CN115928246A - Preparation method of polyester staple fibers - Google Patents
Preparation method of polyester staple fibers Download PDFInfo
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- CN115928246A CN115928246A CN202211441124.4A CN202211441124A CN115928246A CN 115928246 A CN115928246 A CN 115928246A CN 202211441124 A CN202211441124 A CN 202211441124A CN 115928246 A CN115928246 A CN 115928246A
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- 229920000728 polyester Polymers 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 244000060011 Cocos nucifera Species 0.000 claims abstract description 43
- 235000013162 Cocos nucifera Nutrition 0.000 claims abstract description 43
- 239000000843 powder Substances 0.000 claims abstract description 40
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- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 29
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229940119177 germanium dioxide Drugs 0.000 claims abstract description 15
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
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- 239000002131 composite material Substances 0.000 claims abstract description 14
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- 239000000203 mixture Substances 0.000 claims abstract description 10
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- IHJUECRFYCQBMW-UHFFFAOYSA-N 2,5-dimethylhex-3-yne-2,5-diol Chemical compound CC(C)(O)C#CC(C)(C)O IHJUECRFYCQBMW-UHFFFAOYSA-N 0.000 claims abstract description 7
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- 239000004917 carbon fiber Substances 0.000 claims description 40
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- 238000006243 chemical reaction Methods 0.000 claims description 32
- 239000004408 titanium dioxide Substances 0.000 claims description 26
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
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- 238000000034 method Methods 0.000 claims description 21
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- 238000000151 deposition Methods 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 229920001634 Copolyester Polymers 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 10
- 238000005886 esterification reaction Methods 0.000 claims description 10
- 238000009998 heat setting Methods 0.000 claims description 10
- 238000010926 purge Methods 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
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- 239000005020 polyethylene terephthalate Substances 0.000 description 4
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- SWGJCIMEBVHMTA-UHFFFAOYSA-K trisodium;6-oxido-4-sulfo-5-[(4-sulfonatonaphthalen-1-yl)diazenyl]naphthalene-2-sulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(N=NC3=C4C(=CC(=CC4=CC=C3O)S([O-])(=O)=O)S([O-])(=O)=O)=CC=C(S([O-])(=O)=O)C2=C1 SWGJCIMEBVHMTA-UHFFFAOYSA-K 0.000 description 2
- QPYKYDBKQYZEKG-UHFFFAOYSA-N 2,2-dimethylpropane-1,1-diol Chemical compound CC(C)(C)C(O)O QPYKYDBKQYZEKG-UHFFFAOYSA-N 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
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- 240000007594 Oryza sativa Species 0.000 description 1
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- 244000082204 Phyllostachys viridis Species 0.000 description 1
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- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- FJJCIZWZNKZHII-UHFFFAOYSA-N [4,6-bis(cyanoamino)-1,3,5-triazin-2-yl]cyanamide Chemical compound N#CNC1=NC(NC#N)=NC(NC#N)=N1 FJJCIZWZNKZHII-UHFFFAOYSA-N 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
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- 229920002678 cellulose Polymers 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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- Artificial Filaments (AREA)
Abstract
The invention relates to a preparation method of polyester staple fibers, wherein a designed composite functional additive is a mixture of silicon dioxide, germanium dioxide, aluminum oxide and surface-modified aluminum-doped zinc oxide powder, so that the polyester staple fibers can obtain a good far infrared emission function and further obtain good heat preservation performance, and the heat preservation performance can be further improved by matching with the design of the particle size of the powder; the added dimethyl propylene glycol, 2,5-dimethyl-2,5-hexynediol, 2-butene-1,4-di-n-butyl ester and di (hexane-1,6-diol) titanium ensure that the prepared polyester staple fiber has good heat retention property, breaking strength and moisture regain; the coconut carbon can absorb and emit far infrared rays with the wavelength of 4-14 mu m, and then arouse to form negative ions beneficial to a body, can enable the surface of the fiber to generate a porous water seepage surface layer, can dissolve skin sweat, guarantees dryness and comfort while keeping warm, and avoids bacterial breeding.
Description
Technical Field
The invention relates to the technical field of spinning, in particular to a preparation method of polyester staple fibers.
Background
The polyester staple fiber is obtained by spinning polyester (polyethylene terephthalate, PET for short, polymerized by PTA and MEG) into a tow and cutting the tow. PET is in the shape of rice grains or flakes, and has various colors (usually, polyester is the main component which is contacted with many beverage bottles, and the PET can be sliced into polyester staple fibers by two main processes of pre-spinning and post-spinning, and the polyester staple fibers can be cut into the polyester staple fibers with different specifications in the post-spinning according to different requirements.
The Chinese patent with the publication number of CN109252242B discloses a polyester staple fiber and a preparation method thereof, wherein the designed composite functional additive is a mixture of silicon dioxide, germanium dioxide, aluminum oxide and aluminum-doped zinc oxide powder with modified surface, and the mass ratio is designed, so that the polyester staple fiber can obtain good far infrared emission function, and further obtain good heat preservation performance, and the design of the particle size of the powder can be matched to further improve the heat preservation performance.
The coconut charcoal fiber belongs to a novel environment-friendly material, and after the melon pulp and coconut water of coconut are taken away and produced and processed into food, the great pressure is generated on environmental remediation by the coarse coconut shell waste. However, people purchase the coconut shells of waste, can utilize the waste, and finally obtain the cellulose of the coconut shells by soaking, hammering, filtering and airing: and heating the coconut fiber to 1200 ℃, and carbonizing at high temperature to obtain the coconut charcoal with excellent characteristics. The molecular formula of the coconut charcoal is hexagonal, the charcoal is inseparable in density, large in relative density and more in pores, the total area of the microporous plate is more than 4 times of that of the bamboo charcoal, and the coconut charcoal has a strong adsorption function.
In the prior art, although a formula of coconut charcoal fiber as a fabric is disclosed, for example, a Chinese patent with an authorization publication number of CN106435944B discloses a novel antibacterial fabric, and a specific preparation method of the novel antibacterial fabric is to use pearl fiber; wool fibers; corn protein fiber; modal fibers; coconut charcoal fiber; tea fibers; adding a dispersing agent, a binder and a softening agent into the antibacterial finishing agent at 40-45 ℃, adding 100-120 parts of water, mixing and stirring uniformly, and then airing and forming; then the mixture is made into functional yarn strips through blowing, opening, drawing, roving and spinning; then the functional yarn strips adopt knitting or weaving process cloth. Therefore, in the prior art, the carbon fiber is mixed with other fiber materials and then is made into yarn according to the traditional spinning process of blowing, opening, drawing, roving and spun yarn, and is not combined with the melt spinning technology of polyester fiber for application; because the color of the coconut carbon fiber is dark black and the dyeing property of the coconut carbon fiber is poor, the color of the coconut carbon fiber in the yarn or the shell fabric using the coconut carbon fiber in the market is gray black, so that the application range is limited.
Based on the prior art, it is urgently needed to provide a preparation method of polyester staple fibers, so that the prepared polyester staple fibers have the advantages of warm keeping, dryness, comfort and antibiosis, and can have more various colors.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: it is urgently needed to provide a preparation method of polyester staple fibers, so that the prepared polyester staple fibers have the advantages of warm keeping, dryness, comfort and antibiosis, and can have more various colors.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of polyester staple fibers comprises the following steps:
step 1: preparing coconut charcoal fiber superfine powder;
step 2: placing the coconut carbon fiber superfine powder into a reaction vessel of atomic deposition equipment, wherein the reaction temperature is 100-110 ℃;
and step 3: feeding titanium tetraisopropoxide steam into a continuously stirred reaction container, wherein the feeding duration of the titanium tetraisopropoxide steam is 8s, purging the reaction container with nitrogen for 20s, feeding deionized water into the reaction container at intervals, wherein the feeding duration of the deionized water is 8s, and purging the reaction container with nitrogen for 20s;
repeating the step 3 for n times, wherein n is any value between 5 and 10000, so that a layer of titanium dioxide film is deposited on the surface of the coconut carbon fiber superfine powder;
and 4, step 4: mixing 300 parts by weight of terephthalic acid and 50 parts by weight of an organic solvent (ethanol or isopropanol) at 50-60 ℃; then heating to 150-160 ℃ for esterification reaction, wherein the reaction time is 10-15min;
and 5: adding 60-0.005n parts by weight of the carbon fiber superfine powder with the titanium dioxide film deposited on the surface, which is obtained in the step (3), into a product after the esterification reaction; then adding 8-10 parts by weight of dimethylpropanediol, 5-10 parts by weight of 2,5-dimethyl-2,5-hexynediol, 5-15 parts by weight of 2-butene-1,4-di-n-butyl ester, 5-10 parts by weight of bis (hexane-1,6-diol) titanium, 5-10 parts by weight of a composite functional additive, 100 parts by weight of terephthalic acid and 50 parts by weight of glycol ester, heating to 200-250 ℃, and reacting under the vacuum condition of 200-300Pa for 10-15min to perform a first polymerization reaction; adding 90-0.007n of the carbon fiber superfine powder with the titanium dioxide film deposited on the surface, obtained in the step 3, in parts by weight, reacting for 5-10min at 230-260 ℃ under the vacuum condition of 250-350Pa, and carrying out a second polymerization reaction to obtain a copolyester melt; the composite functional additive is a mixture of silicon dioxide, germanium dioxide, aluminum oxide and surface-modified aluminum-doped zinc oxide powder, and the mass ratio of the silicon dioxide to the germanium dioxide to the aluminum oxide to the surface-modified aluminum-doped zinc oxide powder is 1 (2-4) to 1 (2-4) in sequence;
step 6: carrying out melt spinning on the copolyester melt to obtain a melt, wherein the spinning temperature is 270-290 ℃;
and 7: extruding the melt through a profiled spinneret plate to form melt trickle, and cooling, wherein the spinneret micropores of the spinneret plate are gear-shaped;
and 8: and (3) carrying out yarn guiding, heat setting and winding forming on the melt trickle extruded and cooled by the spinneret plate to obtain the polyester staple fiber.
Preferably, in the preparation method of the polyester staple fiber, the step 1 specifically comprises: heating the coconut shell fiber to 1200 ℃, carbonizing in a vacuum environment, and micronizing the carbonized fiber to obtain the coconut charcoal fiber superfine powder.
Preferably, in the preparation method of the polyester staple fiber, the particle size of the silicon dioxide, germanium dioxide, aluminum oxide and surface-modified aluminum-doped zinc oxide powder is 10-30 micrometers.
Preferably, in the preparation method of the polyester staple fiber, the number of teeth of the spinneret micropores of the spinneret plate is 6-8.
Preferably, in the preparation method of the polyester staple fiber, the diameter of the spinning micropores of the spinneret plate is 0.4-0.6mm in a gear shape, and the tooth height of the gear shape is 0.05-0.1mm.
Preferably, in the preparation method of the polyester staple fiber, the step 8 is specifically: feeding the filament bundle after being oiled and collected by the nozzle into a lower godet with the speed of 3105-3610m/min, and then feeding the filament bundle into a hot guide wire roller with the speed of 3105-3610m/min and the temperature of 120-135 ℃ for heat setting; and winding and forming at a winding speed of 3100-3600m/min to obtain the polyester staple fibers.
Preferably, in the above method for preparing coconut charcoal polyester fiber, the cooling in step 7 specifically comprises: solidifying into strands by adopting a side-blowing cooling process; the conditions of the side-blown cooling process are as follows: the speed of the cross air blow is 0.30m/s-0.50m/s, the temperature of the cross air blow is 18 ℃, and the humidity of the cross air blow is 75 percent.
The invention also protects the polyester staple fiber product prepared by the preparation method of the polyester staple fiber.
The invention has the beneficial effects that:
the method for preparing the coconut carbon fiber superfine powder and depositing titanium tetraisopropoxide on the surface of the coconut carbon fiber superfine powder ensures that a titanium dioxide film is uniformly deposited on the surface of the coconut carbon fiber superfine powder by utilizing the surface deposit of the coconut carbon fiberAt the oxygen-containing functional group such as-OH and-COOH, the growth characteristics of the titanium dioxide film can be effectively started, firstly, titanium tetraisopropoxide is introduced, and the-OCH (CH) is formed on the surface of the coconut carbon fiber through the self-limiting chemical reaction of the active group of the oxygen-containing functional group on the surface of the coconut carbon fiber 3 ) 2 And introduce H 2 O and-OCH (CH) 3 ) 2 The reaction formed a monolayer of titanium dioxide film and exposed-OH, with the remainder being purged with nitrogen after each step. The required thickness of the titanium dioxide film can be adjusted by the number of repeated cycles;
the surface of the coconut carbon fiber can present different colors by adjusting the thickness of the titanium dioxide film. In the melt extrusion spinning process, a certain amount of coconut carbon fiber powder with a titanium dioxide film is sequentially added in the second polymerization reaction, and the amount of the added coconut carbon fiber powder in the second polymerization reaction is larger than that of the added coconut carbon fiber powder in the first polymerization reaction, so that the coconut carbon fiber powder and the polymer can be more uniformly mixed, and the coconut carbon fibers can be uniformly distributed when melt extrusion is performed to form melt trickle; in each polymerization reaction, the addition amount of the coconut carbon fiber is properly adjusted according to the selection of the deposition times of the titanium dioxide of the coconut carbon fiber, namely the film thickness, so that the coconut carbon fiber can be stably added in the polymerization reaction.
The composite functional additive is designed to be a mixture of silicon dioxide, germanium dioxide, aluminum oxide and surface-modified aluminum-doped zinc oxide powder, and the mass ratio is designed, so that the polyester staple fibers can obtain a good far infrared emission function, and further obtain good heat preservation performance, and the heat preservation performance can be further improved by matching with the design of the particle size of the powder; the added dimethyl propylene glycol, 2,5-dimethyl-2,5-hexynediol, 2-butene-1,4-di-n-butyl ester and bis (hexane-1,6-diol) titanium can be used as regulators for controlling the molecular structure of the polymer obtained after polymerization reaction, and the composite functional additive can be used in cooperation, so that the prepared polyester staple fiber is promoted to have good heat retention property, breaking strength and moisture regain; the coconut charcoal has various mineral contents. The coconut charcoal can absorb and emit far infrared rays with the wavelength of 4-14 mu m, and then arouse to form negative ions beneficial to a body, and because other raw materials of the polyester staple fiber have the heat preservation performance, the surface layer of porous seepage water can be generated on the surface of the fiber by matching with the coconut charcoal fiber, the skin sweat can be dissolved, and the rapid diffusion and evaporation can be realized, so that the dryness and comfort can be ensured while the heat preservation is realized, and the bacterial breeding can be avoided.
The coconut carbon fiber surface has different colors due to different deposition thicknesses of titanium dioxide, for example, when n is 200, the surface of the coconut carbon fiber surface has a light yellow color when the deposition thickness of the titanium dioxide is 20nm, for example, when n is 400, the surface of the coconut carbon fiber surface has a purple red color when the deposition thickness of the titanium dioxide is 40nm, for example, when n is 600, the surface of the coconut carbon fiber has a bluish purple color when the deposition thickness of the titanium dioxide is 60 nm. The color of the coconut carbon fiber can be selected according to the requirements of subsequent polyester staple fibers or subsequent cloth dyeing, so that the prepared polyester staple fibers meet the processing requirements of different colors.
Detailed Description
The following description will be given with reference to the embodiments in order to explain the technical contents, the objects and the effects of the present invention in detail.
Example 1
A preparation method of polyester staple fibers comprises the following steps:
step 1: heating the fiber of the coconut shell to 1200 ℃, carbonizing the coconut shell in a vacuum environment, and micronizing the carbonized fiber to obtain coconut charcoal fiber superfine powder, wherein the particle size of the coconut charcoal fiber superfine powder is 15 microns;
step 2: placing the coconut carbon fiber superfine powder into a reaction container of atomic deposition equipment, wherein the reaction temperature is 105 ℃;
and step 3: feeding titanium tetraisopropoxide steam into a continuously stirred reaction container, wherein the feeding duration of the titanium tetraisopropoxide steam is 8s, purging the reaction container with nitrogen for 20s, feeding deionized water into the reaction container at intervals, wherein the feeding duration of the deionized water is 8s, and purging the reaction container with nitrogen for 20s;
repeating the step 3 for 200 times to deposit a layer of titanium dioxide film with the thickness of 20nm on the surface of the coconut charcoal fiber superfine powder, so that the surface of the coconut charcoal fiber is light yellow;
and 4, step 4: mixing 300kg of terephthalic acid and 50kg of an organic solvent (ethanol or isopropanol) at 50-60 ℃; then heating to 155 ℃ for esterification reaction, wherein the reaction time is 102min;
and 5: adding 59.9kg of carbon fiber superfine powder with a titanium dioxide film deposited on the surface, which is obtained in the step 3, into a product after the esterification reaction; then adding 9kg of dimethyl propylene glycol, 7kg of 2,5-dimethyl-2,5-hexynediol, 5-15kg of 2-butene-1,4-di-n-butyl ester, 7kg of bis (hexane-1,6-diol) titanium, 7kg of composite functional additive, 100kg of terephthalic acid and 50kg of ethylene glycol ester, heating to 220 ℃, reacting for 12min under the vacuum condition of 250Pa, and carrying out first polymerization reaction; adding 89.86kg of carbon fiber superfine powder with the titanium dioxide film deposited on the surface, obtained in the step 3, reacting for 7min at 245 ℃ under the vacuum condition of 300Pa, and carrying out second polymerization reaction to obtain a copolyester melt; the composite functional additive is a mixture of silicon dioxide, germanium dioxide, aluminum oxide and surface-modified aluminum-doped zinc oxide powder, the mass ratio of the silicon dioxide to the germanium dioxide to the aluminum oxide to the surface-modified aluminum-doped zinc oxide powder is 1;
and 6: carrying out melt spinning on the copolyester melt to obtain a melt, wherein the spinning temperature is 280 ℃;
and 7: extruding the melt through a profiled spinneret to form melt trickle, and cooling, wherein the spinneret micropores of the spinneret are gear-shaped, and the number of teeth is 7; the cooling specifically comprises the following steps: solidifying into strands by adopting a side-blowing cooling process; the conditions of the side-blown cooling process are as follows: the speed of the cross air blow is 0.30m/s-0.50m/s, the temperature of the cross air blow is 18 ℃, and the humidity of the cross air blow is 75 percent;
and step 8: carrying out yarn guiding, heat setting and winding forming on the melt trickle extruded and cooled by the spinneret plate, and specifically comprising the following steps of: the filament bundles after being oiled and collected by the nozzle are input into a lower filament guide disc at the speed of 3410m/min, and then enter a hot filament guide roller at the speed of 3410m/min and at the temperature of 130 ℃ for heat setting; and winding and forming at a winding speed of 3400m/min to obtain the polyester staple fiber.
Example 2
A preparation method of polyester staple fibers comprises the following steps:
step 1: heating the fiber of the coconut shell to 1200 ℃, carbonizing the coconut shell in a vacuum environment, and micronizing the carbonized fiber to obtain coconut charcoal fiber superfine powder, wherein the particle size of the coconut charcoal fiber superfine powder is 10 microns;
and 2, step: placing the coconut carbon fiber superfine powder into a reaction container of atomic deposition equipment, wherein the reaction temperature is 100 ℃;
and 3, step 3: feeding titanium tetraisopropoxide steam into a continuously stirred reaction vessel, wherein the feeding duration of the titanium tetraisopropoxide steam is 8s, purging the reaction vessel with nitrogen for 20s, and then feeding the reaction vessel with deionized water at intervals, wherein the feeding duration of the deionized water is 8s, and purging the reaction vessel with nitrogen for 20s;
repeating the step 3 for 400 times to deposit a layer of titanium dioxide film with the thickness of 40nm on the surface of the coconut charcoal fiber superfine powder so that the coconut charcoal fiber surface is purple red;
and 4, step 4: mixing 300kg of terephthalic acid and 50kg of an organic solvent (ethanol or isopropanol) at 50 ℃; then heating to 150 ℃ for esterification reaction, wherein the reaction time is 10min;
and 5: adding 59.8kg of carbon fiber superfine powder with a titanium dioxide film deposited on the surface, which is obtained in the step 3, into a product after esterification reaction; then adding 8kg of dimethyl propylene glycol, 5kg of 2,5-dimethyl-2,5-hexynediol, 5kg of 2-butene-1,4-di-n-butyl ester, 5kg of titanium bis (hexane-1,6-diol), 5kg of composite functional additive, 100kg of terephthalic acid and 50kg of glycol ester, heating to 200 ℃, and reacting for 10min under the vacuum condition of 200Pa to perform first polymerization reaction; then 89.72kg of carbon fiber superfine powder with titanium dioxide films deposited on the surfaces, which is obtained in the step 3, is added, and the mixture reacts for 5min at 230 ℃ under the vacuum condition of 250Pa, and a second polymerization reaction is carried out to obtain a copolyester melt; the composite functional additive is a mixture of silicon dioxide, germanium dioxide, aluminum oxide and surface-modified aluminum-doped zinc oxide powder, the mass ratio of the silicon dioxide to the germanium dioxide to the aluminum oxide to the surface-modified aluminum-doped zinc oxide powder is 1;
step 6: carrying out melt spinning on the copolyester melt to obtain a melt, wherein the spinning temperature is 270 ℃;
and 7: extruding the melt through a profiled spinneret to form melt trickle, and cooling, wherein the spinneret micropores of the spinneret are gear-shaped, and the number of teeth is 6; the cooling specifically comprises the following steps: solidifying into strands by adopting a side-blowing cooling process; the conditions of the side-blown cooling process are as follows: the speed of cross air blowing is 0.30-0.50 m/s, the temperature of the cross air blowing is 18 ℃, and the humidity of the cross air blowing is 75 percent;
and step 8: carrying out yarn guiding, heat setting and winding forming on the melt trickle extruded and cooled by the spinneret plate, and specifically comprising the following steps: the filament bundles after being oiled and gathered by the nozzle are input into a lower godet with the speed of 3105m/min and then enter a hot wire roller with the speed of 3105m/min and the temperature of 120 ℃ for heat setting; winding and molding at a winding speed of 3100m/min to obtain the polyester staple fibers; obtaining the polyester staple fiber.
Example 3
A preparation method of polyester staple fibers comprises the following steps:
step 1: heating the coconut shell fiber to 1200 ℃, carbonizing in a vacuum environment, and micronizing the carbonized fiber to obtain coconut charcoal fiber superfine powder, wherein the particle size of the coconut charcoal fiber superfine powder is 20 microns;
step 2: placing the coconut carbon fiber superfine powder into a reaction container of atomic deposition equipment, wherein the reaction temperature is 100-110 ℃;
and step 3: feeding titanium tetraisopropoxide steam into a continuously stirred reaction container, wherein the feeding duration of the titanium tetraisopropoxide steam is 8s, purging the reaction container with nitrogen for 20s, feeding deionized water into the reaction container at intervals, wherein the feeding duration of the deionized water is 8s, and purging the reaction container with nitrogen for 20s;
repeating the step 3 for 600 times to deposit a layer of titanium dioxide film with the thickness of 60nm on the surface of the coconut charcoal fiber superfine powder so that the surface of the coconut charcoal fiber is blue-purple;
and 4, step 4: mixing 300kg of terephthalic acid and 50kg of an organic solvent (ethanol or isopropanol) at 60 ℃; then heating to 160 ℃ for esterification reaction, wherein the reaction time is 15min;
and 5: adding 59.7kg of carbon fiber superfine powder with a titanium dioxide film deposited on the surface, which is obtained in the step 3, into a product after the esterification reaction; then adding 10kg of dimethyl propylene glycol, 10kg of 2,5-dimethyl-2,5-hexynediol, 15kg of 2-butene-1,4-di-n-butyl ester, 10kg of bis (hexane-1,6-diol) titanium, 10kg of composite functional additive, 100kg of terephthalic acid and 50kg of ethylene glycol ester, heating to 250 ℃, reacting for 15min under the vacuum condition of 300Pa, and carrying out first polymerization reaction; adding 89.58kg of the carbon fiber superfine powder with the titanium dioxide film deposited on the surface obtained in the step 3, reacting for 10min at 260 ℃ under 350Pa vacuum, and carrying out second polymerization reaction to obtain a copolyester melt; the composite functional additive is a mixture of silicon dioxide, germanium dioxide, aluminum oxide and surface-modified aluminum-doped zinc oxide powder, the mass ratio of the silicon dioxide to the germanium dioxide to the aluminum oxide to the surface-modified aluminum-doped zinc oxide powder is 1;
step 6: carrying out melt spinning on the copolyester melt to obtain a melt, wherein the spinning temperature is 290 ℃;
and 7: extruding the melt through a profiled spinneret to form melt trickle, and cooling, wherein the spinneret micropores of the spinneret are gear-shaped, and the number of teeth is 8; the cooling specifically comprises the following steps: solidifying into strands by adopting a side-blowing cooling process; the conditions of the side-blown cooling process are as follows: the speed of the cross air blow is 0.30m/s-0.50m/s, the temperature of the cross air blow is 18 ℃, and the humidity of the cross air blow is 75 percent;
and 8: carrying out yarn guiding, heat setting and winding forming on the melt trickle extruded and cooled by the spinneret plate, and specifically comprising the following steps: the filament bundle after being oiled and collected by the nozzle is input into a lower godet with the speed of 3610m/min and then enters a hot guide wire roller with the speed of 3610m/min and the temperature of 135 ℃ for heat setting; and (3) winding and forming at a winding speed of 3600m/min to obtain the polyester staple fibers.
And (3) performance testing:
1. according to GB/T6503-2008, the breaking strength and the moisture regain of the polyester staple fibers obtained in examples 1-3 are respectively tested, and the test results are shown in Table 1;
TABLE 1
| Test group | Breaking strength (cN/dtex) | Moisture regain (%) |
| Example 1 | 4.9 | 1.9 |
| Example 2 | 4.6 | 1.7 |
| Example 3 | 4.8 | 1.8 |
As can be seen from table 1, the breaking strength and moisture regain of the polyester staple fibers obtained in examples 1 to 3 both meet the standard requirements.
2. The polyester staple fibers obtained in examples 1 to 3 were respectively spun into fabrics, and then far infrared performance tests were respectively performed, and the test results are shown in table 2.
TABLE 2
| Test group | Normal emissivity | Standard requirement for normal emissivity | Conclusion |
| Example 1 | 0.98 | ≥0.80 | Qualified |
| Example 2 | 0.97 | ≥0.80 | Qualified |
| Example 3 | 0.96 | ≥0.80 | Qualified |
According to table 2, the normal emissivity of the fabrics spun by the polyester staple fibers obtained in examples 1 to 3 is greater than the standard requirement, and the fabrics have the function of keeping warm.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical field are included in the scope of the present invention.
Claims (8)
1. The preparation method of the polyester staple fiber is characterized by comprising the following steps of:
step 1: preparing coconut charcoal fiber superfine powder;
step 2: placing the coconut carbon fiber superfine powder into a reaction vessel of atomic deposition equipment, wherein the reaction temperature is 100-110 ℃;
and step 3: feeding titanium tetraisopropoxide steam into a continuously stirred reaction vessel, wherein the feeding duration of the titanium tetraisopropoxide steam is 8s, purging the reaction vessel with nitrogen for 20s, and then feeding the reaction vessel with deionized water at intervals, wherein the feeding duration of the deionized water is 8s, and purging the reaction vessel with nitrogen for 20s;
repeating the step 3 for n times, wherein n is any numerical value between 5 and 10000, so that a layer of titanium dioxide film is deposited on the surface of the coconut charcoal fiber superfine powder;
and 4, step 4: mixing 300 parts by weight of terephthalic acid and 50 parts by weight of an organic solvent (ethanol or isopropanol) at 50-60 ℃; then heating to 150-160 ℃ for esterification reaction, wherein the reaction time is 10-15min;
and 5: adding 60-0.005n parts by weight of the carbon fiber superfine powder with the titanium dioxide film deposited on the surface, which is obtained in the step (3), into a product after the esterification reaction; then adding 8-10 parts by weight of dimethyl propylene glycol, 5-10 parts by weight of 2,5-dimethyl-2,5-hexynediol, 5-15 parts by weight of 2-butene-1,4-di-n-butyl ester, 5-10 parts by weight of bis (hexane-1,6-diol) titanium, 5-10 parts by weight of a composite functional additive, 100 parts by weight of terephthalic acid and 50 parts by weight of ethylene glycol ester, heating to 200-250 ℃, reacting for 10-15min under the vacuum condition of 200-300Pa, and carrying out first polymerization reaction; adding 90-0.007n of the carbon fiber superfine powder with the titanium dioxide film deposited on the surface, obtained in the step 3, in parts by weight, reacting for 5-10min at 230-260 ℃ under the vacuum condition of 250-350Pa, and carrying out a second polymerization reaction to obtain a copolyester melt; the composite functional additive is a mixture of silicon dioxide, germanium dioxide, aluminum oxide and surface-modified aluminum-doped zinc oxide powder, and the mass ratio of the silicon dioxide, the germanium dioxide, the aluminum oxide and the surface-modified aluminum-doped zinc oxide powder is 1 (2-4) to 1 (2-4) in sequence;
step 6: carrying out melt spinning on the copolyester melt to obtain a melt, wherein the spinning temperature is 270-290 ℃;
and 7: extruding the melt through a profiled spinneret plate to form melt trickle, and cooling, wherein the spinneret micropores of the spinneret plate are gear-shaped;
and 8: and (3) carrying out yarn guiding, heat setting and winding forming on the melt trickle extruded and cooled by the spinneret plate to obtain the polyester staple fiber.
2. The method for preparing polyester staple fibers according to claim 1, wherein the step 1 specifically comprises: heating the coconut shell fiber to 1200 ℃, carbonizing in a vacuum environment, and micronizing the carbonized fiber to obtain the coconut charcoal fiber superfine powder.
3. The method for preparing polyester staple fibers according to claim 1, wherein the particle size of the silicon dioxide, germanium dioxide, aluminum oxide and surface-modified aluminum-doped zinc oxide powder is 10 to 30 μm.
4. The method for preparing polyester staple fibers according to claim 1, wherein the number of teeth of the spinneret micro holes of the spinneret plate is 6-8.
5. The method for preparing polyester staple fibers according to claim 1, wherein the diameter of the spinning micropores of the spinneret plate is 0.4-0.6mm in a gear shape, and the height of the teeth of the gear shape is 0.05-0.1mm.
6. The method for preparing polyester staple fibers according to claim 1, wherein the step 8 specifically comprises: feeding the filament bundle after being oiled and collected by the nozzle into a lower godet with the speed of 3105-3610m/min, and then feeding the filament bundle into a hot guide wire roller with the speed of 3105-3610m/min and the temperature of 120-135 ℃ for heat setting; and winding and molding at a winding speed of 3100-3600m/min to obtain the polyester staple fiber.
7. The method for preparing polyester staple fibers according to claim 1, wherein the cooling in the step 7 is specifically: solidifying into strands by adopting a side-blowing cooling process; the conditions of the side-blown cooling process are as follows: the speed of cross air blowing is 0.30-0.50 m/s, the temperature of the cross air blowing is 18 ℃, and the humidity of the cross air blowing is 75%.
8. A polyester staple product produced by the method for producing polyester staple according to any one of claims 1 to 7.
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