CN112680829A - Preparation method of recycled polyester and polypropylene sheath-core composite fiber - Google Patents
Preparation method of recycled polyester and polypropylene sheath-core composite fiber Download PDFInfo
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- 229920000728 polyester Polymers 0.000 title claims abstract description 198
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 100
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 100
- -1 polypropylene Polymers 0.000 title claims abstract description 85
- 239000000835 fiber Substances 0.000 title claims abstract description 71
- 239000002131 composite material Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000002699 waste material Substances 0.000 claims abstract description 83
- 238000000034 method Methods 0.000 claims abstract description 43
- 239000000126 substance Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 230000001172 regenerating effect Effects 0.000 claims abstract description 3
- 238000006068 polycondensation reaction Methods 0.000 claims description 57
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 48
- 239000012792 core layer Substances 0.000 claims description 30
- 238000006136 alcoholysis reaction Methods 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 28
- 238000009987 spinning Methods 0.000 claims description 27
- 239000004831 Hot glue Substances 0.000 claims description 25
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000003054 catalyst Substances 0.000 claims description 24
- 239000003963 antioxidant agent Substances 0.000 claims description 22
- 230000003078 antioxidant effect Effects 0.000 claims description 22
- 238000001816 cooling Methods 0.000 claims description 19
- 239000010410 layer Substances 0.000 claims description 19
- 230000008569 process Effects 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 15
- 238000004804 winding Methods 0.000 claims description 14
- 239000003381 stabilizer Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 9
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 8
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 claims description 8
- 238000009998 heat setting Methods 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000001301 oxygen Substances 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 5
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 229920002725 thermoplastic elastomer Polymers 0.000 claims description 4
- 239000004246 zinc acetate Substances 0.000 claims description 4
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 3
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 3
- 229940046892 lead acetate Drugs 0.000 claims description 3
- 229940071125 manganese acetate Drugs 0.000 claims description 3
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 3
- 239000001119 stannous chloride Substances 0.000 claims description 3
- 235000011150 stannous chloride Nutrition 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 229940013123 stannous chloride Drugs 0.000 claims description 2
- 229960000314 zinc acetate Drugs 0.000 claims description 2
- 239000011162 core material Substances 0.000 abstract description 71
- 238000011069 regeneration method Methods 0.000 abstract description 9
- 230000007613 environmental effect Effects 0.000 abstract description 8
- 238000011161 development Methods 0.000 abstract description 7
- 230000018109 developmental process Effects 0.000 abstract description 7
- 230000004069 differentiation Effects 0.000 abstract description 7
- 238000003912 environmental pollution Methods 0.000 abstract description 7
- 238000007306 functionalization reaction Methods 0.000 abstract description 7
- 239000003208 petroleum Substances 0.000 abstract description 7
- 239000011347 resin Substances 0.000 abstract description 7
- 229920005989 resin Polymers 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 description 34
- 239000000376 reactant Substances 0.000 description 20
- 238000001125 extrusion Methods 0.000 description 10
- 238000004064 recycling Methods 0.000 description 8
- 239000004753 textile Substances 0.000 description 8
- 239000000654 additive Substances 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 5
- 239000002270 dispersing agent Substances 0.000 description 5
- 239000000155 melt Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 238000002844 melting Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000005108 dry cleaning Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 239000012943 hotmelt 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
The invention discloses a preparation method of a sheath-core composite fiber of regenerated polyester and polypropylene, which is prepared by using the regenerated polyester and the polypropylene as raw materials and regenerating and modifying the polypropylene by a waste polyester chemical method. Compared with the conventional sheath-core composite fiber, the preparation method of the regenerated polyester and polypropylene sheath-core composite fiber has the obvious characteristics of environmental protection due to the fact that waste polyester is used as a raw material, and has the advantages of saving energy, reducing emission, reducing petroleum consumption, preventing environmental pollution and the like. Aiming at the problems that the current recycled polyester product is high in homogeneity degree, low in differentiation and functionalization level and incapable of meeting the market high-quality polyester application, the recycled polyester and polypropylene sheath-core composite fiber prepared by the invention can be compounded and spun with polypropylene thermal bonding resin into a sheath-core material by using a polyester chemical regeneration method, so that the high-valued applicability of the recycled polyester is remarkably improved, and the development of the recycled polyester industry to high-end application is facilitated.
Description
Technical Field
The invention relates to the field of chemical fiber materials, in particular to a preparation method of a sheath-core composite fiber of regenerated polyester and polypropylene.
Background
The global polyester yield in 2019 is about 8000 million tons, the utilization coverage range of polyester is wide, and the polyester is not covered from the non-woven industry to the textile industry, automobile textile products, home textiles, clothes and the like, but the supply amount of renewable polyester is very limited, so that the resource waste is large, and the environmental burden is heavy. At present, physical regeneration, namely a simple melt regeneration spinning process, is mostly adopted in China, bottle piece recycling is mainly used, and the recycling of waste textiles containing impurities cannot be realized. The problem is well solved by chemical method recycled polyester, for example, Chinese patent (publication No. CN110734578A, published as 2020.01.31) discloses a method for separating and obtaining recycled polyester from waste polyester raw materials, the method effectively removes impurities and purifies waste polyester depolymerization products, and can ensure that a filtering device can continuously and stably operate to prepare high-quality recycled polyester.
At present, the alcoholysis method has preliminarily realized industrial production, but compared with the primary polyester, the quality of the regenerated polyester is lower, the homogenization degree is high, and high value-added utilization is difficult, so that research and development of the regenerated polyester in the directions of antibiosis, flame retardance, easy dyeing and the like are needed.
The Chinese invention patent (publication No. CN110616474A, published Japanese 2019.12.27) discloses a method for preparing sheath-core composite low-melting-point regenerated polyester fibers from waste polyester textiles. The method comprises the steps of carrying out low-melting point modification on an esterified substance after multi-stage filtration on the basis of effective separation and alcoholysis esterification, and respectively carrying out polycondensation to obtain low-melting point polyester for a low-melting-point skin layer and polyester for a core layer. The method can realize continuous operation and obtain the high-quality sheath-core composite low-melting-point regenerated polyester fiber.
The hot melt bonding fiber is a fiber bonding agent which can be bonded by heating and melting. Has the advantages of rapid bonding and stable performance. The polypropylene grafted with maleic anhydride has good compatibility with polyester, the melting point of the polypropylene is 90-180 ℃, and the polypropylene can be prepared into sheath-core composite fibers and has wide application prospects. Meanwhile, polypropylene grafted with maleic anhydride can be developed into polypropylene-based hot melt adhesive products, and the polypropylene-based hot melt adhesive has excellent performances of water washing resistance, dry cleaning resistance and sand washing resistance, is easy to bleed, and has high peel strength, so that the polypropylene-based hot melt adhesive has extremely wide application range.
Disclosure of Invention
The invention provides a preparation method of a sheath-core composite fiber of recycled polyester and polypropylene, aiming at solving the problem of single performance of the recycled polyester. The method of the invention utilizes a chemical catalytic alcoholysis method to carry out high-efficiency depolymerization, then carries out refining purification and repolymerization on the product to prepare high-quality regenerated polyester, and utilizes skin-core composite spinning to realize high-valued and functional recycling of the waste polyester.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a sheath-core composite fiber of regenerated polyester and polypropylene utilizes the regenerated polyester and the polypropylene as raw materials, and is prepared by regenerating and modifying the polypropylene by a waste polyester chemical method, and comprises the following steps:
1) carrying out water removal and oxygen removal treatment on the recovered waste polyester material to obtain a waste polyester raw material;
2) carrying out high-temperature depolymerization on the waste polyester and ethylene glycol under the action of an alcoholysis catalyst, and filtering to obtain high-purity waste polyester depolymerization liquid;
3) adding waste polyester depolymerization liquid, a polycondensation catalyst, a stabilizer and an antioxidant into a polymerization kettle for pre-polycondensation, polycondensation and final polycondensation to obtain regenerated polyester;
4) extruding and granulating by adopting a thermoplastic elastomer (POE), polypropylene and polypropylene grafted maleic anhydride (PP-g-MAH) to obtain a hot melt adhesive granulation material;
5) the sheath-core composite fiber of the regenerated polyester and the polypropylene is prepared by adopting a sheath-core composite spinning method according to a spinning and drawing one-step (FDY) process.
The recycled waste polyester material comprises one or more of recycled polyester pulp blocks, polyester bottle flakes, polyester fibers and polyester waste filaments.
The mass ratio of the waste polyester material to the ethylene glycol in the step 2) is 1: 2-1: 4, putting the mixture into a depolymerization kettle, adding an alcoholysis catalyst accounting for 0.5 to 1.0 percent of the total mass of the waste polyester material and the ethylene glycol, and reacting for 2 to 6 hours at the temperature of between 180 and 200 ℃; wherein the alcoholysis catalyst is one of zinc acetate, stannous chloride, lead acetate and manganese acetate.
In the three processes of pre-polycondensation, polycondensation and final polycondensation in the step 3), the pre-polycondensation time is 2-3 hours, the temperature is controlled at 230-260 ℃, and the absolute pressure is 5-30 KPa; the polycondensation reaction time is 1-3 hours, the temperature is controlled at 260-290 ℃, and the absolute pressure is 1-5 KPa; the final polycondensation reaction time is 3-5 hours, the temperature is controlled at 270-300 ℃, and the absolute pressure is 0.05-1 KPa; the polycondensation reaction needs to add a polycondensation catalyst, a stabilizer and an antioxidant in a pre-polycondensation stage; the polycondensation catalyst adopts antimony trioxide; the stabilizer is one of triphenyl phosphate and triphenyl phosphite; the antioxidant is one of 1010 antioxidant or 168 antioxidant; the dosage of the polycondensation catalyst is 0.05 to 0.5 percent of the total mass of the high-purity waste polyester depolymerization liquid; the dosage of the stabilizer is 0.1 to 0.2 percent of the total mass of the high-purity waste polyester depolymerization liquid; the dosage of the antioxidant is 0.5-1% of the total mass of the high-purity waste polyester depolymerization liquid.
The grafting rate of the polypropylene grafted maleic anhydride (PP-g-MAH) in the step 4) is controlled to be 0.5-1.0%; the mass ratio of the thermoplastic elastomer (POE) to the polypropylene (PP) to the polypropylene grafted maleic anhydride (PP-g-MAH) is (2-3): (3-7): (1-5).
The FDY process flow of the step 5) is as follows: metering, spinneret plate extruding, cooling, oiling, stretching, heat setting and winding; the FDY process parameters are as follows: the skin layer spinning temperature is 180-200 ℃, the core layer spinning temperature is 275-285 ℃, the cooling temperature is 16-18 ℃, the network pressure is 0.30-0.40 MPa, the first roller speed is 2000-2200 m/min, the first roller temperature is 50-75 ℃, the two roller speed is 3200-3400 m/min, the two roller temperature is 70-90 ℃, and the winding speed is 3200-3500 m/min.
The prepared regenerated polyester and polypropylene sheath-core composite fiber has the filament number of 1.5-2.0 dtex, the cross section of the fiber is circular, and the mass ratio of the sheath to the core layer is 45: 55-55: 45, a first step of; the breaking strength of the sheath-core composite fiber is more than or equal to 3.5cN/dtex, and the elongation at break is 30-50%.
The invention has the beneficial effects that: compared with the conventional sheath-core composite fiber, the preparation method of the regenerated polyester and polypropylene sheath-core composite fiber has the obvious characteristics of environmental protection due to the fact that waste polyester is used as a raw material, and has the advantages of saving energy, reducing emission, reducing petroleum consumption, preventing environmental pollution and the like. Aiming at the problems that the current recycled polyester product is high in homogeneity degree, low in differentiation and functionalization level and incapable of meeting the market high-quality polyester application, the recycled polyester and polypropylene sheath-core composite fiber prepared by the invention can be compounded and spun with polypropylene thermal bonding resin into a sheath-core material by using a polyester chemical regeneration method, so that the high-valued applicability of the recycled polyester is remarkably improved, and the development of the recycled polyester industry to high-end application is facilitated.
Detailed Description
Example 1
The preparation method of the sheath-core composite fiber of recycled polyester and polypropylene of the embodiment comprises the following steps:
alcoholysis reaction
After water removal and oxygen removal treatment are carried out on waste polyester textiles (polyester fibers and polyester waste filaments), the waste polyester textiles and ethylene glycol are put into an alcoholysis kettle according to the mass ratio of 1: 2, zinc acetate accounting for 0.5 percent of the total mass of reactants (the polyester fibers, the polyester waste filaments and the ethylene glycol) is added to be used as an alcoholysis catalyst, the reaction is carried out for 6 hours under the condition that the alcoholysis temperature is 180 ℃, and then the high-purity waste polyester depolymerization liquid is obtained through filtration.
Polycondensation reaction
In the polycondensation reaction, antimony trioxide is used as a polycondensation catalyst, and the addition amount of the antimony trioxide is 0.05 percent of the total mass of reactants (high-purity waste polyester depolymerization liquid); the stabilizer adopts triphenyl phosphate, the additive amount of which is 0.2 percent of the total mass of the reactant (high-purity waste polyester depolymerization liquid), the antioxidant adopts 1010 antioxidant and basf, the additive amount of which is 0.5 percent of the total mass of the reactant (high-purity waste polyester depolymerization liquid), the pre-polycondensation reaction is carried out under the condition of 5Kpa of vacuum degree, and the reaction is carried out for 2 hours at the set temperature of 230 ℃; after the reaction is finished, continuously vacuumizing to carry out polycondensation reaction, reducing the reaction pressure to 1Kpa absolute pressure, and controlling the temperature at 260 ℃ for 1 h; and then continuously vacuumizing, carrying out final polycondensation reaction in a high vacuum stage, reducing the reaction pressure to 0.05Kpa absolute pressure, controlling the reaction temperature at 270 ℃ and reacting for 4 hours to obtain the low-regeneration polyester for the core layer.
Preparation of polypropylene-based hot melt adhesive
And (2) mixing the following components in percentage by mass: 7: 1, uniformly dispersing POE, PP and PP-G-MAH in a high-speed dispersing agent, adding the mixed materials into a double-screw extruder for extrusion, and performing water cooling and grain cutting to obtain the polypropylene-based hot melt adhesive.
Spinning
The sheath-core composite fiber is prepared by using a melt with a sheath polypropylene-based hot melt adhesive and a core layer as a regenerated polyester according to an FDY (fully drawn yarn) process through metering, spinneret plate extrusion, cooling, oiling, stretching, heat setting and winding, wherein the mass ratio of the sheath layer to the core layer is 45:55, and the parameters of the FDY process are as follows: the skin layer spinning temperature is 180 ℃, the core layer spinning temperature is 275 ℃, the cooling temperature is 16 ℃, the speed of a first roller is 2000m/min, the temperature of a first roller is 50 ℃, the speed of a second roller is 3200m/min, the temperature of a second roller is 70 ℃, and the winding speed is 3200 m/min.
The sheath-core composite fiber of the regenerated polyester and the polypropylene prepared by the steps is of a sheath-core structure, the sheath layer in the sheath-core structure is polypropylene-based hot melt adhesive, and the core layer is the regenerated polyester; the filament number of the single filament is 1.5dtex, the breaking strength of the sheath-core composite fiber reaches 3.5cN/dtex, and the elongation at break is 30%; the peel strength to the primer steel at 20 ℃ reaches 150N cm-1The peel strength to PP reaches 87N cm-1。
Compared with the conventional sheath-core composite fiber, the preparation method of the regenerated polyester and polypropylene sheath-core composite fiber disclosed by the embodiment has the obvious characteristics of environmental protection due to the fact that the waste polyester is used as the raw material, and has the advantages of saving energy, reducing emission, reducing petroleum consumption, preventing environmental pollution and the like. Aiming at the problems that the current recycled polyester product is high in homogeneity degree, low in differentiation and functionalization level and incapable of meeting the market high-quality polyester application, the recycled polyester and polypropylene sheath-core composite fiber prepared by the embodiment can be compounded and spun with polypropylene thermal bonding resin into a sheath-core material by using a polyester chemical recycling method, so that the high-valued applicability of the recycled polyester is remarkably improved, and the development of the recycled polyester industry to high-end application is facilitated.
Example 2
The preparation method of the sheath-core composite fiber of recycled polyester and polypropylene of the embodiment comprises the following steps:
alcoholysis reaction
After water removal and oxygen removal treatment of waste polyester textiles (waste polyester waste filaments), the waste polyester waste filaments and ethylene glycol are put into an alcoholysis kettle according to the mass ratio of 1: 2.5, zinc acetate accounting for 0.8% of the total mass of reactants (waste polyester waste filaments and ethylene glycol) is added as an alcoholysis catalyst, the reaction is carried out for 3 hours at the alcoholysis temperature of 185 ℃, and then the high-purity waste polyester depolymerization liquid is obtained through filtration.
Polycondensation reaction
In the polycondensation reaction, antimony trioxide is used as a catalyst, and the addition amount of the antimony trioxide is 0.5 percent of the total mass of reactants (high-purity waste polyester depolymerization liquid); the stabilizer adopts triphenyl phosphate, the additive amount of which is 0.1 percent of the total mass of the reactant (high-purity waste polyester depolymerization liquid), the antioxidant adopts 168 antioxidant, the Basff and the additive amount of which is 1 percent of the total mass of the reactant (high-purity waste polyester depolymerization liquid), the pre-polycondensation reaction is carried out under the condition of 10Kpa of vacuum degree, and the reaction is carried out for 2.5 hours at the set temperature of 240 ℃; after the reaction is finished, continuously vacuumizing to carry out polycondensation reaction, reducing the reaction pressure to 2Kpa absolute, and controlling the temperature at 270 ℃ for 1 h; and then continuously vacuumizing, carrying out final polycondensation reaction in a high vacuum stage, reducing the reaction pressure to 0.1Kpa absolute pressure, and controlling the reaction temperature at 280 ℃ for 4 hours to obtain the low-regeneration polyester for the core layer.
Preparation of polypropylene-based hot melt adhesive
And (3) mixing the following components in percentage by mass: 3: 5, uniformly dispersing POE, PP and PP-G-MAH in the high-speed dispersing agent, adding the mixed materials into a double-screw extruder for extrusion, and performing water cooling and grain cutting to obtain the polypropylene-based hot melt adhesive.
Spinning
The sheath-core composite fiber is prepared by using a melt with a sheath polypropylene-based hot melt adhesive and a core layer as a regenerated polyester according to an FDY (fully drawn yarn) process through metering, spinneret plate extrusion, cooling, oiling, stretching, heat setting and winding, wherein the mass ratio of the sheath layer to the core layer is 55:45, and the parameters of the FDY process are as follows: the skin layer spinning temperature is 200 ℃, the core layer spinning temperature is 285 ℃, the cooling temperature is 18 ℃, the first roller speed is 2200m/min, the first roller temperature is 75 ℃, the second roller speed is 3400m/min, the second roller temperature is 90 ℃, and the winding speed is 3500 m/min.
The recycled polyester/polypropylene sheath-core composite fiber prepared by the steps is of a sheath-core structure, the sheath layer in the sheath-core structure is polypropylene-based hot melt adhesive, and the core layer is recycled polyester; the filament number of the single filament is 1.8dtex, the breaking strength of the sheath-core composite fiber reaches 4.4cN/dtex, and the elongation at break is 50%; the peel strength to the primer steel at 20 ℃ reaches 168N cm-1The peeling strength to PP reaches 105N cm-1。
Compared with the conventional sheath-core composite fiber, the preparation method of the regenerated polyester and polypropylene sheath-core composite fiber disclosed by the embodiment has the obvious characteristics of environmental protection due to the fact that the waste polyester is used as the raw material, and has the advantages of saving energy, reducing emission, reducing petroleum consumption, preventing environmental pollution and the like. Aiming at the problems that the current recycled polyester product is high in homogeneity degree, low in differentiation and functionalization level and incapable of meeting the market high-quality polyester application, the recycled polyester and polypropylene sheath-core composite fiber prepared by the embodiment can be compounded and spun with polypropylene thermal bonding resin into a sheath-core material by using a polyester chemical recycling method, so that the high-valued applicability of the recycled polyester is remarkably improved, and the development of the recycled polyester industry to high-end application is facilitated.
Example 3
The preparation method of the sheath-core composite fiber of recycled polyester and polypropylene of the embodiment comprises the following steps:
alcoholysis reaction
After the waste polyester bottle chips are subjected to dehydration and deoxidization treatment, the waste polyester bottle chips and ethylene glycol are put into an alcoholysis kettle according to the mass ratio of 1: 3, lead acetate accounting for 1.0 percent of the total mass of reactants (the waste polyester bottle chips and the ethylene glycol) is added to serve as an alcoholysis catalyst, the reaction is carried out for 3 hours at the alcoholysis temperature of 200 ℃, and then the high-purity waste polyester depolymerization solution is obtained through filtration.
Polycondensation reaction
In the polycondensation reaction, antimony trioxide is used as a catalyst, and the addition amount of the antimony trioxide is 0.1 percent of the total mass of reactants (high-purity waste polyester depolymerization liquid); the stabilizer adopts triphenyl phosphite with the addition amount of 0.15 percent of the total mass of the reactant (high-purity waste polyester depolymerization liquid), the antioxidant adopts 1010 antioxidant and basf, the addition amount of 0.8 percent of the total mass of the reactant (high-purity waste polyester depolymerization liquid), the pre-polycondensation reaction is carried out under the condition of 8Kpa of vacuum degree, and the reaction is carried out for 2.5 hours at the set temperature of 260 ℃; after the reaction is finished, continuously vacuumizing to carry out polycondensation reaction, reducing the reaction pressure to 2.5Kpa absolute, and controlling the temperature at 280 ℃ for reaction for 2 hours; and then continuously vacuumizing, carrying out final polycondensation reaction in a high vacuum stage, reducing the reaction pressure to 0.3Kpa absolute pressure, and controlling the reaction temperature at 300 ℃ for reaction for 3h to obtain the low-regeneration polyester for the core layer.
Preparation of polypropylene-based hot melt adhesive
And (2) mixing the following components in percentage by mass: 4: 4, uniformly dispersing POE, PP and PP-G-MAH in the high-speed dispersing agent, adding the mixed materials into a double-screw extruder for extrusion, and performing water cooling and grain cutting to obtain the polypropylene-based hot melt adhesive.
Spinning
The sheath-core composite fiber is prepared by using a melt with a sheath polypropylene-based hot melt adhesive and a core layer as a regenerated polyester according to an FDY (fully drawn yarn) process through metering, spinneret plate extrusion, cooling, oiling, stretching, heat setting and winding, wherein the mass ratio of the sheath layer to the core layer is 45:55, and the parameters of the FDY process are as follows: the skin layer spinning temperature is 180 ℃, the core layer spinning temperature is 280 ℃, the cooling temperature is 16 ℃, the one-roller speed is 2200m/min, the one-roller temperature is 65 ℃, the two-roller speed is 3300m/min, the two-roller temperature is 75 ℃, and the winding speed is 3300 m/min.
Recycled polyester/polypropylene prepared by the above stepsThe sheath-core composite fiber is in a sheath-core structure, the sheath layer in the sheath-core structure is polypropylene-based hot melt adhesive, and the core layer is regenerated polyester; the filament number of the single filament is 1.8dtex, the breaking strength of the sheath-core composite fiber reaches 3.8cN/dtex, and the elongation at break is 40%; the peel strength to the primer steel at 20 ℃ reaches 165N cm-1The peeling strength to PP reaches 90N cm-1。
Compared with the conventional sheath-core composite fiber, the preparation method of the regenerated polyester and polypropylene sheath-core composite fiber disclosed by the embodiment has the obvious characteristics of environmental protection due to the fact that the waste polyester is used as the raw material, and has the advantages of saving energy, reducing emission, reducing petroleum consumption, preventing environmental pollution and the like. Aiming at the problems that the current recycled polyester product is high in homogeneity degree, low in differentiation and functionalization level and incapable of meeting the market high-quality polyester application, the recycled polyester and polypropylene sheath-core composite fiber prepared by the embodiment can be compounded and spun with polypropylene thermal bonding resin into a sheath-core material by using a polyester chemical recycling method, so that the high-valued applicability of the recycled polyester is remarkably improved, and the development of the recycled polyester industry to high-end application is facilitated.
Example 4
The preparation method of the sheath-core composite fiber of recycled polyester and polypropylene of the embodiment comprises the following steps:
alcoholysis reaction
After the waste polyester pulp is subjected to water removal and oxygen removal treatment, the waste polyester pulp and ethylene glycol are put into an alcoholysis kettle according to the mass ratio of 1: 4, manganese acetate accounting for 0.5 percent of the total mass of reactants (the waste polyester pulp and the ethylene glycol) is added as an alcoholysis catalyst, the reaction is carried out for 4 hours at the alcoholysis temperature of 190 ℃, and then the high-purity waste polyester depolymerization solution is obtained through filtration.
Polycondensation reaction
In the polycondensation reaction, antimony trioxide is used as a catalyst, and the addition amount of the antimony trioxide is 0.1 percent of the total mass of reactants (high-purity waste polyester depolymerization liquid); the stabilizer adopts triphenyl phosphate, the additive amount of which is 0.12 percent of the total mass of the reactant (high-purity waste polyester depolymerization liquid), the antioxidant adopts 168 antioxidant Pasteur, the additive amount of which is 0.7 percent of the total mass of the reactant (high-purity waste polyester depolymerization liquid), the pre-polycondensation reaction is carried out under the condition of the vacuum degree of 15Kpa, and the reaction is carried out for 3 hours at the set temperature of 230 ℃; after the reaction is finished, continuously vacuumizing to carry out polycondensation reaction, reducing the reaction pressure to 3Kpa absolute, and controlling the temperature to 290 ℃ for reaction for 1 h; and then continuously vacuumizing, carrying out final polycondensation reaction in a high vacuum stage, reducing the reaction pressure to 0.5Kpa absolute pressure, and controlling the reaction temperature at 290 ℃ for 4h to obtain the low-regeneration polyester for the core layer.
Preparation of polypropylene-based hot melt adhesive
And (2) mixing the following components in percentage by mass: 5: 3, uniformly dispersing POE, PP and PP-G-MAH in the high-speed dispersing agent, adding the mixed material into a double-screw extruder for extrusion, and performing water cooling and grain cutting to obtain the polypropylene-based hot melt adhesive.
Spinning
The sheath-core composite fiber is prepared by using a melt with a sheath polypropylene-based hot melt adhesive and a core layer as a regenerated polyester according to an FDY (fully drawn yarn) process through metering, spinneret plate extrusion, cooling, oiling, stretching, heat setting and winding, wherein the mass ratio of the sheath layer to the core layer is 50:50, and the parameters of the FDY process are as follows: the skin layer spinning temperature is 190 ℃, the core layer spinning temperature is 285 ℃, the cooling temperature is 17 ℃, the first roller speed is 2100m/min, the first roller temperature is 70 ℃, the second roller speed is 3400m/min, the second roller temperature is 80 ℃, and the winding speed is 3400 m/min.
The recycled polyester/polypropylene sheath-core composite fiber prepared by the steps is of a sheath-core structure, the sheath layer in the sheath-core structure is polypropylene-based hot melt adhesive, and the core layer is recycled polyester; the filament number of the single filament is 2.0dtex, the breaking strength of the sheath-core composite fiber reaches 4.2cN/dtex, and the elongation at break is 35%; the peel strength to the primer steel at 20 ℃ reaches 160N cm-1The peel strength to PP reaches 100N cm-1。
Compared with the conventional sheath-core composite fiber, the preparation method of the regenerated polyester and polypropylene sheath-core composite fiber disclosed by the embodiment has the obvious characteristics of environmental protection due to the fact that the waste polyester is used as the raw material, and has the advantages of saving energy, reducing emission, reducing petroleum consumption, preventing environmental pollution and the like. Aiming at the problems that the current recycled polyester product is high in homogeneity degree, low in differentiation and functionalization level and incapable of meeting the market high-quality polyester application, the recycled polyester and polypropylene sheath-core composite fiber prepared by the embodiment can be compounded and spun with polypropylene thermal bonding resin into a sheath-core material by using a polyester chemical recycling method, so that the high-valued applicability of the recycled polyester is remarkably improved, and the development of the recycled polyester industry to high-end application is facilitated.
Example 5
The preparation method of the sheath-core composite fiber of recycled polyester and polypropylene of the embodiment comprises the following steps:
alcoholysis reaction
After the waste polyester pulp and the waste polyester bottle chips are subjected to water removal and oxygen removal treatment, the waste polyester pulp and the waste polyester bottle chips and ethylene glycol are put into an alcoholysis kettle according to the mass ratio of 1: 3, stannous chloride accounting for 0.7 percent of the total mass of reactants (the waste polyester pulp, the waste polyester bottle chips and the ethylene glycol) is added as an alcoholysis catalyst, the reaction is carried out for 4 hours at the alcoholysis temperature of 180 ℃, and then the high-purity waste polyester depolymerization liquid is obtained through filtration.
Polycondensation reaction
In the polycondensation reaction, antimony trioxide is used as a catalyst, and the addition amount of the antimony trioxide is 0.05 percent of the total mass of reactants (high-purity waste polyester depolymerization liquid); the stabilizer adopts triphenyl phosphite with the addition amount of 0.4 percent of the total mass of the reactant (high-purity waste polyester depolymerization liquid), the antioxidant adopts 1010 antioxidant and basf with the addition amount of 0.5 percent of the total mass of the reactant (high-purity waste polyester depolymerization liquid), the pre-polycondensation reaction is carried out under the condition of the vacuum degree of 25Kpa, and the reaction is carried out for 2 hours at the set temperature of 250 ℃; after the reaction is finished, continuously vacuumizing to carry out polycondensation reaction, reducing the reaction pressure to 4Kpa absolute, and controlling the temperature to 285 ℃ for reaction for 2 hours; and then continuously vacuumizing, carrying out final polycondensation reaction in a high vacuum stage, reducing the reaction pressure to 0.8Kpa absolute pressure, and controlling the reaction temperature at 290 ℃ for 5 hours to obtain the low-regeneration polyester for the core layer.
Preparation of polypropylene-based hot melt adhesive
And (2) mixing the following components in percentage by mass: 3: 1, uniformly dispersing POE, PP and PP-G-MAH in a high-speed dispersing agent, adding the mixed materials into a double-screw extruder for extrusion, and performing water cooling and grain cutting to obtain the polypropylene-based hot melt adhesive.
Spinning
The sheath-core composite fiber is prepared by using a melt with a sheath polypropylene-based hot melt adhesive and a core layer as a regenerated polyester according to an FDY (fully drawn yarn) process through metering, spinneret plate extrusion, cooling, oiling, stretching, heat setting and winding, wherein the mass ratio of the sheath layer to the core layer is 50:50, and the parameters of the FDY process are as follows: the skin layer spinning temperature is 195 ℃, the core layer spinning temperature is 280 ℃, the cooling temperature is 18 ℃, the one-roller speed is 2150m/min, the one-roller temperature is 70 ℃, the two-roller speed is 3350m/min, the two-roller temperature is 85 ℃, and the winding speed is 3300 m/min.
The recycled polyester/polypropylene sheath-core composite fiber prepared by the steps is of a sheath-core structure, the sheath layer in the sheath-core structure is polypropylene-based hot melt adhesive, and the core layer is recycled polyester; the filament number of the single filament is 2.0dtex, the breaking strength of the sheath-core composite fiber reaches 4.2cN/dtex, and the elongation at break is 50%; the peel strength to the primer steel at 20 ℃ reaches 160N cm-1The peel strength to PP reaches 100N cm-1。
Compared with the conventional sheath-core composite fiber, the preparation method of the regenerated polyester and polypropylene sheath-core composite fiber disclosed by the embodiment has the obvious characteristics of environmental protection due to the fact that the waste polyester is used as the raw material, and has the advantages of saving energy, reducing emission, reducing petroleum consumption, preventing environmental pollution and the like. Aiming at the problems that the current recycled polyester product is high in homogeneity degree, low in differentiation and functionalization level and incapable of meeting the market high-quality polyester application, the recycled polyester and polypropylene sheath-core composite fiber prepared by the embodiment can be compounded and spun with polypropylene thermal bonding resin into a sheath-core material by using a polyester chemical recycling method, so that the high-valued applicability of the recycled polyester is remarkably improved, and the development of the recycled polyester industry to high-end application is facilitated.
Claims (7)
1. A preparation method of a sheath-core composite fiber of regenerated polyester and polypropylene is characterized in that the sheath-core composite fiber is prepared by using the regenerated polyester and the polypropylene as raw materials and regenerating and modifying the polypropylene by a waste polyester chemical method, and comprises the following steps:
1) carrying out water removal and oxygen removal treatment on the recovered waste polyester material to obtain a waste polyester raw material;
2) carrying out high-temperature depolymerization on the waste polyester and ethylene glycol under the action of an alcoholysis catalyst, and filtering to obtain high-purity waste polyester depolymerization liquid;
3) adding waste polyester depolymerization liquid, a polycondensation catalyst, a stabilizer and an antioxidant into a polymerization kettle for pre-polycondensation, polycondensation and final polycondensation to obtain regenerated polyester;
4) extruding and granulating thermoplastic elastomer, polypropylene and polypropylene grafted maleic anhydride to obtain hot melt adhesive granulating material;
5) the sheath-core composite fiber of the regenerated polyester and the polypropylene is prepared by adopting a sheath-core composite spinning method according to a spinning and stretching one-step process.
2. The method of claim 1, wherein the recycled waste polyester material comprises one or more of recycled polyester pulp, polyester bottle flakes, polyester fibers and polyester waste filaments.
3. The method for preparing a sheath-core composite fiber of recycled polyester and polypropylene according to claim 1, wherein the sheath-core composite fiber comprises the following steps: the mass ratio of the waste polyester material to the ethylene glycol in the step 2) is 1: 2-1: 4, putting the mixture into a depolymerization kettle, adding an alcoholysis catalyst accounting for 0.5 to 1.0 percent of the total mass of the waste polyester material and the ethylene glycol, and reacting for 2 to 6 hours at the temperature of between 180 and 200 ℃; wherein the alcoholysis catalyst is one of zinc acetate, stannous chloride, lead acetate and manganese acetate.
4. The method for preparing the recycled polyester and polypropylene sheath-core composite fiber according to claim 1, wherein in the three processes of pre-polycondensation, polycondensation and final polycondensation in the step 3), the pre-polycondensation time is 2-3 hours, the temperature is controlled at 230-260 ℃, and the absolute pressure is 5-30 KPa; the polycondensation reaction time is 1-3 hours, the temperature is controlled at 260-290 ℃, and the absolute pressure is 1-5 KPa; the final polycondensation reaction time is 3-5 hours, the temperature is controlled at 270-300 ℃, and the absolute pressure is 0.05-1 KPa; the polycondensation reaction needs to add a polycondensation catalyst, a stabilizer and an antioxidant in a pre-polycondensation stage; the polycondensation catalyst adopts antimony trioxide; the stabilizer is one of triphenyl phosphate and triphenyl phosphite; the antioxidant is one of 1010 antioxidant or 168 antioxidant; the dosage of the polycondensation catalyst is 0.05 to 0.5 percent of the total mass of the high-purity waste polyester depolymerization liquid; the dosage of the stabilizer is 0.1 to 0.2 percent of the total mass of the high-purity waste polyester depolymerization liquid; the dosage of the antioxidant is 0.5-1% of the total mass of the high-purity waste polyester depolymerization liquid.
5. The method for preparing a recycled polyester and polypropylene sheath-core composite fiber according to claim 1, wherein the grafting ratio of polypropylene grafted with maleic anhydride in the step 4) is controlled to be 0.5-1.0%; the mass ratio of the thermoplastic elastomer to the polypropylene grafted maleic anhydride is (2-3): (3-7): (1-5).
6. The method for preparing the sheath-core composite fiber of the recycled polyester and polypropylene according to claim 1, wherein the spinning and drawing one-step process flow of the step 5) is as follows: metering, spinneret plate extruding, cooling, oiling, stretching, heat setting and winding; the spinning and drawing one-step process parameters are as follows: the skin layer spinning temperature is 180-200 ℃, the core layer spinning temperature is 275-285 ℃, the cooling temperature is 16-18 ℃, the network pressure is 0.30-0.40 MPa, the first roller speed is 2000-2200 m/min, the first roller temperature is 50-75 ℃, the two roller speed is 3200-3400 m/min, the two roller temperature is 70-90 ℃, and the winding speed is 3200-3500 m/min.
7. The method for preparing the recycled polyester and polypropylene sheath-core composite fiber according to claim 1, wherein the prepared recycled polyester and polypropylene sheath-core composite fiber has a filament number of 1.5-2.0 dtex, a circular cross section, and a mass ratio of the sheath layer to the core layer of 45: 55-55: 45, a first step of; the breaking strength of the sheath-core composite fiber is more than or equal to 3.5cN/dtex, and the elongation at break is 30-50%.
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