CN115161799B - High-purity high-viscosity terylene regenerated fiber and preparation method thereof - Google Patents
High-purity high-viscosity terylene regenerated fiber and preparation method thereof Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 71
- 239000005020 polyethylene terephthalate Substances 0.000 title claims abstract description 31
- 229920004933 Terylene® Polymers 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 39
- 238000009987 spinning Methods 0.000 claims abstract description 34
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 239000000155 melt Substances 0.000 claims abstract description 25
- 239000002699 waste material Substances 0.000 claims abstract description 23
- 238000004804 winding Methods 0.000 claims abstract description 14
- 238000002844 melting Methods 0.000 claims abstract description 13
- 230000008018 melting Effects 0.000 claims abstract description 13
- -1 1-ethyl acetate-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt Chemical class 0.000 claims abstract description 11
- WTPYFJNYAMXZJG-UHFFFAOYSA-N 2-[4-(2-hydroxyethoxy)phenoxy]ethanol Chemical compound OCCOC1=CC=C(OCCO)C=C1 WTPYFJNYAMXZJG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004342 Benzoyl peroxide Substances 0.000 claims abstract description 11
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000019400 benzoyl peroxide Nutrition 0.000 claims abstract description 11
- 125000005442 diisocyanate group Chemical group 0.000 claims abstract description 11
- DNBHVMRIHKHYIN-UHFFFAOYSA-N benzene;4,5-dihydro-1,3-oxazole Chemical compound C1CN=CO1.C1=CC=CC=C1 DNBHVMRIHKHYIN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims description 94
- 238000000034 method Methods 0.000 claims description 48
- 229920000728 polyester Polymers 0.000 claims description 43
- 230000008569 process Effects 0.000 claims description 38
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 36
- 238000009832 plasma treatment Methods 0.000 claims description 20
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 18
- 239000001569 carbon dioxide Substances 0.000 claims description 18
- 238000005273 aeration Methods 0.000 claims description 15
- 238000007664 blowing Methods 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 230000004888 barrier function Effects 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 12
- GWZMWHWAWHPNHN-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate Chemical compound CC(O)COC(=O)C=C GWZMWHWAWHPNHN-UHFFFAOYSA-N 0.000 claims description 8
- 230000009471 action Effects 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- HMOZDINWBHMBSQ-UHFFFAOYSA-N 2-[3-(4,5-dihydro-1,3-oxazol-2-yl)phenyl]-4,5-dihydro-1,3-oxazole Chemical compound O1CCN=C1C1=CC=CC(C=2OCCN=2)=C1 HMOZDINWBHMBSQ-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000009423 ventilation Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 abstract description 3
- 238000010583 slow cooling Methods 0.000 description 10
- 239000004744 fabric Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000008929 regeneration Effects 0.000 description 5
- 238000011069 regeneration method Methods 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- ZXMGHDIOOHOAAE-UHFFFAOYSA-N 1,1,1-trifluoro-n-(trifluoromethylsulfonyl)methanesulfonamide Chemical compound FC(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)F ZXMGHDIOOHOAAE-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- DJUITGNSBYIWFU-UHFFFAOYSA-N ethyl acetate;1-methylimidazole Chemical compound CCOC(C)=O.CN1C=CN=C1 DJUITGNSBYIWFU-UHFFFAOYSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 210000002268 wool Anatomy 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 229920004934 Dacron® Polymers 0.000 description 1
- 229920000433 Lyocell Polymers 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 229920002334 Spandex Polymers 0.000 description 1
- 229920006221 acetate fiber Polymers 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 235000009120 camo Nutrition 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 235000005607 chanvre indien Nutrition 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010559 graft polymerization reaction Methods 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000010409 ironing Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000004759 spandex Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/02—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polycarbonates or saturated polyesters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/10—Filtering or de-aerating the spinning solution or melt
- D01D1/106—Filtering
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
Abstract
The invention discloses a high-purity high-viscosity terylene regenerated fiber and a preparation method thereof, which is prepared by taking terylene waste as a raw material, preparing a melt through melting treatment, adding 1, 3-bis (2-oxazoline) benzene, diisocyanate, acrylic acid-beta-hydroxypropyl, benzoyl peroxide, 1-ethyl acetate-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt, hydroquinone-bis (beta-hydroxyethyl) ether and the like, carrying out heating reaction, spinning and winding to form filaments. Compared with the prior art, the invention has high purity and high viscosity, and greatly improves the mechanical property of the product.
Description
Technical Field
The invention belongs to the technical field of polyester regenerated fiber preparation, and particularly relates to high-purity high-viscosity polyester regenerated fiber and a preparation method thereof.
Background
The polyester fiber, namely polyethylene terephthalate, has higher strength and elastic recovery capability, has the advantages of fastness, durability, wrinkle resistance, non-ironing, non-sticking to wool and the like, and has wide application in civil fabrics and industrial fabrics. The polyester fiber is formed by the polymerization esterification and drawing of chemical raw materials PTA and MEG, the large development and utilization of the polyester fiber are accompanied with the large consumption of petroleum, and the resource shortage and the environmental deterioration are caused in the past.
Based on this, people begin to develop the polyester regeneration technology, that is, recycled materials (polyester cloth, waste polyester bottle chips, waste spinning yarns, bubble materials and the like) are utilized to be granulated and then are drawn into fibers. The terylene regeneration belongs to the recycling of renewable resources, has low cost and good performance, greatly reduces the consumption of petroleum and has important environmental protection significance.
The existing terylene regeneration technology mainly has the following two problems:
1. the purity is low:
at present, the process flow and the production technology of polyester chip spinning are generally adopted, and recycled polyester bottles and the like are utilized for crushing, cleaning, continuous drying, melting and filtering, so that polyester staple fibers are produced, the filtering effect of impurities cannot be guaranteed during filtering, and the product purity is low and the impurity content is high.
2. The viscosity is low:
because the melt can be degraded in the melting process, the viscosity of the melt is reduced, the uniformity is poor, on one hand, the consumption of raw materials is high, and on the other hand, the product quality level is low.
Due to the problems of low purity, low viscosity and the like in the terylene regeneration technology, the finally obtained terylene regenerated fiber has poor performances such as strength and the like, most of the terylene regenerated fiber can only be used for the production of low-grade fabrics or filling materials of furniture, toys and the like, the grade is low, the quality is poor, and the application and popularization of the terylene regenerated fiber are greatly limited.
Patent CN105887283B discloses a regenerated polyester fiber fabric and a production process thereof, which is woven by warp and weft, wherein the warp is 100% of regenerated polyester fiber, the weft is one or more of regenerated polyester fiber, polyamide fiber, spandex fiber, profiled fiber, acetate fiber, viscose fiber, tencel fiber, modal fiber, bamboo fiber, cotton fiber, hemp fiber, silk fiber and wool fiber, and the production process comprises warping, sizing, beaming, drafting, weaving, pre-treatment, dyeing, sizing and post-treatment. The regenerated polyester fiber is obtained by the conventional polyester regeneration technology, and has the problems of low purity, low viscosity and the like.
Patent application CN103510183A discloses a production method of regenerated polyester fiber, which comprises the following specific steps: 1) Esterification: mixing methanol or ethanol with carboxylic acid for reaction to obtain an ester; 2) Copolymerization: copolymerizing the esterified substance, the regenerated PET sheet and the comonomer to form a copolymer; 3) And (3) filtering: filtering the copolymer to remove impurities; 4) And (3) crystallization: crystallizing the copolymer with impurities removed through a crystallization box to form semi-solidified high molecular polymer; 5) Spinning: and (3) making the semi-solidified high molecular polymer into the regenerated polyester fiber through a spinneret plate. The patent technology still has the problems of low purity, low viscosity and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the high-purity high-viscosity terylene regenerated fiber and the preparation method thereof, which have high purity and high viscosity and greatly improve the mechanical property of the product.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of high-purity high-viscosity terylene regenerated fiber comprises the following specific steps:
(1) Firstly, cleaning and drying polyester waste, carrying out plasma treatment, crushing and melting to obtain a melt;
(2) Then, carrying out primary filtration on the melt, carrying out carbon dioxide ventilation treatment, continuously adding 1, 3-bis (2-oxazoline) benzene, diisocyanate, acrylic acid-beta-hydroxypropyl ester, benzoyl peroxide and 1-ethyl acetate-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt, uniformly mixing, carrying out heating reaction, and carrying out secondary filtration to obtain a pre-reaction melt;
(3) And then adding hydroquinone-bis (beta-hydroxyethyl) ether into the pre-reaction melt, heating again to react under the action of an alternating magnetic field, sucking under negative pressure, performing bipolar filtration, spinning and winding to form filaments, thus obtaining the terylene regenerated fiber.
Preferably, in the step (1), the waste polyester is waste polyester cloth or waste polyester silk.
Preferably, in the step (1), the process conditions of the plasma treatment are as follows: under normal pressure, a ceramic electrode is adopted to carry out plasma treatment on the polyester waste through dielectric barrier discharge, the working gas is argon, the flow rate is 18-20 m/s, and the discharge frequency of the dielectric barrier discharge is 100-120 MHz.
Preferably, in the step (1), the melting is carried out by a screw extruder, the screw extruder is divided into 7 zones, and the temperature of each zone is 260-270 ℃, 270-280 ℃, 285-295 ℃, 280-285 ℃ and 265-275 ℃ in sequence.
Preferably, in the step (2), the process conditions of the primary filtration are as follows: the filtering temperature is 285-295 ℃, the filtering precision is 30-40 mu m, and the filtering area is 18-20 m 2 。
Preferably, in the step (2), the process conditions of the carbon dioxide aeration treatment are as follows: the flow rate of the carbon dioxide is 300-400 mL/min, and the aeration time is 30-40 minutes.
Preferably, in the step (2), the mass ratio of the melt, 1, 3-bis (2-oxazolinyl) benzene, diisocyanate, beta-hydroxypropyl acrylate, benzoyl peroxide and 1-ethyl acetate-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt is 100: 8-10: 6 to 7: 1.2-1.5: 2 to 3:2 to 3.
Preferably, in the step (2), the heating reaction process conditions are as follows: the pressure is 0.3-0.5 MPa, the temperature is 230-240 ℃, and the reaction time is 2-3 hours.
Preferably, in the step (2), the process conditions for the second filtration are as follows: the filtering temperature is 290-300 ℃, the filtering precision is 20-30 mu m, and the filtering area is 13-16 m 2 。
Preferably, in step (3), the mass ratio of the pre-reaction melt to hydroquinone-bis (. Beta. -hydroxyethyl) ether is 100:6 to 8.
Preferably, in the step (3), the process conditions of the alternating magnetic field are as follows: the frequency is 3-5 kHz, and the magnetic field intensity is 800-1000G.
Preferably, in the step (3), the heating reaction process conditions are as follows: the pressure is 0.3-0.5 MPa, the temperature is 230-240 ℃, and the reaction time is 1-2 hours.
Preferably, in the step (3), the vacuum degree of the negative pressure suction is 80 to 100Pa, the temperature is 285 to 295 ℃, and the suction time is 25 to 35 minutes.
Preferably, in step (3), the bipolar filtration comprises: the primary filtering precision is less than or equal to 25 mu m, and the secondary filtering precision is less than or equal to 15 mu m.
Preferably, in the step (3), the specific method for spinning and winding into filaments is as follows: extruding filaments from the melt obtained after bipolar filtration in a spinning box through a metering pump, a component and a spinneret plate, and cooling and solidifying the filaments under the condition of lateral blowing at the temperature of between 20 and 25 ℃ to obtain nascent fiber; and then, drafting the nascent fiber by using a first hot roller and a second hot roller in sequence, wherein the temperature of the first hot roller is 90-100 ℃, the drafting multiple is 2.5-3 times, the temperature of the second hot roller is 160-170 ℃, and the drafting multiple is 3-4 times.
More preferably, the temperature in the spinning box is 250-260 ℃, the spinning speed is 1200-1300 r/min, the assembly pressure is 20-25 MPa, the air speed of the side blowing is 2-3 m/s, and the temperature of the side blowing is 32-35 ℃.
Further preferably, a slow cooling heater is arranged below the component, so that the temperature of a corresponding slow cooling area is 350-360 ℃, and the influence of a sheath-core structure generated by the nascent fiber on subsequent drafting is avoided.
The high-purity high-viscosity terylene regenerated fiber is obtained by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
the invention takes terylene waste as raw material, prepares melt through melting treatment, adds 1, 3-bis (2-oxazoline) benzene, diisocyanate, acrylic acid-beta-hydroxypropyl, benzoyl peroxide, 1-ethyl acetate-3-methylimidazole bis (trifluoromethanesulfonyl) imide salt, hydroquinone-bis (beta-hydroxyethyl) ether and the like, carries out heating reaction, and then carries out spinning and winding to obtain the terylene regenerated fiber. Compared with the prior art, the invention has high purity and high viscosity, and greatly improves the mechanical property of the product.
1. The method comprises the following steps of carrying out plasma treatment on cleaned and dried polyester waste before melting treatment, fully activating the polyester waste by the plasma treatment, not damaging a polyester structure, and simultaneously dissociating small molecular impurities to be separated in a subsequent heating process, so that the purity is improved. The melt prepared by the activated terylene waste is easier to participate in the subsequent graft polymerization reaction, which is beneficial to the improvement of viscosity.
2. The preparation method disclosed by the invention has the advantages that three filtering steps are carried out in the preparation process, the melt obtained by melting the waste terylene material is firstly filtered for the first time, filtered again after heating reaction, heated again for reaction and sucked under negative pressure for bipolar filtration, and through the control and matching of the three filtering steps, the purity is greatly improved, and the mechanical property of the product is improved.
3. The carbon dioxide aeration treatment is carried out after the primary filtration of the melt, which is beneficial to the dissociation of small molecular impurities, the improvement of purity and the full mixing of the melt and 1, 3-bis (2-oxazoline) benzene, diisocyanate, acrylic acid-beta-hydroxypropyl ester, benzoyl peroxide, 1-ethyl acetate-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt and the like, thereby ensuring the heating reaction effect and improving the mechanical property of the product. The 1, 3-bis (2-oxazoline) benzene mainly plays a role in chain extension, and the 1-ethyl acetate-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt contains an ester group, so that the compatibility of a system is improved, the viscosity is increased, and the mechanical property of a product is improved.
4. Hydroquinone-bis (beta-hydroxyethyl) ether is added into the pre-reaction melt, and is heated for reaction again under the action of an alternating magnetic field, the alternating magnetic field promotes the interaction between molecules in a system, promotes the chain extension reaction, and plays a better role in tackifying and improving the mechanical property.
5. And (3) performing negative pressure suction after the reheating reaction is finished, and under the action of the negative pressure suction, extracting small molecular substances in the system, so that the purification effect is achieved, the purity is improved, and the mechanical property of the product is ensured.
6. The preparation method provided by the invention keeps high purity and high viscosity, has the advantages of few broken ends in the spinning process, high yield and less loss, and the prepared polyester regenerated fiber has good mechanical property and good quality, can meet the use requirement of high-quality polyester fiber, and has good application and popularization values.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments of the present invention, belong to the protection scope of the present invention.
All commodities are purchased through market channels unless specially stated.
Example 1
A preparation method of high-purity high-viscosity terylene regenerated fiber comprises the following specific steps:
(1) Firstly, cleaning and drying waste terylene cloth, carrying out plasma treatment, crushing, and utilizing a screw extruder to realize melting, wherein the screw extruder is divided into 7 zones, and the temperatures of the zones are 260 ℃, 270 ℃, 285 ℃, 280 ℃ and 265 ℃ in sequence to obtain a melt;
(2) Then 100g of melt is subjected to primary filtration and carbon dioxide ventilation treatment, 8g of 1, 3-bis (2-oxazoline) benzene, 6g of diisocyanate, 1.2g of acrylic acid-beta-hydroxypropyl, 2g of benzoyl peroxide and 2g of 1-ethyl acetate-3-methylimidazolium bis (trifluoromethanesulfonyl) imide are added continuously, the mixture is uniformly mixed, heated and reacted, and filtered again to obtain pre-reaction melt;
(3) And then, adding 0.06 times of hydroquinone-bis (beta-hydroxyethyl) ether by weight into the pre-reaction melt, heating again to react under the action of an alternating magnetic field, sucking under negative pressure, performing bipolar filtration, spinning and winding to form yarns, and thus obtaining the polyester regenerated fiber.
Wherein, in the step (1), the process conditions of the plasma treatment are as follows: and (2) carrying out plasma treatment on the polyester waste through dielectric barrier discharge by adopting a ceramic electrode under normal pressure, wherein the working gas is argon, the flow rate is 18m/s, and the discharge frequency of the dielectric barrier discharge is 100MHz.
In the step (2), the process conditions of the primary filtration are as follows: the filtration temperature is 285 ℃, the filtration precision is 30 mu m, and the filtration area is 18m 2 。
In the step (2), the technological conditions of the carbon dioxide aeration treatment are as follows: the flow rate of carbon dioxide was 300mL/min and the aeration time was 30 minutes.
In the step (2), the process conditions of the heating reaction are as follows: the pressure is 0.3MPa, the temperature is 230 ℃, and the reaction time is 2 hours.
In the step (2), the process conditions of secondary filtration are as follows: the filtering temperature is 290 ℃, the filtering precision is 20 mu m, and the filtering area is 13m 2 。
In the step (3), the process conditions of the alternating magnetic field are as follows: frequency 3kHz, magnetic field intensity 800G.
In the step (3), the process conditions of the heating reaction are as follows: the pressure is 0.3MPa, the temperature is 230 ℃, and the reaction time is 1 hour.
In the step (3), the vacuum degree of negative pressure suction is 80Pa, the temperature is 285 ℃, and the suction time is 25 minutes.
In step (3), the bipolar filtration comprises: the primary filtering precision is less than or equal to 25 mu m, and the secondary filtering precision is less than or equal to 15 mu m.
In the step (3), the specific method for spinning and winding into filaments comprises the following steps: extruding filaments from the melt obtained after bipolar filtration in a spinning box through a metering pump, a component and a spinneret plate, and cooling and solidifying the filaments under the condition of lateral blowing at the temperature of 20 ℃ to obtain nascent fiber; and then, drafting the nascent fiber by using a first hot roller and a second hot roller in sequence, wherein the temperature of the first hot roller is 90 ℃, the drafting multiple is 2.5 times, the temperature of the second hot roller is 160 ℃, and the drafting multiple is 3 times. The temperature in the spinning box is 250 ℃, the spinning speed is 1200r/min, the pressure of the assembly is 20MPa, the wind speed of the side blowing is 2m/s, and the temperature of the side blowing is 32 ℃. A slow cooling heater is arranged below the component, so that the temperature of a corresponding slow cooling area is 350 ℃, and the influence of a sheath-core structure generated by the nascent fiber on subsequent drafting is avoided.
Example 2
A preparation method of high-purity high-viscosity terylene regenerated fiber comprises the following specific steps:
(1) Firstly, cleaning and drying waste polyester yarns, carrying out plasma treatment, crushing, and utilizing a screw extruder to realize melting, wherein the screw extruder is divided into 7 zones, and the temperatures of the zones are 270 ℃, 280 ℃, 295 ℃, 285 ℃ and 275 ℃ in sequence to obtain a melt;
(2) Then 100g of melt is subjected to primary filtration and carbon dioxide aeration treatment, 10g of 1, 3-bis (2-oxazolinyl) benzene, 7g of diisocyanate, 1.5g of acrylic acid-beta-hydroxypropyl ester, 3g of benzoyl peroxide and 3g of 1-ethyl acetate-3-methylimidazolium bis (trifluoromethanesulfonyl) imide are continuously added, the mixture is uniformly mixed, heated and reacted, and filtered again to obtain pre-reaction melt;
(3) And then, adding 0.08 times of hydroquinone-bis (beta-hydroxyethyl) ether by weight into the pre-reaction melt, heating again to react under the action of an alternating magnetic field, sucking under negative pressure, performing bipolar filtration, spinning and winding to form filaments, and thus obtaining the polyester regenerated fiber.
Wherein, in the step (1), the process conditions of the plasma treatment are as follows: and (2) carrying out plasma treatment on the polyester waste through dielectric barrier discharge by adopting a ceramic electrode under normal pressure, wherein the working gas is argon, the flow rate is 20m/s, and the discharge frequency of the dielectric barrier discharge is 120MHz.
In the step (2), the process conditions of the primary filtration are as follows: the filtration temperature is 295 ℃, the filtration precision is 40 mu m, and the filtration area is 20m 2 。
In the step (2), the technological conditions of the carbon dioxide aeration treatment are as follows: the flow rate of carbon dioxide was 400mL/min and the aeration time was 40 minutes.
In the step (2), the process conditions of the heating reaction are as follows: the pressure is 0.5MPa, the temperature is 240 ℃, and the reaction time is 3 hours.
In the step (2), the process conditions of secondary filtration are as follows: the filtering temperature is 300 ℃, the filtering precision is 30 mu m, and the filtering area is 16m 2 。
In the step (3), the process conditions of the alternating magnetic field are as follows: frequency 5kHz, magnetic field strength 1000G.
In the step (3), the process conditions of the heating reaction are as follows: the pressure is 0.5MPa, the temperature is 240 ℃, and the reaction time is 2 hours.
In the step (3), the vacuum degree of negative pressure suction is 100Pa, the temperature is 295 ℃, and the suction time is 35 minutes.
In step (3), the bipolar filtration comprises: the primary filtering precision is less than or equal to 25 mu m, and the secondary filtering precision is less than or equal to 15 mu m.
In the step (3), the specific method for spinning and winding into filaments comprises the following steps: extruding the melt obtained after bipolar filtration into filaments in a spinning box through a metering pump, a component and a spinneret plate, and cooling and solidifying under the condition of lateral blowing at 25 ℃ to obtain nascent fiber; and then, drafting the nascent fiber by using a first hot roller and a second hot roller in sequence, wherein the temperature of the first hot roller is 100 ℃, the drafting multiple is 3 times, the temperature of the second hot roller is 170 ℃, and the drafting multiple is 4 times. The temperature in the spinning box is 260 ℃, the spinning speed is 1300r/min, the pressure of the assembly is 25MPa, the wind speed of the side blowing is 3m/s, and the temperature of the side blowing is 35 ℃. A slow cooling heater is arranged below the component, so that the temperature of a corresponding slow cooling area is 360 ℃, and the influence of a sheath-core structure on subsequent drafting caused by nascent fibers is avoided.
Example 3
A preparation method of high-purity high-viscosity terylene regenerated fiber comprises the following specific steps:
(1) Firstly, cleaning and drying waste terylene cloth, carrying out plasma treatment, crushing, and utilizing a screw extruder to realize melting, wherein the screw extruder is divided into 7 zones, and the temperature of each zone is 265 ℃, 275 ℃, 290 ℃, 282 ℃ and 270 ℃ in sequence to obtain a melt;
(2) Then 100g of the melt is subjected to primary filtration and carbon dioxide aeration treatment, 9g of 1, 3-bis (2-oxazolinyl) benzene, 6.5g of diisocyanate, 1.3g of acrylic acid-beta-hydroxypropyl ester, 2.5g of benzoyl peroxide and 2.5g of 1-ethyl acetate-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt are added continuously, the mixture is uniformly mixed, heated and reacted, and filtered again to obtain a pre-reaction melt;
(3) And then, adding 0.07 time of hydroquinone-bis (beta-hydroxyethyl) ether into the pre-reaction melt, heating for reaction again under the action of an alternating magnetic field, sucking under negative pressure, filtering in a bipolar way, spinning and winding into filaments to obtain the terylene regenerated fiber.
Wherein, in the step (1), the process conditions of the plasma treatment are as follows: and (2) carrying out plasma treatment on the polyester waste through dielectric barrier discharge by adopting a ceramic electrode under normal pressure, wherein the working gas is argon, the flow rate is 19m/s, and the discharge frequency of the dielectric barrier discharge is 110MHz.
In the step (2), the process conditions of the primary filtration are as follows: the filtration temperature was 290 deg.CFiltration accuracy 35 μm, filtration area 19m 2 。
In the step (2), the technological conditions of the carbon dioxide aeration treatment are as follows: the flow rate of carbon dioxide was 350mL/min and the aeration time was 35 minutes.
In the step (2), the process conditions of the heating reaction are as follows: the pressure is 0.4MPa, the temperature is 235 ℃, and the reaction time is 2.5 hours.
In the step (2), the process conditions of secondary filtration are as follows: the filtration temperature is 295 ℃, the filtration precision is 25 mu m, and the filtration area is 15m 2 。
In the step (3), the process conditions of the alternating magnetic field are as follows: frequency 4kHz, magnetic field strength 900G.
In the step (3), the process conditions of the heating reaction are as follows: the pressure is 0.4MPa, the temperature is 235 ℃, and the reaction time is 1.5 hours.
In the step (3), the vacuum degree of negative pressure suction is 90Pa, the temperature is 290 ℃, and the suction time is 30 minutes.
In step (3), the bipolar filtration comprises: the primary filtering precision is less than or equal to 25 mu m, and the secondary filtering precision is less than or equal to 15 mu m.
In the step (3), the specific method for spinning and winding into filaments comprises the following steps: extruding the melt obtained after bipolar filtration into filaments through a metering pump, a component and a spinneret plate in a spinning box, and cooling and solidifying the filaments under the condition of side blowing at the temperature of 22 ℃ to obtain nascent fiber; and then, drafting the nascent fiber by using a first hot roller and a second hot roller in sequence, wherein the temperature of the first hot roller is 95 ℃, the drafting multiple is 3 times, the temperature of the second hot roller is 165 ℃, and the drafting multiple is 3 times. The temperature in the spinning box is 255 ℃, the spinning speed is 1300r/min, the pressure of the assembly is 22MPa, the wind speed of the side blowing is 2.5m/s, and the temperature of the side blowing is 33 ℃. A slow cooling heater is arranged below the component, so that the temperature of a corresponding slow cooling area is 355 ℃ to prevent the skin-core structure of the nascent fiber from influencing subsequent drafting.
Comparative example
A preparation method of high-purity high-viscosity terylene regenerated fiber comprises the following specific steps:
(1) Firstly, cleaning and drying waste polyester cloth, carrying out plasma treatment, crushing, and utilizing a screw extruder to realize melting, wherein the screw extruder is divided into 7 zones, and the temperatures of the zones are 265 ℃, 275 ℃, 290 ℃, 282 ℃ and 270 ℃ in sequence to obtain a melt;
(2) Then 100g of the melt is subjected to primary filtration, 9g of 1, 3-bis (2-oxazolinyl) benzene, 6.5g of diisocyanate, 1.3g of acrylic acid-beta-hydroxypropyl ester, 2.5g of benzoyl peroxide and 2.5g of 1-ethyl acetate-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt are added continuously, the mixture is uniformly mixed, heated to react, and filtered again to obtain a pre-reaction melt;
(3) And then, adding 0.07 time weight of hydroquinone-bis (beta-hydroxyethyl) ether into the pre-reaction melt, heating again to react under the action of an alternating magnetic field, sucking under negative pressure, performing bipolar filtration, spinning and winding to form filaments, and thus obtaining the polyester regenerated fiber.
Wherein, in the step (1), the process conditions of the plasma treatment are as follows: and (2) carrying out plasma treatment on the polyester waste through dielectric barrier discharge by adopting a ceramic electrode under normal pressure, wherein the working gas is argon, the flow rate is 19m/s, and the discharge frequency of the dielectric barrier discharge is 110MHz.
In the step (2), the process conditions of the primary filtration are as follows: the filtering temperature is 290 ℃, the filtering precision is 35 mu m, and the filtering area is 19m 2 。
In the step (2), the process conditions of the heating reaction are as follows: the pressure is 0.4MPa, the temperature is 235 ℃, and the reaction time is 2.5 hours.
In the step (2), the process conditions of secondary filtration are as follows: the filtration temperature is 295 ℃, the filtration precision is 25 mu m, and the filtration area is 15m 2 。
In the step (3), the process conditions of the alternating magnetic field are as follows: frequency 4kHz, magnetic field strength 900G.
In the step (3), the process conditions of the heating reaction are as follows: the pressure is 0.4MPa, the temperature is 235 ℃, and the reaction time is 1.5 hours.
In the step (3), the vacuum degree of negative pressure suction is 90Pa, the temperature is 290 ℃, and the suction time is 30 minutes.
In step (3), the bipolar filtration comprises: the primary filtering precision is less than or equal to 25 mu m, and the secondary filtering precision is less than or equal to 15 mu m.
In the step (3), the specific method for spinning and winding into filaments comprises the following steps: extruding the melt obtained after bipolar filtration into filaments through a metering pump, a component and a spinneret plate in a spinning box, and cooling and solidifying the filaments under the condition of side blowing at the temperature of 22 ℃ to obtain nascent fiber; and then, drafting the nascent fiber by using a first hot roller and a second hot roller in sequence, wherein the temperature of the first hot roller is 95 ℃, the drafting multiple is 3 times, the temperature of the second hot roller is 165 ℃, and the drafting multiple is 3 times. The temperature in the spinning box is 255 ℃, the spinning speed is 1300r/min, the pressure of the assembly is 22MPa, the wind speed of the cross air blow is 2.5m/s, and the temperature of the cross air blow is 33 ℃. A slow cooling heater is arranged below the component, so that the temperature of a corresponding slow cooling area is 355 ℃ to prevent the skin-core structure of the nascent fiber from influencing subsequent drafting.
The performance of the regenerated terylene fibers obtained in the examples 1 to 3 and the comparative example is respectively inspected, and the method specifically comprises the following steps:
1. and (3) viscosity investigation: 0.5g of the polyester regenerated fiber is taken respectively, added into 100g of a mixed solution of phenol-1, 2-tetrachloroethane (the mass ratio of phenol to 1, 2-tetrachloroethane is 1), ultrasonically oscillated to be dissolved, tested by using an Ubbelohde viscometer under the condition of 25 ℃, and the intrinsic viscosity [ eta ] is calculated by utilizing a Solomon-Ciuta equation.
2. Mechanical property investigation: the mechanical properties of the polyester regenerated fiber are examined by referring to GB/T14337-2008 'determination of breaking strength and breaking elongation of chemical fiber single fiber'.
The results are shown in Table 1.
TABLE 1 Performance test results of recycled Dacron fibers
| Intrinsic viscosity (dL/g) | Breaking strength (cN/dtex) | Elongation at Break (%) | |
| Example 1 | 0.81 | 6.7 | 35.9 |
| Example 2 | 0.84 | 6.5 | 35.5 |
| Example 3 | 0.82 | 6.6 | 36.1 |
| Comparative example | 0.69 | 5.3 | 28.6 |
As is clear from Table 1, the regenerated polyester fibers obtained in examples 1 to 3 had high viscosity, large breaking strength and large breaking sound, and demonstrated excellent mechanical properties.
The comparison example omits the carbon dioxide aeration treatment, the purity and the viscosity become worse, the mechanical property of the obtained product becomes obviously worse, and the carbon dioxide aeration treatment is beneficial to improving the purity and the viscosity, so that the mechanical property of the product is improved.
The technical idea of the present invention is illustrated by the above embodiments, but the present invention is not limited to the above embodiments, that is, it does not mean that the present invention must depend on the above embodiments to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitution of individual materials for the product of the present invention and addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. The preparation method of the high-purity high-viscosity terylene regenerated fiber is characterized by comprising the following specific steps:
(1) Firstly, cleaning and drying polyester waste, carrying out plasma treatment, crushing and melting to obtain a melt;
(2) Then, carrying out primary filtration on the melt, carrying out carbon dioxide ventilation treatment, continuously adding 1, 3-bis (2-oxazoline) benzene, diisocyanate, acrylic acid-beta-hydroxypropyl ester, benzoyl peroxide and 1-ethyl acetate-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt, uniformly mixing, carrying out heating reaction, and carrying out secondary filtration to obtain a pre-reaction melt;
(3) And then adding hydroquinone-bis (beta-hydroxyethyl) ether into the pre-reaction melt, heating again to react under the action of an alternating magnetic field, sucking under negative pressure, performing bipolar filtration, spinning and winding to form filaments, thus obtaining the terylene regenerated fiber.
2. The method according to claim 1, wherein in the step (1), the process conditions of the plasma treatment are as follows: under normal pressure, a ceramic electrode is adopted to carry out plasma treatment on the polyester waste through dielectric barrier discharge, the working gas is argon, the flow rate is 18-20 m/s, and the discharge frequency of the dielectric barrier discharge is 100-120 MHz.
3. The process according to claim 1, wherein in the step (1), the melting is carried out by a screw extruder, the screw extruder being divided into 7 zones, and the temperatures of the zones are 260 to 270 ℃, 270 to 280 ℃, 285 to 295 ℃, 280 to 285 ℃ and 265 to 275 ℃ in this order.
4. The preparation method according to claim 1, wherein in the step (2), the process conditions of the primary filtration are as follows: the filtering temperature is 285-295 ℃, the filtering precision is 30-40 mu m, and the filtering area is 18-20 m 2 。
5. The production method according to claim 1, wherein in the step (2), the process conditions for the carbon dioxide aeration treatment are: the flow rate of the carbon dioxide is 300-400 mL/min, and the aeration time is 30-40 minutes.
6. The method according to claim 1, wherein in the step (2), the melt, the 1, 3-bis (2-oxazolinyl) benzene, the diisocyanate, the β -hydroxypropyl acrylate, the benzoyl peroxide, and the 1-acetoxy-3-methylimidazolium bis (trifluoromethanesulfonyl) imide salt are mixed in a mass ratio of 100: 8-10: 6 to 7: 1.2-1.5: 2 to 3:2 to 3.
7. The preparation method according to claim 1, wherein in the step (2), the heating reaction is carried out under the following process conditions: the pressure is 0.3-0.5 MPa, the temperature is 230-240 ℃, and the reaction time is 2-3 hours.
8. The preparation method according to claim 1, wherein in the step (2), the process conditions for the second filtration are as follows: the filtering temperature is 290-300 ℃, the filtering precision is 20-30 mu m, and the filtering area is 13-16 m 2 。
9. The process according to claim 1, wherein in step (3), the mass ratio of the pre-reaction melt to hydroquinone-bis (β -hydroxyethyl) ether is 100:6 to 8 percent;
the process conditions of the alternating magnetic field are as follows: the frequency is 3-5 kHz, and the magnetic field intensity is 800-1000G;
the heating reaction process conditions are as follows: the pressure is 0.3 to 0.5MPa, the temperature is 230 to 240 ℃, and the reaction time is 1 to 2 hours;
the vacuum degree of negative pressure suction is 80-100 Pa, the temperature is 285-295 ℃, and the suction time is 25-35 minutes;
bipolar filtration comprises: the primary filtering precision is less than or equal to 25 mu m, and the secondary filtering precision is less than or equal to 15 mu m;
the specific method for spinning and winding into filaments comprises the following steps: extruding filaments from the melt obtained after bipolar filtration in a spinning box through a metering pump, a component and a spinneret plate, and cooling and solidifying the filaments under the condition of lateral blowing at the temperature of between 20 and 25 ℃ to obtain nascent fiber; and then, drafting the nascent fiber by using a first hot roller and a second hot roller in sequence, wherein the temperature of the first hot roller is 90-100 ℃, the drafting multiple is 2.5-3 times, the temperature of the second hot roller is 160-170 ℃, and the drafting multiple is 3-4 times.
10. A high-purity high-viscosity terylene regenerated fiber which is obtained by the preparation method of any one of claims 1 to 9.
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