CN115726057A - Regenerated low-melting-point polyester composite fiber with ultraviolet shielding function and preparation method thereof - Google Patents
Regenerated low-melting-point polyester composite fiber with ultraviolet shielding function and preparation method thereof Download PDFInfo
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- 229920000728 polyester Polymers 0.000 title claims abstract description 122
- 239000002131 composite material Substances 0.000 title claims abstract description 73
- 239000000835 fiber Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000006136 alcoholysis reaction Methods 0.000 claims abstract description 47
- 238000005886 esterification reaction Methods 0.000 claims abstract description 46
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical group OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims abstract description 40
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000009987 spinning Methods 0.000 claims abstract description 39
- 238000002844 melting Methods 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 27
- 239000012792 core layer Substances 0.000 claims abstract description 19
- 239000010410 layer Substances 0.000 claims abstract description 19
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 18
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 18
- QWGRWMMWNDWRQN-UHFFFAOYSA-N 2-methylpropane-1,3-diol Chemical group OCC(C)CO QWGRWMMWNDWRQN-UHFFFAOYSA-N 0.000 claims abstract description 17
- KKEYFWRCBNTPAC-UHFFFAOYSA-N terephthalic acid group Chemical group C(C1=CC=C(C(=O)O)C=C1)(=O)O KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 230000032050 esterification Effects 0.000 claims abstract description 14
- 230000008018 melting Effects 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 13
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 11
- 238000005520 cutting process Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000012216 screening Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000001125 extrusion Methods 0.000 claims abstract description 5
- 238000010924 continuous production Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical group OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000007664 blowing Methods 0.000 claims description 36
- 239000003054 catalyst Substances 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000003381 stabilizer Substances 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 15
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical group O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 12
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 230000006750 UV protection Effects 0.000 claims description 7
- 230000009477 glass transition Effects 0.000 claims description 7
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical group [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 235000010265 sodium sulphite Nutrition 0.000 claims description 6
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical group C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000004246 zinc acetate Substances 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- ZXDDPOHVAMWLBH-UHFFFAOYSA-N 2,4-Dihydroxybenzophenone Chemical group OC1=CC(O)=CC=C1C(=O)C1=CC=CC=C1 ZXDDPOHVAMWLBH-UHFFFAOYSA-N 0.000 claims description 2
- 150000001298 alcohols Chemical class 0.000 claims description 2
- WSXIMVDZMNWNRF-UHFFFAOYSA-N antimony;ethane-1,2-diol Chemical compound [Sb].OCCO WSXIMVDZMNWNRF-UHFFFAOYSA-N 0.000 claims description 2
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 2
- JVLRYPRBKSMEBF-UHFFFAOYSA-K diacetyloxystibanyl acetate Chemical compound [Sb+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JVLRYPRBKSMEBF-UHFFFAOYSA-K 0.000 claims description 2
- JGFBRKRYDCGYKD-UHFFFAOYSA-N dibutyl(oxo)tin Chemical compound CCCC[Sn](=O)CCCC JGFBRKRYDCGYKD-UHFFFAOYSA-N 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 2
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 claims description 2
- 229940094938 stannous 2-ethylhexanoate Drugs 0.000 claims 1
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims 1
- 238000002074 melt spinning Methods 0.000 abstract 1
- 230000008929 regeneration Effects 0.000 abstract 1
- 238000011069 regeneration method Methods 0.000 abstract 1
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- MEZZCSHVIGVWFI-UHFFFAOYSA-N 2,2'-Dihydroxy-4-methoxybenzophenone Chemical compound OC1=CC(OC)=CC=C1C(=O)C1=CC=CC=C1O MEZZCSHVIGVWFI-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- RXNYJUSEXLAVNQ-UHFFFAOYSA-N 4,4'-Dihydroxybenzophenone Chemical compound C1=CC(O)=CC=C1C(=O)C1=CC=C(O)C=C1 RXNYJUSEXLAVNQ-UHFFFAOYSA-N 0.000 description 2
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- SODJJEXAWOSSON-UHFFFAOYSA-N bis(2-hydroxy-4-methoxyphenyl)methanone Chemical compound OC1=CC(OC)=CC=C1C(=O)C1=CC=C(OC)C=C1O SODJJEXAWOSSON-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012943 hotmelt Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 238000009960 carding Methods 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Classifications
-
- 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
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- Polyesters Or Polycarbonates (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a regenerated low-melting-point polyester composite fiber with an ultraviolet shielding function and a preparation method thereof, wherein the regenerated low-melting-point polyester composite fiber with the ultraviolet shielding function is a fiber with a sheath-core structure, the sheath layer is regenerated low-melting-point polyester, and the core layer is polyethylene terephthalate; the regenerated low-melting-point polyester consists of a terephthalic acid chain segment, an isophthalic acid chain segment, an ethylene glycol chain segment, a 2-methyl-1, 3-propanediol chain segment, a diethylene glycol chain segment and an ultraviolet screening agent chain segment; the preparation method of the regenerated low-melting-point polyester composite fiber with the ultraviolet shielding function comprises the following steps: firstly, taking recycled polyester bottle chips as raw materials, and preparing regenerated low-melting-point polyester through a continuous process flow of screw extrusion melting, filtering, alcoholysis in a reaction kettle, filtering, decoloring by activated carbon, esterification, filtering, polycondensation and regeneration of the regenerated low-melting-point polyester; then, the regenerated low-melting-point polyester and the polyethylene terephthalate are respectively used as raw materials of the skin layer and the core layer to carry out melt composite spinning, and the regenerated low-melting-point polyester composite fiber with the ultraviolet shielding function is prepared through the working procedures of melt spinning, drafting, washing, curling, cutting, drying and the like. The prepared low-melting-point polyester composite fiber has a good ultraviolet shielding function, and can be widely applied to the high-added-value fields of automotive interiors and the like.
Description
Technical Field
The invention belongs to the field of low-melting-point polyester composite fibers, relates to a low-melting-point polyester composite fiber and a preparation method thereof, and particularly relates to a regenerated low-melting-point polyester composite fiber with an ultraviolet shielding function and a preparation method thereof.
Background
With the rapid development of the non-woven industry, the low-melting point polyester composite fiber special for non-woven is more and more valued by academia and industry. The low-melting-point polyester composite fiber generally exists in a sheath-core structure mode, the sheath layer and the core layer are respectively low-melting-point polyester and conventional polyester, the melting point of the sheath layer is lower than that of the core layer, the compatibility is good, the sheath layer is melted in the non-woven processing process to play a role in bonding, the core layer keeps the original structural form, the low-melting-point polyester composite fiber has the characteristics of low hot-melt bonding temperature, rapidness in bonding and high bonding strength, can replace a chemical bonding agent, is green and environment-friendly, and has good safety, and at present, the low-melting-point polyester composite fiber is mainly applied to the fields of silk-like cotton, non-collodion cotton, hard cotton, sound insulation boards, palm mattresses, automotive interiors, sports goods, medical sanitation and the like. A great deal of development and research is carried out on the fiber at home and abroad. However, in the market, there are few functional low-melting-point polyester composite fibers, in the field of automotive interiors, automobiles are often exposed under the sun directly for exposure, and the low-melting-point polyester composite fibers for automotive interiors are required to have an ultraviolet shielding function, but so far, only anhui donggi resource recycling technology limited company discloses a processing method (CN 201910420104.0) of a polyester hot melt filament for 3D fly-woven fabrics, and titanium dioxide and low-melting-point polyester chips are melt blended and spun to enable the low-melting-point polyester fibers to have a certain ultraviolet resistance function.
At present, the low-melting point polyester on the market almost contains isophthalic acid (IPA), the content is more than 30 percent, and the corresponding low-melting point polyester composite fiber also has better performance. However, the use of IPA has problems that, first, IPA is expensive; secondly, IPA is easy to cyclize at high temperature to form cyclized substances with the melting point as high as 325 ℃, and the cyclized substances are not melted during spinning, so that the replacement frequency of the filter screen is increased, the efficiency is reduced, and the cost is increased; and thirdly, the rigidity of the IPA chain segment is higher, the viscosity of the low-melting-point polyester with higher content is sensitive to temperature, the spinnability is poor, and the fiber forming is poor. Therefore, alternatives to IPA are sought to solve the problems with IPA.
In addition, the use of the regenerated polyester fiber is closely related to national strategies of 'carbon standard reaching, carbon neutralization' of the state, and becomes a responsibility and fashion, and international famous textile and clothing brands are all moving. Therefore, the recovery of polyester by chemical methods and the synthesis of low-melting polyester will be a trend in the field of low-melting polyester composite fibers.
Disclosure of Invention
The invention provides a regenerated low-melting-point polyester composite fiber with an anti-ultraviolet function and a preparation method thereof, which are developed aiming at the problems of few low-melting-point polyester composite fiber products with an anti-ultraviolet function and the development trend of environmental protection and low carbon in the conventional low-melting-point polyester spinning process.
The regenerated low-melting-point polyester composite fiber with the ultraviolet shielding function is characterized in that: the regenerated low-melting-point polyester composite fiber with the ultraviolet shielding function is a fiber with a skin-core structure, the skin layer is regenerated low-melting-point polyester, and the core layer is polyethylene terephthalate.
The low-melting-point polyester consists of a terephthalic acid chain segment, an isophthalic acid chain segment, an ethylene glycol chain segment, a 2-methyl-1, 3-propanediol chain segment, a diethylene glycol chain segment and an ultraviolet screening agent chain segment;
the ultraviolet shielding agent corresponding to the ultraviolet shielding agent chain segment is a dihydric alcohol series, and specifically is 2, 4-dihydroxy benzophenone, 4' -dihydroxy benzophenone, 2' -dihydroxy-4-methoxy benzophenone, 2' -dihydroxy-4, 4' -dimethoxy benzophenone or 2,2' -dihydroxy-4, 4' -dimethoxy benzophenone-5, 5' -sodium disulfonate;
the softening point of the low-melting-point polyester is 110-140 ℃, and the glass transition temperature is more than 60 ℃; the intrinsic viscosity of the low-melting-point polyester is 0.5-0.7 dL/g.
The regenerated low-melting-point polyester composite fiber with the ultraviolet shielding function is characterized in that the regenerated low-melting-point polyester with the ultraviolet shielding functionThe breaking strength of the composite fiber is more than or equal to 3.0cN/dtex; the composite ratio of the skin-core structure is 40-60: 60 to 40 percent; the corresponding area density is 18g/m 2 The UV protection index is greater than 50, and the transmittances of UV A and B are both less than 5%.
The preparation method of the regenerated low-melting-point polyester composite fiber with the ultraviolet shielding function is characterized by comprising the following steps of:
1) Preparation of recycled low-melting polyester
Taking recycled polyester bottle chips as raw materials, and preparing the recycled low-melting polyester through a continuous process flow of screw extrusion melting, filtering, reaction kettle alcoholysis, filtering, activated carbon decoloration, esterification reaction, filtering, polycondensation reaction and recycled low-melting polyester;
(1) Alcoholysis reaction
The temperature of screw extrusion melting is 280-300 ℃; the alcoholysis solution for alcoholysis in the reaction kettle is a mixed solution of ethylene glycol, 2-methyl-1, 3-propylene glycol and a dihydric alcohol ultraviolet shielding agent, the alcoholysis temperature is 180-220 ℃, the pressure is 0.15-0.3 MPa, and the mass ratio of the polyester bottle chips to the dihydric alcohol mixed solution is 1-3: 1, alcoholysis time is 0.5-3 hours, and a catalyst is zinc acetate which is 0.1-0.5 percent of the weight of the polyester bottle chips;
(2) Esterification reaction
The alcoholysis product is filtered on line and decolored by active carbon and then enters an esterification reaction kettle, new terephthalic acid and new isophthalic acid are added besides the alcoholysis liquid to carry out esterification reaction, the pressure reaction is carried out under the nitrogen atmosphere, the pressure is normal pressure to 0.3MPa, the temperature is 190-260 ℃, and the esterification reaction is terminated when the distillation amount of water in the esterification reaction is more than 90 percent of the theoretical value, thus preparing the esterification product;
(3) Polycondensation reaction
The esterification product is filtered on line and then enters a polycondensation reaction kettle, and the polycondensation reaction in a low vacuum stage is started under the action of a catalyst and a stabilizer under the condition of negative pressure; the pressure in the stage is steadily pumped from normal pressure to below 500Pa absolute pressure, the temperature is controlled to be 260-270 ℃, and the reaction time is 30-50 min; then continuously vacuumizing, and carrying out the polycondensation reaction in a high vacuum stage, so that the reaction pressure is reduced to be less than 100Pa, the reaction temperature is controlled to be 275-280 ℃, and the reaction time is 50-90 min, thereby obtaining the regenerated low-melting-point polyester.
2) Composite spinning
The pre-spinning adopts a skin-core composite spinning process, the regenerated low-melting-point polyester is taken as a skin layer, the polyethylene terephthalate is taken as a core layer, the spinning temperatures of the skin layer and the core layer are 260-275 ℃ and 280-290 ℃ respectively, and the spinning speed is 500-1100 m/min; the blowing is two cooling circular blowing; the temperature of the first circular blowing is 50-80 ℃, and the wind speed of the circular blowing is 1.0-3.0 m/s; the temperature of the second circular blowing is 14-20 ℃, and the speed of the circular blowing is 2.0-4.0 m/s; the interval between two cooling circular air blows is 30-50 cm;
the post-spinning adopts a drawing-washing process, and the regenerated low-melting-point polyester composite fiber with the ultraviolet shielding function is obtained through curling, cutting and drying; the drafting adopts oil bath drafting, 5-10 wt% of sodium sulfite is added in the oil bath, the temperature of the oil bath is 65-75 ℃, the drafting multiple is 2.5-2.7 times, the curling temperature is 50-60 ℃, the curling main pressure is 0.4-0.6 MPa, the curling back pressure is 0.2-0.4 MPa, the curling number is 8-10/25 mm, and the curling degree is 11-13%.
The preparation method of the regenerated low-melting-point polyester composite fiber with the ultraviolet shielding function is characterized in that the catalyst is antimony trioxide, ethylene glycol antimony, antimony acetate, isopropyl titanate, tetrabutyl titanate, dibutyltin oxide or 2-ethyl stannous hexanoate, and the addition amount of the catalyst is 0.01-0.05% of the total weight of dibasic acid; the stabilizer is triphenyl phosphate and trimethyl phosphate, and the addition amount of the stabilizer is 0.01-0.05% of the total weight of the dibasic acid.
The invention has the beneficial effects that:
(1) The invention uses 2-methyl-1, 3-propylene glycol chain segment to replace IPA, reduces the using amount of IPA, the methyl group on the 2-position carbon atom in the 2-methyl-1, 3-propylene glycol chain segment is beneficial to the rotation of the polymer, increases the fluidity of the polymer, reduces the crystallinity of the polymer, and has the similar function of IPA; the consumption of IPA is reduced, the formation of cyclized products can be reduced, the sensitivity of the viscosity of the regenerated low-melting-point polyester to temperature is reduced, the spinnability of the low-melting-point polyester is increased, the cost is reduced, the stability of the concentric-circle skin-core structure is ensured, and the quality of fibers is improved;
(2) In the invention, the 2-methyl-1, 3-propylene glycol and the dihydric alcohol ultraviolet shielding agent are also used as alcoholysis agents to carry out alcoholysis on the PET bottle flakes, thereby reducing the usage amount of ethylene glycol and reducing the generation of acetaldehyde;
(3) The invention combines the melting and alcoholysis technologies, melts the waste PET bottle flakes, overcomes the influence of the size of solid PET on the alcoholysis reaction speed in the conventional alcoholysis method, and increases the reaction speed of PET and dihydric alcohol;
(4) The excessive dihydric alcohol is not distilled and removed, and the excessive dihydric alcohol is less because the alcoholysis method of the waste PET under the condition of low using amount of the dihydric alcohol is adopted in the invention; secondly, the dimer formed by the reaction of excessive dihydric alcohol is one of the reactants of the low-melting-point polyester; in addition, terephthalic acid and isophthalic acid are introduced in the esterification reaction to react with excessive dihydric alcohol; therefore, the depolymerization of the waste PET and the polymerization process of the regenerated low-melting-point polyester are a continuous process, a complex extraction procedure is not needed, only solid particles mixed with the waste polyester are filtered out and pigments are removed, and the production efficiency is high;
(5) According to the invention, the ultraviolet screening agent is directly introduced into the macromolecular chain of the low-melting-point polyester, the functional factors are uniformly distributed and have good durability and no influence on spinnability, and the ultraviolet protection index of the prepared regenerated low-melting-point polyester composite fiber with the ultraviolet screening function is more than 50.
Detailed Description
The following description is of preferred embodiments of the invention, and it is to be understood that the embodiments are for the purpose of illustrating the invention better and are not to be taken in a limiting sense.
Example 1
1) Preparation of recycled low-melting polyester
(1) Alcoholysis reaction
Adding PET bottle flakes into a hopper of a double-screw extruder, extruding and melting by a double screw at 280 ℃, filtering, and performing alcoholysis in a high-temperature high-pressure reaction kettle filled with a mixed solution of ethylene glycol, 2-methyl-1, 3-propylene glycol and 4,4' -dihydroxy benzophenone to obtain an alcoholysis product; the alcoholysis temperature is 200 ℃, the pressure is 0.15MPa, and the mass ratio of the polyester bottle flakes to the dihydric alcohol mixed solution is 1:1, the molar ratio of the ethylene glycol, the 2-methyl-1, 3-propanediol and the 4,4' -dihydroxy benzophenone in the mixed solution is 1:1:0.1, alcoholysis time is 1.5 hours, and the catalyst is zinc acetate which is 0.1 percent of the weight of the polyester bottle chips;
(2) Esterification reaction
The alcoholysis product is filtered on line and decolored by active carbon and then enters an esterification reaction kettle, new terephthalic acid and new isophthalic acid are added in addition to the alcoholysis solution to carry out esterification reaction, the pressure reaction is carried out under the nitrogen atmosphere, the pressure is 0.3MPa, the temperature is 220 ℃, and the esterification reaction is terminated when the theoretical value of the distilled amount of water in the esterification reaction is more than 90 percent, thus obtaining the esterification product;
(3) Polycondensation reaction
The esterification product is filtered on line and then enters a polycondensation reaction kettle, and the polycondensation reaction in a low vacuum stage is started under the action of a catalyst and a stabilizer under the condition of negative pressure; the pressure in the stage is stably pumped from normal pressure to below 500Pa absolute, the temperature is controlled at 265 ℃, and the reaction time is 50min; then continuously vacuumizing, and carrying out polycondensation reaction in a high vacuum stage, so that the reaction pressure is reduced to be less than 100Pa, the reaction temperature is controlled at 275 ℃, and the reaction time is 90min, thereby preparing the regenerated low-melting-point polyester; the catalyst and the stabilizer are antimony trioxide and triphenyl phosphate respectively, and the addition amount of the catalyst and the stabilizer is 0.01 percent of the total weight of the dibasic acid.
2) Composite spinning
The pre-spinning adopts a skin-core composite spinning process, the regenerated low-melting-point polyester is taken as a skin layer, the polyethylene terephthalate is taken as a core layer, the spinning temperatures of the skin layer and the core layer are 270 ℃ and 280 ℃ respectively, and the spinning speed is 800m/min; the blowing is two cooling circular blowing; the temperature of the first circular blowing is 60 ℃, and the wind speed of the circular blowing is 2.0m/s; the temperature of the second circular blowing is 16 ℃, and the speed of the circular blowing is 3.0m/s; the interval between two cooling circular air blows is 40cm;
the post-spinning adopts a drawing-washing process, and the low-melting-point polyester composite fiber with the ultraviolet shielding function is obtained through curling, cutting and drying; the drafting adopts oil bath drafting, 6wt% of sodium sulfite is added into the oil bath, the temperature of the oil bath is 70 ℃, the drafting multiple is 2.5 times, the curling temperature is 55 ℃, the curling main pressure is 0.4MPa, the curling back pressure is 0.2MPa, the curling number is 8/25 mm, and the curling degree is 12%.
The polyester with low melting point in the polyester composite fiber with the ultraviolet shielding function prepared by the steps has the softening point of 118.6 ℃, the glass transition temperature of 61.3 ℃ and the intrinsic viscosity of 0.62dL/g; the filament number of the composite fiber is 1.8dtex, and the breaking strength is 3.48cN/dtex; the UPF of the composite fiber was 80.9 and the transmittances for ultraviolet a and B were 4.83% and 0.72%, respectively.
Example 2
1) Preparation of recycled low-melting polyester
(1) Alcoholysis reaction
Adding PET bottle flakes into a hopper of a double-screw extruder, extruding and melting the PET bottle flakes by a double screw at 285 ℃, filtering the PET bottle flakes, and performing alcoholysis in a high-temperature high-pressure reaction kettle filled with a mixed solution of ethylene glycol, 2-methyl-1, 3-propylene glycol and 2,2' -dihydroxy-4-methoxybenzophenone to obtain an alcoholysis product; the alcoholysis temperature is 210 ℃, the pressure is 0.2MPa, and the mass ratio of the polyester bottle flakes to the dihydric alcohol mixed solution is 2:1, the molar ratio of the ethylene glycol, the 2-methyl-1, 3-propylene glycol and the 2,2' -dihydroxy-4-methoxybenzophenone in the mixed solution is 1:1:0.5, the alcoholysis time is 1 hour, and the catalyst is zinc acetate which is 0.15 percent of the weight of the polyester bottle chips;
(2) Esterification reaction
The alcoholysis product is filtered on line and decolored by active carbon and then enters an esterification reaction kettle, new terephthalic acid and new isophthalic acid are added in addition to the alcoholysis solution to carry out esterification reaction, the pressure reaction is carried out under the nitrogen atmosphere, the pressure is 0.25MPa, the temperature is 240 ℃, and the esterification reaction is terminated when the theoretical value of the distilled amount of water in the esterification reaction is more than 90 percent, so as to prepare the esterification product;
(3) Polycondensation reaction
The esterification product is filtered on line and then enters a polycondensation reaction kettle, and the polycondensation reaction in a low vacuum stage is started under the action of a catalyst and a stabilizer under the condition of negative pressure; the pressure in the stage is steadily pumped from normal pressure to below 500Pa absolute pressure, the temperature is controlled at 265 ℃, and the reaction time is 50min; then continuing to vacuumize, and carrying out the polycondensation reaction in a high vacuum stage, so that the reaction pressure is reduced to be less than 100Pa, the reaction temperature is controlled at 280 ℃, and the reaction time is 90min, thereby preparing the regenerated low-melting-point polyester; the catalyst and the stabilizer are antimony trioxide and triphenyl phosphate respectively, and the addition amount of the catalyst and the stabilizer is 0.01 percent of the total weight of the dibasic acid.
2) Composite spinning
The pre-spinning adopts a skin-core composite spinning process, the regenerated low-melting-point polyester is taken as a skin layer, polyethylene terephthalate is taken as a core layer, the spinning temperatures of the skin layer and the core layer are 265 ℃ and 280 ℃ respectively, and the spinning speed is 750m/min; the air blowing is two cooling ring air blowing; the temperature of the first circular blowing is 60 ℃, and the wind speed of the circular blowing is 2.0m/s; the temperature of the second circular blowing is 16 ℃, and the speed of the circular blowing is 3.0m/s; the interval between two cooling circular air blows is 40cm;
the post-spinning adopts a drawing-washing process, and the regenerated low-melting-point polyester composite fiber with the ultraviolet shielding function is obtained through curling, cutting and drying; the drafting adopts oil bath drafting, 8wt% of sodium sulfite is added into the oil bath, the temperature of the oil bath is 70 ℃, the drafting multiple is 2.6 times, the curling temperature is 55 ℃, the curling main pressure is 0.4MPa, the curling back pressure is 0.2MPa, the curling number is 8/25 mm, and the curling degree is 12%.
The polyester with the ultraviolet shielding function in the polyester composite fiber has the advantages that the softening point of the low-melting-point polyester is 118.7 ℃, the glass transition temperature is 60.8 ℃, and the intrinsic viscosity is 0.58dL/g; the filament number of the composite fiber is 1.8dtex, and the breaking strength is 3.03cN/dtex; the UPF of the composite fiber was 140.3 and the transmission to uv a and B was 2.03% and 0.22%, respectively.
Example 3
1) Preparation of recycled low-melting polyester
(1) Alcoholysis reaction
Adding PET bottle flakes into a hopper of a double-screw extruder, extruding and melting by a double screw at 285 ℃, filtering, and performing alcoholysis in a high-temperature high-pressure reaction kettle filled with a mixed solution of ethylene glycol, 2-methyl-1, 3-propylene glycol and 2,2 '-dihydroxy-4, 4' -dimethoxy benzophenone to obtain an alcoholysis product; the alcoholysis temperature is 200 ℃, the pressure is 0.2MPa, and the mass ratio of the polyester bottle flakes to the mixed solution of the dihydric alcohol is 3: alcoholysis for 1 hour, wherein the molar ratio of the ethylene glycol, the 2-methyl-1, 3-propanediol and the 2,2 '-dihydroxy-4, 4' -dimethoxybenzophenone in the mixed solution is 1:1:0.3, the catalyst is zinc acetate which is 0.1 percent of the weight of the polyester bottle chips;
(2) Esterification reaction
The alcohol hydrolysis solution enters an esterification reaction kettle after being filtered on line and decolorized by active carbon, new terephthalic acid and isophthalic acid are added in addition to the alcohol hydrolysis solution to carry out esterification reaction, the pressure reaction is carried out under the nitrogen atmosphere, the pressure is 0.3MPa, the temperature is 250 ℃, and the esterification reaction is terminated when the theoretical value of the distilled amount of water in the esterification reaction is more than 90 percent, so as to prepare an esterification product;
(3) Polycondensation reaction
The esterification product is filtered on line and then enters a polycondensation reaction kettle, and the polycondensation reaction in a low vacuum stage is started under the action of a catalyst and a stabilizer under the condition of negative pressure; the pressure in the stage is stably pumped from normal pressure to below 500Pa absolute, the temperature is controlled at 270 ℃, and the reaction time is 50min; then continuously vacuumizing, and carrying out polycondensation reaction in a high vacuum stage, so that the reaction pressure is reduced to be less than 100Pa, the reaction temperature is controlled at 280 ℃, and the reaction time is 90min, thereby preparing the regenerated low-melting-point polyester; the catalyst and the stabilizer are antimony trioxide and triphenyl phosphate respectively, and the addition amount of the catalyst and the stabilizer is 0.01 percent of the total weight of the dibasic acid.
2) Composite spinning
The pre-spinning adopts a skin-core composite spinning process, the regenerated low-melting-point polyester is taken as a skin layer, polyethylene terephthalate is taken as a core layer, the spinning temperatures of the skin layer and the core layer are 270 ℃ and 280 ℃ respectively, and the spinning speed is 800m/min; the blowing is two cooling circular blowing; the temperature of the first circular blowing is 60 ℃, and the air speed of the circular blowing is 2.0m/s; the temperature of the second circular blowing is 16 ℃, and the speed of the circular blowing is 3.0m/s; the interval between two cooling circular air blows is 40cm;
the post-spinning adopts a drawing-washing process, and the regenerated low-melting-point polyester composite fiber with the ultraviolet shielding function is obtained through curling, cutting and drying; the drafting adopts oil bath drafting, 6wt% of sodium sulfite is added into the oil bath, the temperature of the oil bath is 70 ℃, the drafting multiple is 2.5 times, the curling temperature is 55 ℃, the curling main pressure is 0.4MPa, the curling back pressure is 0.2MPa, the curling number is 8/25 mm, and the curling degree is 12%.
The polyester with the ultraviolet shielding function in the polyester composite fiber prepared by the steps has the advantages that the softening point of the low-melting-point polyester is 128 ℃, the glass transition temperature is 60.2 ℃, and the intrinsic viscosity is 0.62dL/g; the filament number of the composite fiber is 1.8dtex, and the breaking strength is 3.17cN/dtex; the UPF of the composite fiber was 99.8 and the transmittances to ultraviolet a and B were 2.83% and 0.48%, respectively.
Example 4
1) Preparation of recycled low-melting polyester
(1) Alcoholysis reaction
Adding PET bottle flakes into a hopper of a double-screw extruder, extruding and melting by using double screws at 280 ℃, filtering, and then adding the mixture into a high-temperature high-pressure reaction kettle filled with mixed liquid of ethylene glycol, 2-methyl-1, 3-propylene glycol and 2,2' -dihydroxy-4, 4' -dimethoxy benzophenone-5, 5' -sodium disulfonate for alcoholysis to obtain an alcoholysis product; the alcoholysis temperature is 200 ℃, the pressure is 0.15MPa, and the mass ratio of the polyester bottle flakes to the mixed solution of the dihydric alcohol is 1:1, the molar ratio of the ethylene glycol, the 2-methyl-1, 3-propylene glycol and the 2,2' -dihydroxy-4, 4' -dimethoxybenzophenone-5, 5' -sodium disulfonate in the mixed solution is 1:1:0.25, alcoholysis time is 2 hours, and the catalyst is zinc acetate which is 0.1 percent of the weight of the polyester bottle chips;
(2) Esterification reaction
The alcohol hydrolysis solution enters an esterification reaction kettle after being filtered on line and decolorized by active carbon, new terephthalic acid and isophthalic acid are added in addition to the alcohol hydrolysis solution to carry out esterification reaction, the pressure reaction is carried out under the nitrogen atmosphere, the pressure is 0.3MPa, the temperature is 220 ℃, and the esterification reaction is terminated when the theoretical value of the distilled amount of water in the esterification reaction is more than 90 percent, so as to prepare an esterification product;
(3) Polycondensation reaction
The esterification product is filtered on line and then enters a polycondensation reaction kettle, and the polycondensation reaction in a low vacuum stage is started under the action of a catalyst and a stabilizer under the condition of negative pressure; the pressure in the stage is stably pumped from normal pressure to below 500Pa absolute, the temperature is controlled at 265 ℃, and the reaction time is 50min; then continuously vacuumizing, and carrying out polycondensation reaction in a high vacuum stage, so that the reaction pressure is reduced to be less than 100Pa, the reaction temperature is controlled at 275 ℃, and the reaction time is 90min, thereby preparing the regenerated low-melting-point polyester; the catalyst and the stabilizer are antimony trioxide and triphenyl phosphate respectively, and the addition amount of the catalyst and the stabilizer is 0.01 percent of the total weight of the dibasic acid.
2) Composite spinning
The pre-spinning adopts a skin-core composite spinning process, the regenerated low-melting-point polyester is taken as a skin layer, the polyethylene terephthalate is taken as a core layer, the spinning temperatures of the skin layer and the core layer are 270 ℃ and 280 ℃ respectively, and the spinning speed is 800m/min; the blowing is two cooling circular blowing; the temperature of the first circular blowing is 60 ℃, and the air speed of the circular blowing is 2.0m/s; the temperature of the second circular blowing is 16 ℃, and the speed of the circular blowing is 3.0m/s; the interval between two cooling circular air blows is 40cm;
the post-spinning adopts a drawing-washing process, and the regenerated low-melting-point polyester composite fiber with the ultraviolet shielding function is obtained through curling, cutting and drying; the drafting adopts oil bath drafting, 6wt% of sodium sulfite is added into the oil bath, the temperature of the oil bath is 70 ℃, the drafting multiple is 2.5 times, the curling temperature is 55 ℃, the curling main pressure is 0.4MPa, the curling back pressure is 0.2MPa, the curling number is 8/25 mm, and the curling degree is 12%.
The polyester with the ultraviolet shielding function in the polyester composite fiber prepared by the steps has the advantages that the softening point of the low-melting-point polyester is 129 ℃, the glass transition temperature is 62.2 ℃, and the intrinsic viscosity is 0.65dL/g; the filament number of the composite fiber is 1.8dtex, and the breaking strength is 3.0cN/dtex; the UPF of the composite fiber was 96.2 and the transmittances to ultraviolet a and B were 3.18% and 0.53%, respectively.
Examples 5 to 10
According to the preparation method of example 1, various low melting point polyester composite fibers having an ultraviolet shielding function were prepared by changing only the molar ratio of ethylene glycol, 2-methyl-1, 3-propanediol and 2,2' -dihydroxy-4-methoxybenzophenone.
Comparative example 1
According to the preparation method of the embodiment 1, the low-melting-point polyester composite fiber is prepared without introducing a dihydric alcohol ultraviolet shielding agent.
And (3) performance testing:
the mechanical properties, the ultraviolet protection properties, the linear density, the softening point, the glass transition temperature, the viscosity and the like of the low-melting polyester composite fibers of examples 5 to 10 and comparative example 1 were measured, and the specific test results are shown in table 1 below:
TABLE 1 comparison table of the results of the structure and performance tests of each low-melting polyester composite fiber
a, carding composite fibers with the length of 38mm and the linear density of 1.8dtex into a web by short fibers, bonding and reinforcing by hot air to obtain the composite fiber with the surface density of 18g/m 2 The non-woven material is tested for ultraviolet resistance according to the standard GB/T18830-2009 ultraviolet resistance of textiles.
From table 1 above, it can be seen that:
compared with the control group 1, the low-melting-point polyester composite fiber introduced with the ultraviolet shielding agent chain segment has good ultraviolet shielding function and has little influence on other performances.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (4)
1. A regenerated low-melting-point polyester composite fiber with an ultraviolet shielding function is characterized in that: the regenerated low-melting-point polyester composite fiber with the ultraviolet shielding function is a skin-core structure fiber, the skin layer is regenerated low-melting-point polyester, and the core layer is polyethylene terephthalate.
The low-melting-point polyester consists of a terephthalic acid chain segment, an isophthalic acid chain segment, an ethylene glycol chain segment, a 2-methyl-1, 3-propanediol chain segment, a diethylene glycol chain segment and an ultraviolet screening agent chain segment;
the ultraviolet screening agent corresponding to the ultraviolet screening agent chain segment is a dihydric alcohol series, and specifically is 2, 4-dihydroxy benzophenone, 4' -dihydroxy benzophenone, 2' -dihydroxy-4-methoxy benzophenone, 2' -dihydroxy-4, 4' -dimethoxy benzophenone or 2,2' -dihydroxy-4, 4' -dimethoxy benzophenone-5, 5' -sodium disulfonate;
the softening point of the low-melting-point polyester is 110-140 ℃, and the glass transition temperature is more than 60 ℃; the intrinsic viscosity of the low-melting-point polyester is 0.5-0.7 dL/g.
2. The recycled low-melting-point polyester composite fiber with the ultraviolet shielding function of claim 1, wherein the breaking strength of the recycled low-melting-point polyester composite fiber with the ultraviolet shielding function is more than or equal to 3.0cN/dtex; the composite ratio of the skin-core structure is 40-60: 60 to 40 percent; the corresponding area density is 18g/m 2 The ultraviolet protection index is more than 50, and the transmissivity of the ultraviolet A and the ultraviolet B is less than 5 percent.
3. The method for preparing the regenerated low-melting-point polyester composite fiber with the ultraviolet shielding function according to claim 1, which is characterized by comprising the steps of:
1) Preparation of recycled low-melting polyester
Taking recycled polyester bottle chips as raw materials, and preparing the recycled low-melting polyester through a continuous process flow of screw extrusion melting, filtering, alcoholysis in a reaction kettle, filtering, decoloring by activated carbon, esterification, filtering, polycondensation and recycling of the low-melting polyester;
(1) Alcoholysis reaction
The temperature of screw extrusion melting is 280-300 ℃; the alcoholysis solution for alcoholysis in the reaction kettle is a mixed solution of ethylene glycol, 2-methyl-1, 3-propylene glycol and a dihydric alcohol ultraviolet shielding agent, the alcoholysis temperature is 180-220 ℃, the pressure is 0.15-0.3 MPa, and the mass ratio of the polyester bottle chips to the dihydric alcohol mixed solution is 1-3: 1, alcoholysis time is 0.5-3 hours, and a catalyst is zinc acetate which is 0.1-0.5 percent of the weight of the polyester bottle chips;
(2) Esterification reaction
The alcoholysis product is filtered on line and decolored by active carbon and then enters an esterification reaction kettle, new terephthalic acid and new isophthalic acid are added besides the alcoholysis liquid to carry out esterification reaction, the pressure reaction is carried out under the nitrogen atmosphere, the pressure is normal pressure to 0.3MPa, the temperature is 190-260 ℃, and the esterification reaction is terminated when the distillation amount of water in the esterification reaction is more than 90 percent of the theoretical value, thus preparing the esterification product;
(3) Polycondensation reaction
The esterification product is filtered on line and then enters a polycondensation reaction kettle, and the polycondensation reaction in a low vacuum stage is started under the action of a catalyst and a stabilizer under the condition of negative pressure; the pressure in the stage is stably pumped from normal pressure to below 500Pa absolute, the temperature is controlled to be 260-270 ℃, and the reaction time is 30-50 min; then continuously vacuumizing, and carrying out the polycondensation reaction in a high vacuum stage, so that the reaction pressure is reduced to be less than 100Pa, the reaction temperature is controlled to be 275-280 ℃, and the reaction time is 50-90 min, thereby obtaining the regenerated low-melting-point polyester.
2) Composite spinning
The pre-spinning adopts a skin-core composite spinning process, the regenerated low-melting-point polyester is taken as a skin layer, the polyethylene terephthalate is taken as a core layer, the spinning temperatures of the skin layer and the core layer are 260-275 ℃ and 280-290 ℃ respectively, and the spinning speed is 500-1100 m/min; the blowing is two cooling circular blowing; the temperature of the first circular blowing is 50-80 ℃, and the wind speed of the circular blowing is 1.0-3.0 m/s; the temperature of the second circular blowing is 14-20 ℃, and the speed of the circular blowing is 2.0-4.0 m/s; the interval between two cooling circular air blows is 30-50 cm;
the post-spinning adopts a drawing-washing process, and the regenerated low-melting-point polyester composite fiber with the ultraviolet shielding function is obtained through curling, cutting and drying; the drafting adopts oil bath drafting, 5-10 wt% of sodium sulfite is added in the oil bath, the temperature of the oil bath is 65-75 ℃, the drafting multiple is 2.5-2.7 times, the curling temperature is 50-60 ℃, the curling main pressure is 0.4-0.6 MPa, the curling back pressure is 0.2-0.4 MPa, the curling number is 8-10/25 mm, and the curling degree is 11-13%.
4. The preparation method of the renewable low-melting-point polyester composite fiber with the ultraviolet shielding function according to claim 3, wherein the catalyst is antimony trioxide, ethylene glycol antimony, antimony acetate, isopropyl titanate, tetrabutyl titanate, dibutyltin oxide or stannous 2-ethyl hexanoate, and the addition amount of the catalyst is 0.01-0.05% of the total weight of the dibasic acid; the stabilizer is triphenyl phosphate and trimethyl phosphate, and the addition amount of the stabilizer is 0.01-0.05% of the total weight of the dibasic acid.
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