the antistatic performance of the acrylic fibers, so that the comfort of acrylic fiber textiles can be relatively improved to a certain extent, the improvement effect is poor, and the acrylic fibers do not have the comfort required by the textiles close to the skin and in spring and summer.
In conclusion, acrylic fibers are called as artificial wool, the warmth retention rate is the best of synthetic fibers, heat conduction is not facilitated, phase change microcapsules are added into the acrylic fibers, when the external temperature is low, the phase change microcapsules are subjected to phase change to release heat, but the released heat is not dissipated, and the stuffiness feeling and the static aggregation of underwear are greatly increased; when the external temperature is higher, the ideal state is that the microcapsules quickly change phase, and the temperature is reduced by absorbing heat, but because the acrylic fibers are slow in heat conduction, the phase change rate of the phase change microcapsules is slow and insensitive, and the effect of quickly reducing the temperature cannot be achieved. When the applicant prepares the phase-change acrylic fiber, the heat conduction material is added, so that the heat conduction can be facilitated to a certain extent, but the defect that the heat conduction efficiency and the heat preservation time of the phase-change acrylic fiber cannot be balanced exists, namely the heat conduction efficiency is improved, so that the heat preservation time of the phase-change acrylic fiber is short.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an intelligent thermoregulation acrylic fiber with high-sensitivity heat absorption and discharge functions and a preparation method thereof, so as to realize the following purposes:
(1) the thermal conductivity of the thermoregulation acrylic fiber is improved, the instant contact cool feeling is improved, and the resistivity is reduced;
(2) meanwhile, the heat preservation time of the thermoregulation acrylic fiber is improved.
In order to solve the technical problems, the invention adopts the following technical scheme:
an intelligent thermoregulation acrylon with high-sensitivity heat absorption and discharge functions and a preparation method thereof, comprising the following steps:
1. preparation of cellulose composite powder
Mixing the crushed pulp (the granularity is less than or equal to 800 microns) with paraformaldehyde powder according to the mass ratio of 1:1.2-1.5, adding auxiliary agent magnesium sulfate powder, the mass of which is 0.1-0.3% of the weight of the pulp, adding cosolvent, the mass of which is 0.05-0.08% of the weight of the pulp, stirring for 2-3 hours at the temperature of 50 +/-2 ℃ until the pulp and the paraformaldehyde are uniformly mixed to obtain the cellulose composite powder.
The average polymerization degree of the pulp is 750-850;
the dissolution promoter consists of polyethylene glycol monolaurate-400 and hydrogenated tallow amine polyoxyethylene ether;
the mass ratio of the polyethylene glycol monolaurate-400 to the hydrogenated tallow amine polyoxyethylene ether is 2: 1;
the polyethylene glycol monolaurate-400 has a molecular weight of 400 and an HLB value of 13.1;
the paraformaldehyde is low-polymerization-degree formaldehyde HO (CH)2O)nH, wherein the content of formaldehyde is more than or equal to 92.5%, and the polymerization degree n = 8-10.
2. Preparation of cellulose solution
Slowly adding the cellulose composite powder into a dimethyl sulfoxide solvent while stirring, adding a protective dispersant at the same time, wherein the addition amount of the protective dispersant is 1-2% of the weight of the pulp, stirring for 4-6 hours at the temperature of 95-100 ℃, and filtering to obtain a cellulose solution; in the cellulose solution, the mass concentration of the cellulose composite powder is 4.1-5%;
the protective dispersant comprises polyethylene glycol 400 and sodium hexametaphosphate in a mass ratio of 2: 1.
3. Preparation of polyacrylonitrile composite powder
Mixing polyacrylonitrile powder and phase-change microcapsule powder according to a mass ratio of 3-5.5:1, adding a dispersant beta-sodium naphthalenesulfonate formaldehyde condensate, and stirring at 60 +/-2 ℃ for 3-4 hours until the materials are uniformly mixed.
The addition amount of the dispersant is 0.2 to 0.5 percent of the mass of the polyacrylonitrile powder;
the relative molecular mass of polyacrylonitrile is 80000-120000.
The phase change microcapsule comprises the following capsule core materials: n-octadecane, hexadecanol and decanoic acid in a mass ratio of 3:7: 10;
the capsule wall material consists of etherified melamine resin and polyacrylonitrile with the mass ratio of 5: 1.
The phase change material microcapsule is prepared by adopting the prior art.
4. Preparation of polyacrylonitrile phase-change microcapsule composite emulsion
Slowly adding the polyacrylonitrile composite powder into a dimethyl sulfoxide solvent while stirring, keeping the temperature and stirring for 4-6 hours at 80-90 ℃, cooling to 60 +/-2 ℃, and filtering to obtain the polyacrylonitrile phase-change microcapsule composite emulsion.
The mass ratio of the polyacrylonitrile composite powder to the dimethyl sulfoxide is 1: 4-5.
In the composite emulsion, the mass concentration of the polyacrylonitrile composite powder is 16-20%.
5. Preparation of stock solution of composite spinning solution
Mixing the prepared cellulose solution with the polyacrylonitrile phase change microcapsule composite emulsion, adding heat-conducting powder, stirring for 2 hours at the temperature of 60 +/-2 ℃ under the protection of nitrogen gas, and filtering to obtain a composite spinning solution stock solution.
6. Spinning
Metering the spinning solution stock solution by a metering pump, extruding the spinning solution stock solution by a spinning nozzle, allowing the spinning solution stock solution to enter a coagulating bath, allowing tows out of the coagulating bath to enter a preheating bath, stretching the fiber by 1-2 times in the preheating bath, allowing the tows treated by the preheating bath to enter a high-temperature water washing tank for water washing, stretching the tows in a stretching bath tank after water washing, wherein the total stretching multiple of the two times is 5-8 times, and then oiling, heat setting and cutting to obtain the finished fiber.
The mass ratio of the polyacrylonitrile to the alpha cellulose contained in the pulp is 12-13: 3-4;
the heat-conducting powder comprises mica, silicon carbide and jade powder, the mass ratio of the mica to the silicon carbide to the jade powder is 2:1:1, the particle size D90 is less than or equal to 0.9 micrometer, and the addition amount of the heat-conducting powder is 2-8% of the total weight of the alpha cellulose, the polyacrylonitrile, the heat-conducting powder and the phase-change microcapsule.
The coagulating bath comprises the following components in parts by weight: 7-9 parts of dimethyl sulfoxide, 0.5-1.0 part of isoamyl alcohol, 1-2 parts of n-butanol and 88-91.5 parts of water at the temperature of 15-20 ℃;
the preheating bath comprises the following components in parts by weight: 2-3 parts of dimethyl sulfoxide, 0.2-0.6 part of isoamyl alcohol and 0.6-1.2 parts of n-butyl alcohol at the temperature of 70-75 ℃.
Compared with the prior art, the invention has the following beneficial effects:
(1) the polyacrylonitrile fiber prepared by the invention accounts for 61-63% of the absolute dry finished fiber, the alpha cellulose accounts for 15-20%, the phase change microcapsule accounts for 11-21%, and the heat conduction powder accounts for 1.8-8%, wherein the dry strength of the fiber is not less than 3.68cN/dtex, the wet strength is not less than 2.10 cN/dtex, the bonding strength is not less than 0.94 cN/dtex, and the standard moisture regain is 8-9%.
(2) The prepared fiber has the melting enthalpy value of 20-35J/g, the melting temperature of 25-28 ℃, the crystallization enthalpy value of 19-34J/g, the crystallization temperature of 22-25 ℃, and the instant contact cooling (Q-max) of more than 0.38W/cm2The resistivity of the fiber is 10-1Omega cm-10 omega cm, and the heat conductivity of the fiber from the inside to the outside environment is 0.52-0.58W/mK at the phase transition point.
(3) The invention can improve the heat preservation time of the thermoregulation acrylic fiber.
When the external temperature is more than or equal to 25-28 ℃, the prepared fiber has phase change, absorbs heat, reduces the temperature of a local microenvironment, maintains the temperature at 25-28 ℃, and gradually reaches the environmental temperature after 2 hours at the external environmental temperature of 40 ℃.
When the external temperature is less than or equal to 22-25 ℃, the prepared fiber undergoes phase change, releases heat, improves the temperature of a local microenvironment, maintains the temperature at 22-25 ℃, and gradually reaches the environmental temperature after 2 hours at the external environmental temperature of 10 ℃.
(4) The intelligent thermoregulation acrylic fiber prepared by the invention comprises four parts of fibers, namely the polypropylene acrylic fiber, cellulose, phase change microcapsules and heat conducting powder, and has the characteristics of the acrylic fiber and the cellulose, and the phase change microcapsules and the heat conducting powder are uniformly dispersed in a macromolecular matrix formed by fusing polyacrylonitrile molecules and cellulose molecules. The fiber has excellent hygroscopicity and antistatic property, and thoroughly solves the stuffiness feeling generated by common acrylic fibers of spring and summer and underwear.
(5) The intelligent thermoregulation acrylic fiber prepared by the invention has the advantages that when the environmental temperature changes, the phase change microcapsule generates phase change, the high hygroscopicity and the heat conducting powder exist, the heat generated by the microcapsule in the fiber can be rapidly conducted, and the discomfort caused by the change of microclimate is greatly improved.
(6) The textile made of the intelligent thermoregulation acrylic fibers prepared by the invention is particularly suitable for producing underwear in summer due to the characteristics of sun-proof property, high moisture absorption and air permeability and active phase change heat absorption.
Detailed Description
Embodiment 1 Intelligent thermoregulation acrylic fiber with high-sensitivity heat absorption and release functions and preparation method thereof
The method comprises the following steps:
1. preparation of cellulose composite powder
Mixing the crushed pulp (the granularity is less than or equal to 800 microns) with paraformaldehyde powder according to the mass ratio of 1:1.2, adding auxiliary agent magnesium sulfate powder and a dissolution promoter, and stirring for 2 hours at 50 ℃ until the mixture is uniformly mixed to obtain the cellulose composite powder.
The addition amount of the auxiliary agent magnesium sulfate powder is 0.1 percent of the weight of the pulp;
the addition amount of the cosolvent is 0.05 percent of the weight of the pulp;
the average polymerization degree of the pulp is 750;
the dissolution promoter consists of polyethylene glycol monolaurate-400 and hydrogenated tallow amine polyoxyethylene ether;
the mass ratio of the polyethylene glycol monolaurate-400 to the hydrogenated tallow amine polyoxyethylene ether is 2: 1;
the polyethylene glycol monolaurate is 400, the molecular weight is 400, and the HLB value is 13.1;
the paraformaldehyde is low-polymerization-degree formaldehyde HO (CH)2O)nH, wherein the formaldehyde content is more than or equal to 92.5%, and the polymerization degree n = 8.
2. Preparation of cellulose solution
Slowly adding the cellulose composite powder into a dimethyl sulfoxide solvent while stirring, adding a protective dispersant with the mass of 1% of the weight of the pulp, keeping the temperature and stirring for 4 hours at 95 ℃, and filtering to obtain a cellulose solution with the concentration of 4.1% of the cellulose composite powder.
The protective dispersant comprises polyethylene glycol 400: the mass ratio of the sodium hexametaphosphate is 2: 1.
3. Preparation of polyacrylonitrile composite powder
Mixing polyacrylonitrile powder and phase-change microcapsule powder according to a ratio of 3:1, adding a dispersant beta-sodium naphthalene sulfonate formaldehyde condensate, wherein the addition amount of the dispersant is 0.2 percent of the mass of the polyacrylonitrile powder, and stirring for 3 hours at 60 ℃ until the mixture is uniformly mixed.
The relative molecular mass of the polyacrylonitrile was 80000.
The phase change microcapsule comprises the following capsule core materials: n-octadecane, hexadecanol and decanoic acid in a mass ratio of 3:7: 10;
the capsule wall material consists of etherified melamine resin and polyacrylonitrile with the mass ratio of 5: 1.
The phase change material microcapsule is prepared by adopting the prior art.
4. Preparation of polyacrylonitrile phase-change microcapsule composite emulsion
Slowly adding the polyacrylonitrile composite powder into a dimethyl sulfoxide solvent while stirring, keeping the temperature and stirring for 4 hours at 80 ℃, cooling to 60 ℃, and filtering to obtain the polyacrylonitrile phase change microcapsule composite emulsion.
The mass ratio of the polyacrylonitrile composite powder to the dimethyl sulfoxide is 1: 4.
In the composite emulsion, the mass concentration of the polyacrylonitrile composite powder is as follows: 20 percent.
5. Preparation of composite dope stock solution
Mixing the prepared cellulose solution with the polyacrylonitrile phase change microcapsule composite emulsion, adding heat-conducting powder, stirring for 2 hours at the temperature of 60 ℃ under the protection of nitrogen gas, and filtering to obtain a composite spinning solution stock solution.
6. Spinning
Metering a spinning solution stock solution by a metering pump, extruding the spinning solution stock solution by a spinning nozzle, allowing the spinning solution stock solution to enter a coagulating bath, allowing tows out of the coagulating bath to enter a preheating bath, stretching the fiber by 1-2 times in the preheating bath, allowing the tows treated by the preheating bath to enter a high-temperature water washing tank for water washing, stretching the tows in a stretching bath tank after water washing, wherein the total stretching multiple of the two times is 5 times, and then oiling, heat setting and cutting to obtain the finished fiber.
The mass ratio of the polyacrylonitrile to the alpha cellulose in the pulp is 12: 3;
the heat-conducting powder, mica: silicon carbide: the mass ratio of the jade powder is 2:1:1, the particle size D90 is less than or equal to 0.9 micrometer, and the addition amount of the heat-conducting powder is 2% of the total weight of the alpha cellulose, the polyacrylonitrile, the heat-conducting powder and the phase-change microcapsule.
The coagulating bath comprises the following components in parts by weight: 7 parts of dimethyl sulfoxide, 0.5 part of isoamyl alcohol and 1 part of n-butyl alcohol, wherein the temperature is 15 ℃;
the preheating bath comprises the following components in parts by weight: 2 parts of dimethyl sulfoxide, 0.2 part of isoamyl alcohol and 0.6 part of n-butyl alcohol, and the temperature is 70 ℃.
The fiber prepared in the embodiment 1 comprises 61.9% of polyacrylonitrile, 15.6% of alpha cellulose, 20.7% of phase change microcapsule and 1.8% of heat-conducting powder, wherein the dry strength of the fiber is 3.68cN/dtex, the wet strength is 2.10 cN/dtex, the bonding strength is 0.94 cN/dtex, and the standard moisture regain is 8%.
The prepared fiber has the melting enthalpy value of 30-35J/g, the melting temperature of 25-28 ℃, the crystallization enthalpy value of 32-34J/g, the crystallization temperature of 22-25 ℃, and the instant contact cooling (Q-max) of more than 0.38W/cm2And at the phase transformation point, the thermal conductivity of the fiber from the inside to the outside is 0.52W/mK.
Example 2
An intelligent thermoregulation acrylon with high-sensitivity heat absorption and discharge functions and a preparation method thereof, comprising the following steps:
1. preparation of cellulose composite powder
Mixing the crushed pulp (the granularity is less than or equal to 800 microns) with paraformaldehyde powder according to the mass ratio of 1: 1.5, adding auxiliary agent magnesium sulfate powder and a dissolution promoter, and stirring for 3 hours at the temperature of 52 ℃ until the mixture is uniformly mixed to obtain the cellulose composite powder.
The addition amount of the auxiliary agent magnesium sulfate powder is 0.3 percent of the weight of the pulp;
the addition amount of the cosolvent is 0.08 percent of the weight of the pulp;
the average polymerization degree of the pulp is 850;
the dissolution promoter consists of polyethylene glycol monolaurate-400 and hydrogenated tallow amine polyoxyethylene ether;
the mass ratio of the polyethylene glycol monolaurate-400 to the hydrogenated tallow amine polyoxyethylene ether is 2: 1;
the polyethylene glycol monolaurate is 400, the molecular weight is 400, and the HLB value is 13.1;
paraformaldehyde is formaldehyde of low degree of polymerization, HO (CH)2O)nH, wherein the formaldehyde content is more than or equal to 92.5%, and the polymerization degree n = 10.
2. Preparation of cellulose solution
Slowly adding the cellulose composite powder into a dimethyl sulfoxide solvent while stirring, adding a protective dispersant with the mass being 2% of the weight of the pulp, keeping the temperature and stirring for 6 hours at 100 ℃, and filtering to obtain a cellulose solution with the concentration of 5% of the cellulose composite powder.
The protective dispersant comprises polyethylene glycol 400 and sodium hexametaphosphate in a mass ratio of 2: 1.
3. Preparation of polyacrylonitrile composite powder
Mixing polyacrylonitrile powder and phase-change microcapsule powder at a ratio of 5.5:1, adding dispersant beta-sodium naphthalene sulfonate formaldehyde condensate with a mass fraction of 0.5% of the mass of polyacrylonitrile powder, and stirring at 60 deg.C for 4 hr until uniformly mixed.
The relative molecular mass of the polyacrylonitrile was 120000.
The phase change microcapsule comprises the following capsule core materials: n-octadecane, hexadecanol and decanoic acid in a mass ratio of 3:7: 10;
the capsule wall material consists of etherified melamine resin and polyacrylonitrile with the mass ratio of 5: 1.
The phase change material microcapsule is prepared by adopting the prior art.
4. Preparation of polyacrylonitrile phase-change microcapsule composite emulsion
Slowly adding the polyacrylonitrile composite powder into a dimethyl sulfoxide solvent while stirring, keeping the temperature and stirring for 6 hours at the temperature of 90 ℃, cooling to 60 ℃, and filtering to obtain the polyacrylonitrile phase change microcapsule composite emulsion.
The mass ratio of the polyacrylonitrile composite powder to the dimethyl sulfoxide is 1: 5.
In the composite emulsion, the mass concentration of the polyacrylonitrile composite powder is 16.7%.
5. Preparation of composite dope stock solution
Mixing the prepared cellulose solution with the polyacrylonitrile phase change microcapsule composite emulsion, adding heat-conducting powder, stirring for 2 hours at the temperature of 60 +/-2 ℃ under the protection of nitrogen gas, and filtering to obtain a composite spinning solution stock solution.
6. Spinning
Metering a spinning solution stock solution by a metering pump, extruding the spinning solution stock solution by a spinning nozzle, allowing the spinning solution stock solution to enter a coagulating bath, allowing tows out of the coagulating bath to enter a preheating bath, stretching the fiber by 1-2 times in the preheating bath, allowing the tows treated by the preheating bath to enter a high-temperature water washing tank for water washing, stretching the tows in a stretching bath tank after water washing, wherein the total stretching multiple of the two times is 8 times, and then oiling, heat setting and cutting to obtain the finished fiber.
The mass ratio of the polyacrylonitrile to the alpha cellulose in the pulp is 13: 4;
the heat-conducting powder comprises mica, silicon carbide and jade powder, the mass ratio of the mica to the silicon carbide to the jade powder is 2:1:1, the particle size D90 is less than or equal to 0.9 micrometer, and the adding amount of the heat-conducting powder is 8% of the total weight of the alpha cellulose, the polyacrylonitrile, the heat-conducting powder and the phase-change microcapsule.
The coagulating bath comprises the following components in parts by weight: 9 parts of dimethyl sulfoxide, 1.0 part of isoamyl alcohol and 2 parts of n-butyl alcohol, wherein the temperature is 20 ℃;
the preheating bath comprises the following components in parts by weight: 3 parts of dimethyl sulfoxide, 0.6 part of isoamyl alcohol and 1.2 parts of n-butyl alcohol, and the temperature is 75 ℃.
The fiber prepared in the embodiment 2 comprises 61.7% of polyacrylonitrile, 19.1% of alpha cellulose, 11.5% of phase change microcapsule and 7.7% of heat-conducting powder, wherein the dry strength of the fiber is 3.76cN/dtex, the wet strength is 2.21 cN/dtex, the bonding strength is 0.98 cN/dtex, and the standard moisture regain is 9%.
The prepared fiber has the melting enthalpy value of 23-25J/g, the melting temperature of 25-28 ℃, the crystallization enthalpy value of 22-26J/g, the crystallization temperature of 22-25 ℃, and the instant contact cooling (Q-max) of more than 0.38W/cm2And at the phase transformation point, the thermal conductivity of the fiber from the inside to the outside is 0.58W/mK.
Unless otherwise specified, the proportions used in the present invention are mass proportions, and the percentages used are mass percentages.
Claims (1)
1. A preparation method of intelligent thermoregulation acrylic fiber with high-sensitivity heat absorption and release functions is characterized by comprising the following steps: in the fiber, polyacrylonitrile accounts for 61-63% of the absolute dry finished fiber, alpha cellulose accounts for 15-20%, phase change microcapsules account for 11-21%, and heat conduction powder accounts for 1.8-8%;
the heat-conducting powder comprises mica, silicon carbide and jade powder, and the mass ratio of the mica to the silicon carbide to the jade powder is 2:1: 1;
the preparation method comprises the steps of preparing cellulose composite powder, preparing cellulose solution, preparing polyacrylonitrile composite powder, preparing polyacrylonitrile phase change microcapsule composite emulsion, preparing composite spinning solution stock solution and spinning;
the preparation method of the cellulose composite powder comprises the steps of mixing crushed pulp with paraformaldehyde powder according to the mass ratio of 1:1.2-1.5, adding auxiliary agent magnesium sulfate powder and a dissolution promoter, and stirring for 2-3 hours at 50 +/-2 ℃ until the mixture is uniformly mixed to obtain the cellulose composite powder;
the addition amount of the magnesium sulfate powder is 0.1-0.3% of the weight of the pulp; the addition amount of the dissolution accelerator is 0.05-0.08% of the weight of the pulp; the content of formaldehyde in the paraformaldehyde is more than or equal to 92.5wt%, and the polymerization degree is 8-10;
the mass concentration of the prepared cellulose solution obtained by adding dimethyl sulfoxide into the cellulose composite powder is 4.1-5%;
the preparation method comprises the following steps of (1) slowly adding polyacrylonitrile composite powder into a dimethyl sulfoxide solvent to obtain polyacrylonitrile phase change microcapsule composite emulsion with the mass concentration of the polyacrylonitrile composite powder being 16-20%; in the polyacrylonitrile composite powder, the mass ratio of polyacrylonitrile to the phase-change microcapsule is 3-5.5: 1; the relative molecular mass of the polyacrylonitrile is 80000-120000;
preparing a composite spinning solution stock solution, mixing a cellulose solution and a polyacrylonitrile phase change microcapsule composite emulsion, adding heat-conducting powder, uniformly mixing, and filtering to obtain a filtered composite spinning solution stock solution; the adding amount of the heat-conducting powder is 2-8% of the total weight of the alpha cellulose, the polyacrylonitrile, the heat-conducting powder and the phase-change microcapsule;
the mass ratio of the polyacrylonitrile to the alpha cellulose contained in the pulp is 12-13: 3-4;
in the spinning, the spinning solution stock solution enters a coagulating bath, the tows out of the coagulating bath enter a preheating bath, the fibers are stretched by 1-2 times in the preheating bath, the tows treated by the preheating bath are washed with water, the tows are stretched after washing with water, and the total stretching multiple of the two times of stretching is 5-8 times;
the coagulating bath comprises the following components in parts by weight: 7-9 parts of dimethyl sulfoxide, 0.5-1.0 part of isoamyl alcohol, 1-2 parts of n-butanol and 88-91.5 parts of water at the temperature of 15-20 ℃;
the preheating bath comprises the following components in parts by weight: 2-3 parts of dimethyl sulfoxide, 0.2-0.6 part of isoamyl alcohol and 0.6-1.2 parts of n-butyl alcohol at the temperature of 70-75 ℃.
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