CN110591067B - Preparation method and application of polyester chip with fat-reducing function - Google Patents
Preparation method and application of polyester chip with fat-reducing function Download PDFInfo
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- CN110591067B CN110591067B CN201910845328.6A CN201910845328A CN110591067B CN 110591067 B CN110591067 B CN 110591067B CN 201910845328 A CN201910845328 A CN 201910845328A CN 110591067 B CN110591067 B CN 110591067B
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- 229920000728 polyester Polymers 0.000 title claims abstract description 94
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 120
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 117
- 239000000843 powder Substances 0.000 claims abstract description 89
- 239000000835 fiber Substances 0.000 claims abstract description 65
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 62
- 230000032050 esterification Effects 0.000 claims abstract description 26
- 238000005886 esterification reaction Methods 0.000 claims abstract description 26
- 238000004537 pulping Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 229920000642 polymer Polymers 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 238000009833 condensation Methods 0.000 claims abstract description 7
- 230000005494 condensation Effects 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 78
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 48
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 40
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 34
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- 238000001354 calcination Methods 0.000 claims description 15
- FUECGUJHEQQIFK-UHFFFAOYSA-N [N+](=O)([O-])[O-].[W+4].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] Chemical compound [N+](=O)([O-])[O-].[W+4].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] FUECGUJHEQQIFK-UHFFFAOYSA-N 0.000 claims description 14
- 239000004925 Acrylic resin Substances 0.000 claims description 13
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 6
- 229910052787 antimony Inorganic materials 0.000 claims description 6
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 235000017281 sodium acetate Nutrition 0.000 claims description 6
- 239000001632 sodium acetate Substances 0.000 claims description 6
- 238000001179 sorption measurement Methods 0.000 claims description 6
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000007909 melt granulation Methods 0.000 claims 1
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- 239000004753 textile Substances 0.000 abstract description 7
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- 230000007547 defect Effects 0.000 abstract description 5
- CBACFHTXHGHTMH-UHFFFAOYSA-N 2-piperidin-1-ylethyl 2-phenyl-2-piperidin-1-ylacetate;dihydrochloride Chemical compound Cl.Cl.C1CCCCN1C(C=1C=CC=CC=1)C(=O)OCCN1CCCCC1 CBACFHTXHGHTMH-UHFFFAOYSA-N 0.000 description 22
- 239000002245 particle Substances 0.000 description 21
- 239000000047 product Substances 0.000 description 16
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- 238000012360 testing method Methods 0.000 description 8
- 230000000844 anti-bacterial effect Effects 0.000 description 7
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 6
- 229910001930 tungsten oxide Inorganic materials 0.000 description 6
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- 239000011159 matrix material Substances 0.000 description 4
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- 238000011056 performance test Methods 0.000 description 4
- -1 polyethylene terephthalate Polymers 0.000 description 4
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 229910001431 copper ion Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000003094 microcapsule Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 2
- 235000017491 Bambusa tulda Nutrition 0.000 description 2
- 241001330002 Bambuseae Species 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000011425 bamboo Substances 0.000 description 2
- 229910001451 bismuth ion Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
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- 230000001590 oxidative effect Effects 0.000 description 2
- 229920001707 polybutylene terephthalate Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 229920002215 polytrimethylene terephthalate Polymers 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000222122 Candida albicans Species 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
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- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
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- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
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- 238000003837 high-temperature calcination Methods 0.000 description 1
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- 238000001228 spectrum Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- BDPNSNXYBGIFIE-UHFFFAOYSA-J tungsten;tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[W] BDPNSNXYBGIFIE-UHFFFAOYSA-J 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Images
Classifications
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
-
- 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
-
- 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
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Polyesters Or Polycarbonates (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to the technical field of functional textile fibers, and relates to a preparation method and application of polyester chips of fat-reducing functional fibers. The method comprises the specific steps of S1, preparing functional powder; s2, putting the functional powder, terephthalic acid and ethylene glycol into a container to prepare pulping liquid; s3, carrying out pressure esterification on the pulping liquid to obtain esterified pulp; s4, carrying out normal pressure polycondensation reaction on the esterified slurry to obtain a pre-polycondensation polymer; s5, carrying out vacuum polycondensation on the pre-polycondensation to obtain a final polycondensation; and S6, carrying out melt dicing on the final condensation polymer to prepare the functional polyester chip. The invention effectively overcomes the defect of uneven heat generation caused by unbalanced dispersion of polyester chips in the prior art, improves the high-efficiency fat-reducing performance of the polyester chips of the fat-reducing functional fiber, and simultaneously ensures that the fat-reducing functional fiber prepared from the polyester chips has the high-efficiency fat-reducing and warm-keeping performance, thereby achieving the purposes of high-efficiency dispersion, uniform heating and heat preservation.
Description
Technical Field
The invention relates to the technical field of functional textile fibers, in particular to a preparation method and application of polyester chips of fat-reducing functional fibers.
Background
The polyester is a generic name of a polymer obtained by polycondensation of a polyhydric alcohol and a polybasic acid; generally, dibasic acid, dihydric alcohol and an additive are mixed into slurry and then prepared into finished polyester through a direct esterification method, wherein the finished polyester mainly refers to polyethylene terephthalate (PET), and also conventionally comprises linear thermoplastic resins such as polybutylene terephthalate (PBT), polytrimethylene terephthalate (PTT) and the like. Is one of the earliest materials used as textile raw materials and is also the first large variety of synthetic fibers in the present day. The most important advantages are good crease resistance and shape retention, and high strength. It is firm and durable, has the functions of resisting wrinkle, preventing ironing and preventing hair from sticking. The polyester fiber has many excellent textile performance and clothing performance, and has wide application. Fat reduction means that the fat in the body exceeds the normal range, and the redundant fat on the body is reduced by various means due to the health of the body. Even if a human body per se is a moving machine, the human body walks at ordinary times, energy is not generated and consumed at any moment in the working process, but the consumption amount generated in the motion process of the human body per se is far less than the intake amount.
The existing polyester fiber preparation process generally comprises the steps of firstly preparing polyester chips, and then carrying out melt spinning on the polyester chips to prepare the polyester fiber. In the prior patent CN201510841948.4, a bamboo carbon magnetic fiber layer is arranged to achieve the purpose of heating and reducing fat; patent CN201721081613.8 discloses a heating and fat-reducing fabric made of two different yarns. In the preparation process of the polyester functional layer of patent CN201510841948.4, magnetic ions in the bamboo carbon magnetic fiber layer are easy to agglomerate in the polyester process, so that the dispersibility is poor, the magnetic ions in the polyester chip are not uniformly distributed, and finally the heat generated by the polyester fiber prepared in the patent is unbalanced; in the RPET fiber coated with the copper ion layer in CN201721081613.8, in the preparation process, the copper ions are injected into the raw material, then the polyester is formed into polyester chips, and then the polyester chips are melt-spun to prepare the RPET polyester fiber with the copper ion layer. In the polyester process, the high viscosity of the polyester chip is not beneficial to the dispersion of copper particles in the polyester chip, and finally the heat generated by the RPET polyester fiber prepared by the patent is unbalanced. Obviously, the premise of preparing the fat-reducing functional fiber with uniform heat-generating performance is to prepare a polyester chip capable of uniformly dispersing heat-generating functional ions.
Disclosure of Invention
In view of the above, the invention provides a preparation method and an application of a polyester chip with a fat-reducing function fiber, so as to solve the defect of uneven heat generation caused by uneven dispersion of the polyester chip in the prior art.
The invention discloses a preparation method of a polyester chip of fat-reducing functional fiber, which comprises the following steps:
s1, preparing functional powder;
s2, putting the functional powder, terephthalic acid and ethylene glycol into a container, and adding a catalyst, an ether inhibitor and an antioxidant for pulping to prepare pulping liquid; in step S2, the catalyst is specifically antimony glycol, the ether inhibitor is specifically sodium acetate, and the antioxidant is specifically triphenyl phosphate; the molar ratio of the terephthalic acid to the ethylene glycol is 1: 1.05-1: 1.25; the mass ratio of the functional powder to the glycol is 1: 50-1: 200; the mass fraction of the catalyst relative to the terephthalic acid is 0.05%; the mass fraction of the ether inhibitor relative to the terephthalic acid is 0.05 percent; the mass fraction of the antioxidant relative to the terephthalic acid is 0.05 percent; the specific beating condition of the step S2 is that the pressure is 100KPa, the beating temperature is 80 ℃, the beating time is 15min, and the beating speed is 200 r/min.
S3, carrying out pressurization esterification on the pulping liquid to obtain esterified pulp, wherein in the pressurization esterification process, the pressure is 0.35-0.45 MPa, the esterification temperature is 230-245 ℃, and the esterification time is 2.5-3.0 h;
s4, carrying out normal pressure polycondensation reaction on the esterified slurry to obtain a pre-polycondensation product, wherein the pressure of the normal pressure polycondensation reaction is 100KPa, the normal pressure polycondensation temperature is 250-260 ℃, and the normal pressure polycondensation time is 0.5-1.5 h;
s5, carrying out vacuum polycondensation on the pre-polycondensation to obtain a final polycondensation; the vacuum polycondensation reaction of the step S5 includes a low vacuum polycondensation reaction and a high vacuum polycondensation reaction, wherein the step S5 specifically includes performing a low vacuum polycondensation reaction on the pre-polycondensation product, and then performing a high vacuum polycondensation reaction to obtain a final polycondensation product; the vacuum degree of the low vacuum polycondensation reaction is 500-5000 Pa, and the time of the low vacuum polycondensation reaction is 0.5-1.0 h; the vacuum degree of the high vacuum polycondensation reaction is 50-100 Pa, and the time of the low vacuum polycondensation reaction is 1.0-3.0 h;
and S6, carrying out melt dicing on the final condensation polymer to prepare the functional polyester chip.
As a preferred embodiment of the present invention, the specific content of step S1 includes:
S11, firstly, dissolving bismuth nitrate powder in an ethylene glycol solution to prepare a bismuth nitrate solution for later use; in the step S11, the mass fraction of the bismuth nitrate in the bismuth nitrate solution is 5-15%;
s12, dispersing polyacrylic resin in an ethylene glycol solution, and stirring with ammonia water to dissolve the polyacrylic resin in the ethylene glycol solution to prepare a polyacrylic acid mixed solution; in the step S12, the mass fraction of polyacrylic acid in the polyacrylic acid mixed solution is 5-15%;
s13, adding potassium iodide into the polyacrylic acid mixed solution, dissolving, and obtaining a functional powder precursor solution after the solution is clarified; in the step S13, the mass fraction of potassium iodide in the functional powder precursor solution is 5 to 15%;
s14, dropwise adding the bismuth nitrate solution prepared in the step S1 into the functional powder precursor solution under ultrasonic and rapid stirring to perform ultrasonic stirring reaction for several hours; in the step S14, the volume ratio of the functional powder precursor solution to the bismuth nitrate solution is 1:0.25 to 1: 0.50;
s15, adding tungsten nitrate powder, carrying out dissolving and adsorption reaction, continuously carrying out ultrasonic stirring reaction for a plurality of hours, filtering, and washing with deionized water for a plurality of times to obtain filter residue; in the step S15, the addition amount of the tungsten nitrate powder is 5-10% of the mass fraction of the functional powder precursor solution;
S16, calcining the filter residue in an aerobic environment at 450-750 ℃ for several hours, and then calcining in an aerobic environment at 800-1000 ℃ to prepare the functional powder.
The invention also discloses an application of the polyester chip of the fat-reducing functional fiber, wherein the prepared polyester chip of the fat-reducing functional fiber is applied to the fat-reducing functional fiber, the heat insulation performance of a sample of the fat-reducing functional fiber prepared by using the polyester chip of the fat-reducing functional fiber is radiated for 1min at 100 ℃ (15cm), the temperature difference between the front surface and the rear surface of the sample of the fat-reducing functional fiber before heating is 1.0-2.0 ℃, and the surface temperature of a fabric is more than 100 ℃.
The technical scheme shows that the invention has the beneficial effects that: oxidizing bismuth nitrate by using potassium iodide to form bismuth oxyiodide particles with hollow structures, and then passivating and coating the surfaces of the bismuth oxyiodide particles by using polyacrylic acid to form bismuth oxyiodide capsule particles with hollow microcapsule structures; then dissolving and adsorbing the tungsten nitrate powder particles into bismuth oxyiodide capsule particles, thereby effectively and uniformly dispersing the spherical hollow-structure bismuth oxyiodide capsule particles on the surface of the functional fiber polyester chip, therefore, the polyester chip has excellent heating and heat-insulating properties due to low addition, so that the polyester chip with the fat-reducing function can directly and uniformly generate heat through spherical bismuth oxyiodide capsule particles with a hollow structure, the defect of uneven heat generation caused by uneven dispersion of the polyester chip in the prior art is effectively overcome, the problem of low fat-reducing efficiency caused by uneven heat generation of the polyester chip with the fat-reducing function is solved, the high-efficiency fat-reducing performance of the polyester chip with the fat-reducing function is improved, meanwhile, the fat-reducing functional fiber prepared from the polyester chips has the performance of efficient fat reduction and heat preservation, and the purposes of efficient dispersion, uniform heating and heat preservation are achieved.
Drawings
FIG. 1 is an XRD spectrum of a functional powder prepared by the present invention;
FIG. 2 is a scanning electron microscope image of the functional powder prepared by the present invention;
FIG. 3 is a sectional electron microscope atlas of the polyester chip of the fat-reducing functional fiber prepared by the invention;
FIG. 4 is a photograph showing a three-dimensional curling shape of a polyester chip made of a fat-reducing functional fiber according to the present invention;
Detailed Description
The following examples are intended to illustrate the invention in further detail, but are not intended to limit the invention in any way, and unless otherwise indicated, the reagents, methods and apparatus used in the invention are conventional in the art, and are not intended to limit the invention in any way.
Example 1: the invention discloses a preparation method of a polyester chip of a fat-reducing functional fiber, which comprises the following steps:
s1, preparing functional powder; the specific content of step S1 includes: s11, firstly, dissolving bismuth nitrate powder in an ethylene glycol solution to prepare a bismuth nitrate solution for later use; in the step S11, the mass fraction of bismuth nitrate in the bismuth nitrate solution is 15%; s12, dispersing polyacrylic resin in an ethylene glycol solution, and stirring with ammonia water to dissolve the polyacrylic resin in the ethylene glycol solution to prepare a polyacrylic acid mixed solution; in the step S12, the mass fraction of polyacrylic acid in the polyacrylic acid mixed solution is 15%; s13, adding potassium iodide into the polyacrylic acid mixed solution, dissolving, and obtaining a functional powder precursor solution after the solution is clarified; in the step S13, the mass fraction of potassium iodide in the functional powder precursor solution is 15%; s14, dropwise adding the bismuth nitrate solution prepared in the step S1 into the functional powder precursor solution under ultrasonic and rapid stirring to perform ultrasonic stirring reaction for 4 hours; in the step S14, the volume ratio of the functional powder precursor solution to the bismuth nitrate solution is 1: 0.50; s15, adding tungsten nitrate powder, carrying out dissolving and adsorption reaction, continuously carrying out ultrasonic stirring reaction for 4 hours, filtering, and washing for 3 times by using deionized water to obtain filter residue; in the step S15, the addition amount of the tungsten nitrate powder is 10% by mass of the functional powder precursor solution; and S16, calcining the filter residue in an aerobic environment at 650 ℃ for 3 hours, and then calcining in an aerobic environment at 900 ℃ for 15min to obtain the functional powder.
S2, putting the functional powder, terephthalic acid and ethylene glycol into a container, and adding a catalyst, an ether inhibitor and an antioxidant for pulping to prepare pulping liquid; in step S2, the catalyst is specifically antimony glycol, the ether inhibitor is specifically sodium acetate, and the antioxidant is specifically triphenyl phosphate; the molar ratio of terephthalic acid to ethylene glycol is 1: 1.25; the mass ratio of the functional powder to the glycol is 1: 50; the mass fraction of the catalyst relative to the terephthalic acid is 0.05 percent; the mass fraction of the ether inhibitor relative to the terephthalic acid is 0.05 percent; the mass fraction of the antioxidant relative to the terephthalic acid is 0.05 percent; the specific pulping condition of step S2 is that the pressure is 100KPa, the pulping temperature is 80 ℃, the pulping time is 15min, and the pulping speed is 200 r/min.
S3, carrying out pressurization esterification on the pulping liquid to obtain esterified pulp, wherein in the pressurization esterification process, the pressure is 0.45MPa, the esterification temperature is 245 ℃, and the esterification time is 3.0 h;
s4, carrying out normal pressure polycondensation reaction on the esterified slurry to obtain a pre-polycondensation product, wherein the pressure of the normal pressure polycondensation reaction is 100KPa, the normal pressure polycondensation temperature is 260 ℃, and the normal pressure polycondensation time is 1.5 h;
S5, carrying out vacuum polycondensation on the pre-polycondensation to obtain a final polycondensation; the vacuum polycondensation reaction of the step S5 includes a low vacuum polycondensation reaction and a high vacuum polycondensation reaction, wherein the step S5 specifically includes performing a low vacuum polycondensation reaction on the pre-polycondensation product, and then performing a high vacuum polycondensation reaction to obtain a final polycondensation product; the vacuum degree of the low vacuum polycondensation reaction is 5000Pa, and the time of the low vacuum polycondensation reaction is 1.0 h; the vacuum degree of the high vacuum polycondensation reaction is 100Pa, and the time of the low vacuum polycondensation reaction is 3.0 h;
and S6, carrying out melt dicing on the final condensation polymer to prepare the functional polyester chip.
The invention also discloses an application of the polyester chip of the fat-reducing functional fiber, and the prepared polyester chip of the fat-reducing functional fiber is applied to the fat-reducing functional fiber.
Example 2: the invention discloses a preparation method of a polyester chip of fat-reducing functional fiber, which comprises the following steps:
s1, preparing functional powder; the specific content of step S1 includes: s11, firstly, dissolving bismuth nitrate powder in an ethylene glycol solution to prepare a bismuth nitrate solution for later use; in the step S11, the mass fraction of bismuth nitrate in the bismuth nitrate solution is 5%; s12, dispersing polyacrylic resin in an ethylene glycol solution, and stirring with ammonia water to dissolve the polyacrylic resin in the ethylene glycol solution to prepare a polyacrylic acid mixed solution; in the step S12, the mass fraction of polyacrylic acid in the polyacrylic acid mixed solution is 5%; s13, adding potassium iodide into the polyacrylic acid mixed solution, dissolving, and obtaining a functional powder precursor solution after the solution is clarified; in the step S13, the mass fraction of potassium iodide in the functional powder precursor solution is 5%; s14, dropwise adding the bismuth nitrate solution prepared in the step S1 into the functional powder precursor solution under ultrasonic and rapid stirring to perform ultrasonic stirring reaction for 4 hours; in the step S14, the volume ratio of the functional powder precursor solution to the bismuth nitrate solution is 1: 0.25; s15, adding tungsten nitrate powder, carrying out dissolving and adsorption reaction, continuously carrying out ultrasonic stirring reaction for 4 hours, filtering, and washing for 3 times by using deionized water to obtain filter residue; in the step S15, the addition amount of the tungsten nitrate powder is 5% by mass of the functional powder precursor solution; and S16, calcining the filter residue in an aerobic environment at 650 ℃ for 3 hours, and then calcining in an aerobic environment at 900 ℃ for 15min to obtain the functional powder.
S2, putting the functional powder, terephthalic acid and ethylene glycol into a container, and adding a catalyst, an ether inhibitor and an antioxidant for pulping to prepare pulping liquid; in step S2, the catalyst is specifically antimony glycol, the ether inhibitor is specifically sodium acetate, and the antioxidant is specifically triphenyl phosphate; the molar ratio of the terephthalic acid to the ethylene glycol is 1: 1.05; the mass ratio of the functional powder to the glycol is 1: 200; the mass fraction of the catalyst relative to the terephthalic acid is 0.05 percent; the mass fraction of the ether inhibitor relative to the terephthalic acid is 0.05 percent; the mass fraction of the antioxidant relative to the terephthalic acid is 0.05 percent; the specific beating condition of the step S2 is that the pressure is 100KPa, the beating temperature is 80 ℃, the beating time is 15min, and the beating speed is 200 r/min.
S3, carrying out pressurization esterification on the pulping liquid to obtain esterified pulp, wherein in the pressurization esterification process, the pressure is 0.45MPa, the esterification temperature is 245 ℃, and the esterification time is 2.5 h;
s4, carrying out normal pressure polycondensation reaction on the esterified slurry to obtain a pre-polycondensation product, wherein the pressure of the normal pressure polycondensation reaction is 100KPa, the normal pressure polycondensation temperature is 260 ℃, and the normal pressure polycondensation time is 0.5 h;
S5, carrying out vacuum polycondensation on the pre-polycondensation to obtain a final polycondensation; the vacuum polycondensation reaction of the step S5 includes a low vacuum polycondensation reaction and a high vacuum polycondensation reaction, wherein the step S5 specifically includes performing a low vacuum polycondensation reaction on the pre-polycondensation product, and then performing a high vacuum polycondensation reaction to obtain a final polycondensation product; the vacuum degree of the low vacuum polycondensation reaction is 5000Pa, and the time of the low vacuum polycondensation reaction is 0.5 h; the vacuum degree of the high vacuum polycondensation reaction is 100Pa, and the time of the low vacuum polycondensation reaction is 1.0 h;
and S6, carrying out melt dicing on the final condensation polymer to prepare the functional polyester chip.
The invention also discloses an application of the polyester chip of the fat-reducing functional fiber, and the prepared polyester chip of the fat-reducing functional fiber is applied to the fat-reducing functional fiber.
Example 3: the invention discloses a preparation method of a polyester chip of fat-reducing functional fiber, which comprises the following steps:
s1, preparing functional powder; the specific content of step S1 includes: s11, firstly, dissolving bismuth nitrate powder in an ethylene glycol solution to prepare a bismuth nitrate solution for later use; in the step S11, the mass fraction of bismuth nitrate in the bismuth nitrate solution is 7.5%; s12, dispersing polyacrylic resin in an ethylene glycol solution, and stirring with ammonia water to dissolve the polyacrylic resin in the ethylene glycol solution to prepare a polyacrylic acid mixed solution; in the step S12, the mass fraction of polyacrylic acid in the polyacrylic acid mixed solution is 7.5%; s13, adding potassium iodide into the polyacrylic acid mixed solution, dissolving, and obtaining a functional powder precursor solution after the solution is clarified; in the step S13, the mass fraction of potassium iodide in the functional powder precursor solution is 7.5%; s14, dropwise adding the bismuth nitrate solution prepared in the step S1 into the functional powder precursor solution under ultrasonic and rapid stirring to perform ultrasonic stirring reaction for 4 hours; in the step S14, the volume ratio of the functional powder precursor solution to the bismuth nitrate solution is 1: 0.35; s15, adding tungsten nitrate powder, carrying out dissolving and adsorption reaction, continuously carrying out ultrasonic stirring reaction for 4 hours, filtering, and washing for 3 times by using deionized water to obtain filter residue; in the step S15, the addition amount of the tungsten nitrate powder is 7.5% by mass of the functional powder precursor solution; and S16, calcining the filter residue in an aerobic environment at 650 ℃ for 2.5 hours, and then calcining in an aerobic environment at 900 ℃ for 15min to obtain the functional powder.
S2, putting the functional powder, terephthalic acid and ethylene glycol into a container, and adding a catalyst, an ether inhibitor and an antioxidant for pulping to prepare pulping liquid; in step S2, the catalyst is specifically antimony glycol, the ether inhibitor is specifically sodium acetate, and the antioxidant is specifically triphenyl phosphate; the molar ratio of terephthalic acid to ethylene glycol is 1: 1.25; the mass ratio of the functional powder to the glycol is 1: 100; the mass fraction of the catalyst relative to the terephthalic acid is 0.05%; the mass fraction of the ether inhibitor relative to the terephthalic acid is 0.05 percent; the mass fraction of the antioxidant relative to the terephthalic acid is 0.05 percent; the specific beating condition of the step S2 is that the pressure is 100KPa, the beating temperature is 80 ℃, the beating time is 15min, and the beating speed is 200 r/min.
S3, carrying out pressurization esterification on the pulping liquid to obtain esterified pulp, wherein in the pressurization esterification process, the pressure is 0.45MPa, the esterification temperature is 245 ℃, and the esterification time is 2.5 h;
s4, carrying out normal pressure polycondensation reaction on the esterified slurry to obtain a pre-polycondensation product, wherein the pressure of the normal pressure polycondensation reaction is 100KPa, the normal pressure polycondensation temperature is 260 ℃, and the normal pressure polycondensation time is 1.0 h;
S5, carrying out vacuum polycondensation on the pre-polycondensation to obtain a final polycondensation; the vacuum polycondensation reaction of the step S5 includes a low vacuum polycondensation reaction and a high vacuum polycondensation reaction, wherein the step S5 specifically includes performing a low vacuum polycondensation reaction on the pre-polycondensation product, and then performing a high vacuum polycondensation reaction to obtain a final polycondensation product; the vacuum degree of the low vacuum polycondensation reaction is 5000Pa, and the time of the low vacuum polycondensation reaction is 1.0 h; the vacuum degree of the high vacuum polycondensation reaction is 100Pa, and the time of the low vacuum polycondensation reaction is 2.0 h;
and S6, carrying out melt dicing on the final condensation polymer to prepare the functional polyester chip.
The invention also discloses an application of the polyester chip of the fat-reducing functional fiber, and the prepared polyester chip of the fat-reducing functional fiber is applied to the fat-reducing functional fiber.
Example 4: the invention discloses a preparation method of a polyester chip of fat-reducing functional fiber, which comprises the following steps:
s1, preparing functional powder; the specific content of step S1 includes: s11, firstly, dissolving bismuth nitrate powder in an ethylene glycol solution to prepare a bismuth nitrate solution for later use; in the step S11, the mass fraction of bismuth nitrate in the bismuth nitrate solution is 15%; s12, dispersing polyacrylic resin in an ethylene glycol solution, and stirring with ammonia water to dissolve the polyacrylic resin in the ethylene glycol solution to prepare a polyacrylic acid mixed solution; in the step S12, the mass fraction of polyacrylic acid in the polyacrylic acid mixed solution is 5%; s13, adding potassium iodide into the polyacrylic acid mixed solution, dissolving, and obtaining a functional powder precursor solution after the solution is clarified; in the step S13, the mass fraction of potassium iodide in the functional powder precursor solution is 10%; s14, dropwise adding the bismuth nitrate solution prepared in the step S1 into the functional powder precursor solution under ultrasonic and rapid stirring to perform ultrasonic stirring reaction for 4 hours; in the step S14, the volume ratio of the functional powder precursor solution to the bismuth nitrate solution is 1: 0.25; s15, adding tungsten nitrate powder, carrying out dissolving and adsorption reaction, continuously carrying out ultrasonic stirring reaction for 4 hours, filtering, and washing for 3 times by using deionized water to obtain filter residue; in the step S15, the addition amount of the tungsten nitrate powder is 5% by mass of the functional powder precursor solution; and S16, calcining the filter residue in an aerobic environment at 650 ℃ for 2.5 hours, and then calcining in an aerobic environment at 900 ℃ for 15min to obtain the functional powder.
S2, putting the functional powder, terephthalic acid and ethylene glycol into a container, and adding a catalyst, an ether inhibitor and an antioxidant for pulping to prepare pulping liquid; in step S2, the catalyst is specifically antimony glycol, the ether inhibitor is specifically sodium acetate, and the antioxidant is specifically triphenyl phosphate; the molar ratio of terephthalic acid to ethylene glycol is 1: 1.25; the mass ratio of the functional powder to the glycol is 1: 75; the mass fraction of the catalyst relative to the terephthalic acid is 0.05 percent; the mass fraction of the ether inhibitor relative to the terephthalic acid is 0.05 percent; the mass fraction of the antioxidant relative to the terephthalic acid is 0.05 percent; the specific beating condition of the step S2 is that the pressure is 100KPa, the beating temperature is 80 ℃, the beating time is 15min, and the beating speed is 200 r/min.
S3, carrying out pressurization esterification on the pulping liquid to obtain esterified pulp, wherein in the pressurization esterification process, the pressure is 0.45MPa, the esterification temperature is 245 ℃, and the esterification time is 2.5 h;
s4, carrying out normal pressure polycondensation reaction on the esterified slurry to obtain a pre-polycondensation product, wherein the pressure of the normal pressure polycondensation reaction is 100KPa, the normal pressure polycondensation temperature is 260 ℃, and the normal pressure polycondensation time is 1.5 h;
S5, carrying out vacuum polycondensation on the pre-polycondensation to obtain a final polycondensation; the vacuum polycondensation reaction of the step S5 includes a low vacuum polycondensation reaction and a high vacuum polycondensation reaction, wherein the step S5 specifically includes performing a low vacuum polycondensation reaction on the pre-polycondensation product, and then performing a high vacuum polycondensation reaction to obtain a final polycondensation product; the vacuum degree of the low vacuum polycondensation reaction is 5000Pa, and the time of the low vacuum polycondensation reaction is 0.5 h; the vacuum degree of the high vacuum polycondensation reaction is 100Pa, and the time of the low vacuum polycondensation reaction is 2.0 h;
and S6, carrying out melt dicing on the final condensation polymer to prepare the functional polyester chip.
The invention also discloses an application of the polyester chip of the fat-reducing functional fiber, and the prepared polyester chip of the fat-reducing functional fiber is applied to the fat-reducing functional fiber.
Comparative example 1: far infrared fiber polyester chip.
Performance test of the polyester chips of fat-reducing functional fiber prepared in examples 1 to 4 and the polyester chips of far infrared fiber used in comparative example 1
1. According to GB/T30127-2013 textile far infrared performance detection and evaluation, far infrared performance tests are carried out on the cloth prepared from the polyester chip with the fat reducing function disclosed in the embodiments 1-4 of the invention and the cloth prepared from the polyester chip with the far infrared fiber used in the comparative example 1, and the test results are shown in Table 1.
TABLE 1 far infrared Performance test results
According to the test results in the table 1, the far infrared emissivity of the polyester chip with the fat reducing function produced by the production method of the invention reaches more than 92%, the far infrared radiation temperature rise value is more than 1.9 ℃, the far infrared emissivity exceeds the technical requirements of textile materials on far infrared performance test, namely, the far infrared emissivity is more than or equal to 88%, and the far infrared radiation temperature rise value is more than or equal to 1.4 ℃, so that the polyester chip has the effects of heat preservation and far infrared emission and absorption; and the far infrared wavelength range is close to the wavelength of the human body, and the emitted far infrared is absorbed by the human body, so that the blood circulation and the metabolism of the human body can be promoted, the immunity of the human body is improved, and the health is benefited. Obviously, the polyester chip with the fat reducing function prepared by the technical scheme in the embodiment 1 of the invention has better effects of heat preservation and far infrared emission and absorption, and can achieve the purpose of efficiently preparing the high-performance heat preservation, bacteriostasis and fat reducing functional polyester chip.
2. According to GB/T20944.3-2008, evaluation of antibacterial performance of textiles part 3: the cloth prepared from the polyester chips of fat-reducing functional fibers disclosed in examples 1 to 4 of the present invention and the cloth prepared from the polyester chips of far infrared fibers used in comparative example 1 were subjected to the antibacterial effect test of staphylococcus aureus (AATCC6538), escherichia coli (AATCC8739) and candida albicans (AATCC10231), and the test results are shown in table 2.
TABLE 2 antibacterial Property test results
According to the test results in table 2, the cloth of the polyester chip with fat-reducing function produced by the production method of the invention has the integral bacteriostasis rate of 92%, 98% for staphylococcus aureus, 97% for escherichia coli and higher than that of the cloth of the polyester chip with far infrared fiber produced by the comparative example 1; bismuth oxyiodide has excellent antibacterial and catalytic effects, is widely applied to preparation of antibacterial powder, but has large antibacterial activity per se, so that the bismuth oxyiodide is difficult to be added and dispersed in situ in a polymer, and is difficult to be applied to a polyester matrix; obviously, in the preparation method and the application of the polyester chip with the fat-reducing function fiber disclosed by the invention, the technical scheme can effectively apply bismuth oxyiodide to the polyester matrix, so that bismuth oxyiodide capsule particles with a hollow microcapsule structure can be quickly, efficiently and uniformly dispersed and distributed on the polyester matrix of polyacrylic resin, the defect of poor performance caused by uneven dispersion of functional fiber powder on the matrix in the prior art is overcome, and the purpose of efficiently preparing the polyester chip with the heat-preserving, bacterium-inhibiting and fat-reducing function fiber is achieved.
3. According to GB/T3362-.
TABLE 3 results of the elasticity test
According to the test results in table 3, the tensile strength of the cloth of the polyester chip of the fat-reducing functional fiber produced by the production method of the invention is obviously improved, and the air permeability of the cloth is stronger than that of the common functional cloth. Obviously, the cloth of the polyester chip with the fat-reducing functional fiber prepared by the embodiment of the invention not only has good heat preservation and bacteriostasis performance, but also has good elastic recovery rate, and the cloth can utilize the heat generated by the polyester chip with the fat-reducing functional fiber to stimulate the human body to consume fat so as to generate more heat, and meanwhile, the cloth can also utilize the elastic structure of the functional fiber prepared by the polyester chip with the fat-reducing functional fiber to achieve the purpose of keeping the human body curve through the elasticity of the functional fiber.
In the invention, firstly, bismuth nitrate reacts with potassium iodide to generate bismuth oxyiodide, then tungsten ions are introduced to the bismuth oxyiodide, and the bismuth oxyiodide antibacterial agent is loaded with tungsten oxide powder through calcination in an aerobic environment, so that the functional powder has an antibacterial effect and a far infrared emission function. In the reaction process, polyacrylic acid is mainly dispersed into small balls through emulsification, an ammonium polyacrylate salt solution is formed on the surface of polyacrylic acid through the pH regulation of ammonia water, bismuth ions in bismuth nitrate in an alkaline environment are complexed with amino groups, then potassium iodide and the bismuth ions react to generate bismuth oxyiodide microspheres, tungsten hydroxide precipitate is loaded on the surfaces of the bismuth oxyiodide microspheres through complexation and precipitation, after the reaction is finished, the polyacrylic acid in a core layer can be removed through high-temperature calcination, and meanwhile, the loading of tungsten oxide with a far infrared emission function on the bismuth oxyiodide microspheres is realized through the regulation of a calcination process, so that the problems that conventional loaded microsphere particles are too large, the stability of tungsten oxide in the powder is poor, and the particle size of functional powder is large and the dispersibility is poor are solved. The aerobic environment set in step S16 is mainly for complete decomposition of polyacrylic acid, so as to avoid the residue of polyacrylic acid from affecting the color of the functional powder, and the distributed pyrolysis is mainly decomposition of polyacrylic acid at low temperature, and is mainly beneficial to formation of tungsten oxide at high temperature. In addition, the specific proportion of each product is mainly used for regulating the proportion of the core layer and the shell layer, the core layer contains excessive polyacrylic acid, the particle size of the polyacrylic acid is too large, the subsequent wall layer is thin, the wall is easy to break during calcination, spherical complete functional powder is difficult to form, the core layer is too few, the wall layer is thick, the particle size process of the wall layer is caused, the wall layer crushing pressure is increased during subsequent processing, the wall layer is difficult to crush and uniformly disperse in the melt spinning process, the content of tungsten oxide powder is too low, the far infrared effect of the tungsten oxide powder is poor, the color is excessively bluish, and the particle size of the powder is increased.
Obviously, as shown in fig. 1 to 4, the bismuth oxyiodide capsule particles with hollow structures are formed by oxidizing bismuth nitrate with potassium iodide, and then the surfaces of the bismuth oxyiodide particles are passivated and coated with polyacrylic acid to form the bismuth oxyiodide capsule particles with hollow microcapsule structures; then dissolving and adsorbing the tungsten nitrate powder particles into bismuth oxyiodide capsule particles, thereby effectively and uniformly dispersing the spherical hollow-structure bismuth oxyiodide capsule particles on the surface of the functional fiber polyester chip, therefore, the polyester chip has excellent heating and heat-insulating properties due to low addition, so that the polyester chip with the fat-reducing function can directly and uniformly generate heat through spherical bismuth oxyiodide capsule particles with a hollow structure, the defect of uneven heat generation caused by uneven dispersion of the polyester chip in the prior art is effectively overcome, the problem of low fat-reducing efficiency caused by uneven heat generation of the polyester chip with the fat-reducing function is solved, the high-efficiency fat-reducing performance of the polyester chip with the fat-reducing function is improved, meanwhile, the fat-reducing functional fiber prepared from the polyester chips has the performance of efficient fat reduction and heat preservation, and the purposes of efficient dispersion, uniform heating and heat preservation are achieved.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments can be referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (5)
1. The preparation method of the fiber polyester chip is characterized by comprising the following steps:
S1, preparing functional powder; the specific content of step S1 includes:
s11, firstly, dissolving bismuth nitrate powder in an ethylene glycol solution to prepare a bismuth nitrate solution for later use;
s12, dispersing polyacrylic resin in an ethylene glycol solution, and stirring with ammonia water to dissolve the polyacrylic resin in the ethylene glycol solution to prepare a polyacrylic acid mixed solution;
s13, adding potassium iodide into the polyacrylic acid mixed solution, dissolving, and obtaining a functional powder precursor solution after the solution is clarified;
s14, dropwise adding the bismuth nitrate solution prepared in the step S1 into the functional powder precursor solution under ultrasonic and rapid stirring to perform ultrasonic stirring reaction for several hours;
s15, adding tungsten nitrate powder, carrying out dissolving and adsorption reaction, continuously carrying out ultrasonic stirring reaction for a plurality of hours, filtering, and washing with deionized water for a plurality of times to obtain filter residue;
s16, calcining the filter residue in an aerobic environment at 450-750 ℃ for several hours, and then calcining in an aerobic environment at 800-1000 ℃ to prepare functional powder;
s2, putting the functional powder, terephthalic acid and ethylene glycol into a container, and adding a catalyst, an ether inhibitor and an antioxidant for pulping to prepare pulping liquid;
S3, carrying out pressurization esterification on the pulping liquid to obtain esterified pulp, wherein in the pressurization esterification process, the pressure is 0.35-0.45 MPa, the esterification temperature is 230-245 ℃, and the esterification time is 2.5-3.0 h;
s4, carrying out normal pressure polycondensation reaction on the esterified slurry to obtain a pre-polycondensation product, wherein the pressure of the normal pressure polycondensation reaction is 100KPa, the normal pressure polycondensation temperature is 250-260 ℃, and the normal pressure polycondensation time is 0.5-1.5 h;
s5, carrying out vacuum polycondensation on the pre-polycondensation to obtain a final polycondensation;
s6, carrying out melt granulation on the final condensation polymer to prepare a functional polyester chip;
in the step S11, the mass fraction of the bismuth nitrate in the bismuth nitrate solution is 5-15%;
in the step S12, the mass fraction of polyacrylic acid in the polyacrylic acid mixed solution is 5-15%; in the step S13, the mass fraction of potassium iodide in the functional powder precursor solution is 5 to 15%; in the step S14, the volume ratio of the functional powder precursor solution to the bismuth nitrate solution is 1:0.25 to 1: 0.50; in the step S15, the addition amount of the tungsten nitrate powder is 5-10% of the mass fraction of the functional powder precursor solution;
In step S2, the catalyst is specifically antimony glycol, the anti-etherizing agent is specifically sodium acetate, and the antioxidant is specifically triphenyl phosphate;
in step S2, the molar ratio of terephthalic acid to ethylene glycol is 1: 1.05-1: 1.25; the mass ratio of the functional powder to the glycol is 1: 50-1: 200.
2. The method of claim 1, wherein in step S2, the mass fraction of the catalyst relative to the terephthalic acid is 0.05%; the mass fraction of the ether inhibitor relative to the terephthalic acid is 0.05 percent; the antioxidant was 0.05% by mass relative to terephthalic acid.
3. The method for preparing polyester fiber chips as claimed in claim 2, wherein the specific beating conditions of step S2 are 100KPa, 80 deg.C, 15min and 200 r/min.
4. The method of claim 3, wherein the vacuum polycondensation reaction of step S5 includes a low vacuum polycondensation reaction and a high vacuum polycondensation reaction, and wherein step S5 is to perform the low vacuum polycondensation reaction on the pre-polycondensation product and then perform the high vacuum polycondensation reaction to obtain the final polycondensation product.
5. The method for preparing polyester fiber chips as claimed in claim 4, wherein the degree of vacuum of the low vacuum polycondensation reaction of step S5 is 500-5000 Pa, and the time of the low vacuum polycondensation reaction is 0.5-1.0 h; the vacuum degree of the high vacuum polycondensation reaction in the step S5 is 50-100 Pa, and the time of the low vacuum polycondensation reaction is 1.0-3.0 h.
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