CN107793560A - A kind of method that Waste Polyester alcoholysis method prepares regeneration high-contraction polyester - Google Patents
A kind of method that Waste Polyester alcoholysis method prepares regeneration high-contraction polyester Download PDFInfo
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- CN107793560A CN107793560A CN201710842713.6A CN201710842713A CN107793560A CN 107793560 A CN107793560 A CN 107793560A CN 201710842713 A CN201710842713 A CN 201710842713A CN 107793560 A CN107793560 A CN 107793560A
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- polyester
- alcoholysis
- contraction
- waste
- waste polyester
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- 229920000728 polyester Polymers 0.000 title claims abstract description 152
- 238000006136 alcoholysis reaction Methods 0.000 title claims abstract description 81
- 239000002699 waste material Substances 0.000 title claims abstract description 65
- 230000008929 regeneration Effects 0.000 title claims abstract description 61
- 238000011069 regeneration method Methods 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 40
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 283
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 43
- 150000007942 carboxylates Chemical class 0.000 claims abstract description 23
- XRAVYESZTUBEBU-UHFFFAOYSA-N cyclohexane;propan-2-ol Chemical compound CC(C)O.C1CCCCC1 XRAVYESZTUBEBU-UHFFFAOYSA-N 0.000 claims abstract description 12
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims description 30
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 26
- 230000035484 reaction time Effects 0.000 claims description 24
- 238000005886 esterification reaction Methods 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 14
- 239000003054 catalyst Substances 0.000 claims description 11
- 239000003381 stabilizer Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000003963 antioxidant agent Substances 0.000 claims description 10
- 230000003078 antioxidant effect Effects 0.000 claims description 10
- FYIBGDKNYYMMAG-UHFFFAOYSA-N ethane-1,2-diol;terephthalic acid Chemical compound OCCO.OC(=O)C1=CC=C(C(O)=O)C=C1 FYIBGDKNYYMMAG-UHFFFAOYSA-N 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000000835 fiber 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
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 3
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 238000005453 pelletization Methods 0.000 claims description 3
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 235000009508 confectionery Nutrition 0.000 claims 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 claims 1
- 238000004064 recycling Methods 0.000 abstract description 10
- 229920006267 polyester film Polymers 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 description 11
- 239000002994 raw material Substances 0.000 description 11
- 230000032050 esterification Effects 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 8
- 239000012452 mother liquor Substances 0.000 description 8
- 238000003786 synthesis reaction Methods 0.000 description 8
- 239000007791 liquid phase Substances 0.000 description 7
- 230000006641 stabilisation Effects 0.000 description 7
- 238000011105 stabilization Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 230000000717 retained effect Effects 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- -1 Polyethylene terephthalate Polymers 0.000 description 3
- QPKOBORKPHRBPS-UHFFFAOYSA-N bis(2-hydroxyethyl) terephthalate Chemical compound OCCOC(=O)C1=CC=C(C(=O)OCCO)C=C1 QPKOBORKPHRBPS-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000034659 glycolysis Effects 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229920000229 biodegradable polyester Polymers 0.000 description 2
- 239000004622 biodegradable polyester Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920001634 Copolyester Polymers 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000006140 methanolysis reaction Methods 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate tribasic Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 229910000404 tripotassium phosphate Inorganic materials 0.000 description 1
- 235000019798 tripotassium phosphate Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/672—Dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/18—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material
- C08J11/22—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic oxygen-containing compounds
- C08J11/24—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic oxygen-containing compounds containing hydroxyl groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/12—Applications used for fibers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention discloses a kind of method that Waste Polyester alcoholysis method prepares regeneration high-contraction polyester, comprise the following steps：1）The pretreatment of Waste Polyester；2）The alcoholysis of Waste Polyester；3）The addition of the controlling of quality of carboxylate and M-phthalic acid or Isosorbide-5-Nitrae cyclohexane dimethyl carbinol comonomer；4）The preparation of polycondensation and section；The inherent viscosity of the regeneration high-contraction polyester finally given is 0.60 ~ 0.70 dl/g, 210 ~ 230 DEG C of fusing point, diethylene glycol content are less than 6 in 3.0 ± 0.3%, colourity b values.Regeneration high-contraction polyester produced by the present invention can be used for high-shrinkage polyester filaments, short fine and high-contraction polyester film preparation, realize the high-valued recycling of Waste Polyester.
Description
Technical field
The present invention relates to a kind of method that Waste Polyester alcoholysis method prepares regeneration high-contraction polyester, belongs to Waste Polyester recycling
Field.
Background technology
Polyethylene terephthalate (PET, abbreviation polyester) is widely used in beverage bottle, fibre as important raw material
The production of dimension, film, sheet material etc..With developing rapidly for polyester industrial, processing in production of polyester and product, process is used
In, caused polyester waste material is also skyrocketed through.Because polyester has very strong chemical inertness, natural storage is difficult degraded or micro-
Biological decomposition, the huge wasting of resources is not only caused, and produce serious environmental pollution.Therefore, by recycling with reality
Existing resource benign cycle, improves environmental quality, turns into the important topic of current polyester industrial.
Reclaim of PET Scrap, which is utilized, at present mainly Physical and chemical method.Physical is mainly by Waste Polyester and its system
Product are made regenrated slice by the simple physical treatment method such as directly blending, blending, granulation and are used, but because of regenrated slice
Quality fluctuation it is larger, can only typically produce conventional short fine product.Chemical method mainly has Hydrolyze method, Methanolysis method, second two
Alcohol alcoholysis method etc., Waste Polyester make it resolve into the raw material or intermediate of production polyester, reach reuse by chemical treatment
Purpose, but because of reasons such as technical requirements, cost recovery height, fail widely to promote.Therefore, publication number CN106113319A is disclosed
" containing waste textile reclaiming technique is washed ", polyester waste material, spent glycol it will complete alcoholysis, ester in alcoholysis kettle after processing
Change, after polycondensation and multistage filtering, obtain recycled polyester.In order to enrich the kind of recycled polyester, publication number CN102153734A is public
" a kind of method that Biodegradable polyester is prepared by post-consumer polyester " has been opened, oligomer has been obtained by glycolysis alcoholysis, then
Biodegradable polyester is made through being copolymerized in the esterification derivative for adding aliphatic dibasic acid or aliphatic dibasic acid.Publication number
CN102617839A discloses " a kind of method that composite fibre water-soluble polyester is prepared with Waste Polyester ", by Waste Polyester second two
Alcohol carries out alcoholysis and obtains ethylene glycol terephthalate, then adds the 5-sodium sulfo isophthalate of certain mass percent
Copolyreaction is carried out with polyethylene glycol to be made.Publication number CN103145957B discloses " degradation of ethylene glycol production core-skin type polyester
With the method for high convergency recycled polyester ", the high convergency recycled polyester of its mediopellis is using recycled polyester as raw material, is dropped with ethylene glycol
Solution method, it is made by adding specific comonomer.
But the above obtains ethylene glycol terephthalate or oligomer by glycolysis alcoholysis, then carries out the side of polycondensation
Method, because of the uncertainty of raw material sources, recycled polyester form and aspect variation be present, accessory substance diethylene glycol (DEG) (DEG) content fluctuates big, fusing point
The problems such as whard to control, decline product quality.
Therefore, problem present in Waste Polyester alcoholysis method regenerative process how is overcome, and according to being obtained after Waste Polyester alcoholysis
Oligomer characteristic, carry out copolyesters research prepare, be recycled polyester area research and break through emphasis.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of Waste Polyester alcoholysis method prepares the side of regeneration high-contraction polyester
Method, regeneration high-contraction polyester produced by the present invention can be used for high-shrinkage polyester filaments, short fine and high-contraction polyester film preparation, real
The high-valued recycling of existing Waste Polyester.
The in order to solve the above-mentioned technical problem used technical scheme of the present invention is：
A kind of method that Waste Polyester alcoholysis method prepares regeneration high-contraction polyester, comprises the following steps：1) the pre- place of Waste Polyester
Reason, the Waste Polyester block of cleaning is directly smashed into feed bin, the Waste Polyester fiber of cleaning is sent into feed bin, Waste Polyester after being cut off
Bottle piece sorted, cleaned, being cleaned, being crushed, cut off after be sent into feed bin, then mix, for next procedure；2) Waste Polyester
Alcoholysis, by Waste Polyester：The molar percentage 1 of ethylene glycol:2~6 ratio input alcoholysis kettle, contains wherein in alcoholysis kettle and accounts for input
The ethylene glycol terephthalate (BHET) and oligomer (hereinafter referred to as mother liquor) of the mass percent of Waste Polyester total amount 20~40%, and
Add alcoholysis catalysts；190~210 DEG C of controlling reaction temperature, 2~6 hours reaction time, obtain containing terephthalate
The alcoholysate of ester (BHET) and oligomer, is sent into esterifying kettle after filtering；3) controlling of quality of carboxylate and comonomer add
Add, control 220~240 DEG C of esterification reaction temperature, 1~2 hour reaction time in esterifying kettle, while add M-phthalic acid
Or Isosorbide-5-Nitrae cyclohexane dimethyl carbinol comonomer, stabilizer, antioxidant (IPA)；Contained according to the reality of diethylene glycol (DEG) in alcoholysate (DEG)
Amount, addition diethylene glycol (DEG) (DEG), make diethylene glycol (DEG) (DEG) stable content in carboxylate account for products therefrom mass percent 2.5 ±
0.3% scope, obtained carboxylate enter precondensation kettle after filtering again；4) preparation of polycondensation and section, step 3) is entered
The carboxylate of precondensation kettle successively enters polycondensation-I and polycondensation-II, controls 240~260 DEG C, 1~100Kpa of vacuum of temperature, in advance
The inherent viscosity 0.2~0.4 of polymers；Subsequently into vertical whole polycondensation vessel, 260~270 DEG C of controlling reaction temperature, vacuum 0.1
~1Kpa, 1.0~2.0 hours reaction time, then discharged, filtered by Melt Pump, pelletizing, packaging；The regeneration finally given
The inherent viscosity of high-contraction polyester is 0.60~0.70dl/g, 210~230 DEG C of fusing point, DEG content in 3.0 ± 0.3%, colourity b
Value is less than 6.
The addition of described M-phthalic acid (IPA) accounts for the 5~15% of products therefrom mass percent；Described Isosorbide-5-Nitrae
The addition of cyclohexane dimethyl carbinol accounts for the 5~15% of products therefrom mass percent.
The addition of described alcoholysis catalysts accounts for the 2 ‰ of products therefrom mass percent；The addition of described stabilizer
Amount accounts for the 0.2 ‰ of products therefrom mass percent；The addition of described antioxidant accounts for products therefrom mass percent
0.5‰；Described alcoholysis catalysts use acetic acid saline catalyst；Described stabilizer is using triphenyl phosphate, phosphorous acid, phosphorus
One kind in sour trimethyl；Described antioxidant uses the antioxidant of hindered phenolic.
Described alcoholysis catalysts preferably use zinc acetate；Described stabilizer preferably uses triphenyl phosphate；Described
Antioxidant is preferably using antioxidant 1010 (being purchased from beneficial (Guangzhou) the chemical materials Co., Ltd in day).
Beneficial effects of the present invention are：1) retain a certain amount of mother liquor in alcoholysis kettle, alcoholysis efficiency, stably can be improved
Alcoholysis product quality；2) due to the uncertainty of Waste Polyester raw material, the DEG content fluctuation of alcoholysis product is larger, by being esterified
DEG controlling of quality systems are introduced in thing, ensure that the stabilization of DEG content；3) after utilizing glycolysis alcoholysis, DEG content is higher
Characteristic, it is used as comonomer by adding M-phthalic acid or Isosorbide-5-Nitrae cyclohexane dimethyl carbinol, realizes the life of regeneration high-contraction polyester
Production.4) from alcoholysis to esterification, again to polycondensation, using relatively low reaction temperature, the generation of accessory substance is effectively reduced；5) control relatively low
Precondensation inherent viscosity, final polycondensation reaction kettle is used as using efficient vertical liquid-phase tackifying kettle, it is poly- instead in final minification to reduce melt
Residence time and the reaction temperature of kettle are answered, overcomes reaction time length, reaction temperature existing for general horizontal final polycondensation reaction kettle high
The shortcomings that being detained with melt, the form and aspect of product are preferable, and regeneration high-contraction polyester items product quality indicator is stable.The present invention is made
Regeneration high-contraction polyester can be used for high-shrinkage polyester filaments, short fine and high-contraction polyester film preparation, realize the height of Waste Polyester
Value recycles.
Brief description of the drawings
Fig. 1 is present invention process flow chart.
Embodiment
Illustrate with reference to embodiments, but do not limit the present invention.
The property indices of high retraction polyester chip are regenerated, by GBT 14190-2008 fiber polyester chips (PET)
Test method performs.
Embodiment 1
The method that a kind of Waste Polyester alcoholysis method of the present embodiment prepares regeneration high-contraction polyester, as shown in figure 1, including as follows
Step：1) pretreatment of Waste Polyester, the Waste Polyester block of cleaning is directly smashed into feed bin, the Waste Polyester fiber of cleaning and cut
Have no progeny and be sent into feed bin, waste polyester bottle piece sorted, cleaned, being cleaned, being crushed, cut off after be sent into feed bin, then mix, confession
Next procedure；2) alcoholysis of Waste Polyester, by pretreated Waste Polyester, by Waste Polyester (Waste Polyester is added in mouth 7 and added) and second
The molar percentage 1 of glycol (ethylene glycol is added in mouth 6 and added):2 ratio puts into alcoholysis kettle 1, contains in alcoholysis kettle 1 to benzene two
Formic acid glycol ester and oligomer (mother liquor) (the first additive is added in mouth 8 and added), wherein ethylene glycol terephthalate and
The addition of oligomer (mother liquor) accounts for the 40% of input Waste Polyester gross mass percentage, and the addition of alcoholysis catalysts zinc acetate is
2 ‰ (accounting for products therefrom mass percent) (the first additive is added in mouth 8 and added).210 DEG C of controlling reaction temperature, reaction time
6 hours, the alcoholysate containing BHET and oligomer is obtained, is sent into esterifying kettle 2 after filtering；3) controlling of quality of carboxylate and copolymerization
The addition of monomer, control and 240 DEG C of esterification reaction temperature, 2 hours reaction time are controlled in esterifying kettle 2, while add 5% and (account for institute
Product quality percentage) M-phthalic acid (IPA) (comonomer add mouth 9 in add), 0.2 ‰ (account for products therefrom matter
Amount percentage) triphenyl phosphate stabilizer (Second addition add mouth 10 in add) and 0.5 ‰ (account for products therefrom quality hundred
Divide ratio) antioxidant 1010 (Second addition is added in mouth 10 and added), and according to the content of DEG in alcoholysate, addition 0.4%
The DEG (Second addition is added in mouth 10 and added) of (accounting for products therefrom mass percent), makes the DEG content in carboxylate (account for
Products therefrom mass percent) it is 2.6%, obtained carboxylate enters precondensation kettle after filtering again；4) polycondensation and section
Prepare, the carboxylate that step 3) is entered to precondensation kettle successively enters polycondensation-I and polycondensation-II (prepolymerization reaction kettle-I 3 and pre-
4), the temperature for controlling polycondensation-I and polycondensation-II is respectively 240,250 DEG C to batch condensation polymerization reactor-II, 1~100Kpa of vacuum, pre-polymerization
The inherent viscosity 0.4 of thing；Subsequently into vertical whole polycondensation vessel 5,270 DEG C, 0.1~1Kpa of vacuum of controlling reaction temperature, reaction
1.0 hours time, then discharged, filtered by Melt Pump, pelletizing, packaging；The characteristic of the regeneration high-contraction polyester finally given
Viscosity is 0.698dl/g, 229.5 DEG C of fusing point, DEG content 3.1%, colourity b values 5.1 (the results are shown in Table 1, table 1 is regeneration high convergency
Polyester synthesis condition and performance indications table).
Regeneration high-contraction polyester manufactured in the present embodiment has following features：1) a certain amount of mother is retained in alcoholysis kettle
Liquid, alcoholysis efficiency, stable alcoholysis product quality can be improved；2) due to the uncertainty of Waste Polyester raw material, the DEG of alcoholysis product
Content fluctuation is larger, by introducing DEG controlling of quality systems in carboxylate, ensure that the stabilization of DEG content；3) second two is utilized
After alcohol alcoholysis, the higher characteristic of DEG content, it is used as comonomer by adding M-phthalic acid (IPA), realizes regeneration high convergency
The production of polyester.4) from alcoholysis to esterification, again to polycondensation, using relatively low reaction temperature, the generation of accessory substance is effectively reduced；5)
Relatively low precondensation inherent viscosity is controlled, using efficient vertical liquid-phase tackifying kettle as final polycondensation reaction kettle, melt is reduced and exists
The residence time of final polycondensation reaction kettle and reaction temperature, overcome the reaction time existing for general horizontal final polycondensation reaction kettle long, anti-
The shortcomings that answering temperature high with melt delay, the form and aspect of product are preferable, and regeneration high-contraction polyester items product quality indicator is stable.This
The obtained regeneration high-contraction polyester of embodiment can be used for high-shrinkage polyester filaments, short fine and high-contraction polyester film preparation, realize
The high-valued recycling of Waste Polyester.
Embodiment 2
As described in Example 1, except that：The molar percentage 1 of Waste Polyester and ethylene glycol:4, in alcoholysis kettle containing pair
PET and oligomer (mother liquor), the addition of wherein ethylene glycol terephthalate and oligomer (mother liquor) account for
Put into the 30% of Waste Polyester gross mass percentage, 200 DEG C of reaction temperature, 4 hours reaction time.Add 0.2 ‰ and (account for products therefrom
Mass percent) phosphorous acid stabilizer；230 DEG C of esterification reaction temperature, 1.5 hours reaction time, while add 10% and (account for institute
Product quality percentage) M-phthalic acid (IPA), the DEG of 0.3% (accounting for products therefrom mass percent), make carboxylate
In DEG content (accounting for products therefrom mass percent) be 2.5%.The temperature of control polycondensation-I and polycondensation-II is respectively 250,
260 DEG C, the inherent viscosity 0.2 of prepolymer；Vertical whole polycondensation vessel, 265 DEG C of reaction temperature, 1.5 hours reaction time.Finally give
Regeneration high-contraction polyester inherent viscosity for 0.652dl/g, 220.1 DEG C of fusing point, DEG content 3.0%, colourity b values 5.5.(knot
Fruit is shown in Table 1, and table 1 is regeneration high-contraction polyester synthesis condition and performance indications table).
Regeneration high-contraction polyester manufactured in the present embodiment has following features：1) a certain amount of mother is retained in alcoholysis kettle
Liquid, alcoholysis efficiency, stable alcoholysis product quality can be improved；2) due to the uncertainty of Waste Polyester raw material, the DEG of alcoholysis product
Content fluctuation is larger, by introducing DEG controlling of quality systems in carboxylate, ensure that the stabilization of DEG content；3) second two is utilized
After alcohol alcoholysis, the higher characteristic of DEG content, it is used as comonomer by adding M-phthalic acid (IPA), realizes regeneration high convergency
The production of polyester.4) from alcoholysis to esterification, again to polycondensation, using relatively low reaction temperature, the generation of accessory substance is effectively reduced；5)
Relatively low precondensation inherent viscosity is controlled, using efficient vertical liquid-phase tackifying kettle as final polycondensation reaction kettle, melt is reduced and exists
The residence time of final polycondensation reaction kettle and reaction temperature, overcome the reaction time existing for general horizontal final polycondensation reaction kettle long, anti-
The shortcomings that answering temperature high with melt delay, the form and aspect of product are preferable, and regeneration high-contraction polyester items product quality indicator is stable.This
The obtained regeneration high-contraction polyester of embodiment can be used for high-shrinkage polyester filaments, short fine and high-contraction polyester film preparation, realize
The high-valued recycling of Waste Polyester.
Embodiment 3
As described in Example 1, except that：The molar percentage 1 of Waste Polyester and ethylene glycol:6, in alcoholysis kettle containing pair
PET and oligomer (mother liquor), the addition of wherein ethylene glycol terephthalate and oligomer (mother liquor) account for
Put into the 20% of Waste Polyester gross mass percentage, 190 DEG C of reaction temperature, 2 hours reaction time.Add 0.2 ‰ and (account for products therefrom
Mass percent) tripotassium phosphate ester stabilizer；220 DEG C of esterification reaction temperature, 1 hour reaction time, while add 15% and (account for
Products therefrom mass percent) M-phthalic acid (IPA), the DEG of 0.2% (accounting for products therefrom mass percent), make esterification
DEG content (accounting for products therefrom mass percent) in thing is 2.4%.Control polycondensation-I and the temperature of polycondensation-II are respectively
245th, 255 DEG C, the inherent viscosity 0.3 of prepolymer；Vertical whole polycondensation vessel, 260 DEG C of reaction temperature, 2 hours reaction time.Final
The inherent viscosity of the regeneration high-contraction polyester arrived is 0.605dl/g, 211.7 DEG C of fusing point, DEG content 2.9%, colourity b values 5.8
(the results are shown in Table 1, table 1 is regeneration high-contraction polyester synthesis condition and performance indications table).
Regeneration high-contraction polyester manufactured in the present embodiment has following features：1) a certain amount of mother is retained in alcoholysis kettle
Liquid, alcoholysis efficiency, stable alcoholysis product quality can be improved；2) due to the uncertainty of Waste Polyester raw material, the DEG of alcoholysis product
Content fluctuation is larger, by introducing DEG controlling of quality systems in carboxylate, ensure that the stabilization of DEG content；3) second two is utilized
After alcohol alcoholysis, the higher characteristic of DEG content, it is used as comonomer by adding M-phthalic acid (IPA), realizes regeneration high convergency
The production of polyester.4) from alcoholysis to esterification, again to polycondensation, using relatively low reaction temperature, the generation of accessory substance is effectively reduced；5)
Relatively low precondensation inherent viscosity is controlled, using efficient vertical liquid-phase tackifying kettle as final polycondensation reaction kettle, melt is reduced and exists
The residence time of final polycondensation reaction kettle and reaction temperature, overcome the reaction time existing for general horizontal final polycondensation reaction kettle long, anti-
The shortcomings that answering temperature high with melt delay, the form and aspect of product are preferable, and regeneration high-contraction polyester items product quality indicator is stable.This
The obtained regeneration high-contraction polyester of embodiment can be used for high-shrinkage polyester filaments, short fine and high-contraction polyester film preparation, realize
The high-valued recycling of Waste Polyester.
Embodiment 4
As described in Example 1, except that：The Isosorbide-5-Nitrae of 5% (accounting for products therefrom mass percent) is added in esterifying kettle
Cyclohexane dimethyl carbinol, and according to the content of DEG in alcoholysate, add the DEG of 0.3% (accounting for products therefrom mass percent), make
DEG content (accounting for products therefrom mass percent) in carboxylate is 2.5%.The characteristic of the regeneration high-contraction polyester finally given
Viscosity is 0.695dl/g, 228.1 DEG C of fusing point, DEG content 3.0%, colourity b values 5.3 (the results are shown in Table 1, table 1 is regeneration high convergency
Polyester synthesis condition and performance indications table).
Regeneration high-contraction polyester manufactured in the present embodiment has following features：1) a certain amount of mother is retained in alcoholysis kettle
Liquid, alcoholysis efficiency, stable alcoholysis product quality can be improved；2) due to the uncertainty of Waste Polyester raw material, the DEG of alcoholysis product
Content fluctuation is larger, by introducing DEG controlling of quality systems in carboxylate, ensure that the stabilization of DEG content；3) second two is utilized
After alcohol alcoholysis, the higher characteristic of DEG content, it is used as comonomer by adding Isosorbide-5-Nitrae cyclohexane dimethyl carbinol, realizes regeneration high convergency
The production of polyester.4) from alcoholysis to esterification, again to polycondensation, using relatively low reaction temperature, the generation of accessory substance is effectively reduced；5)
Relatively low precondensation inherent viscosity is controlled, using efficient vertical liquid-phase tackifying kettle as final polycondensation reaction kettle, melt is reduced and exists
The residence time of final polycondensation reaction kettle and reaction temperature, overcome the reaction time existing for general horizontal final polycondensation reaction kettle long, anti-
The shortcomings that answering temperature high with melt delay, the form and aspect of product are preferable, and regeneration high-contraction polyester items product quality indicator is stable.This
The obtained regeneration high-contraction polyester of embodiment can be used for high-shrinkage polyester filaments, short fine and high-contraction polyester film preparation, realize
The high-valued recycling of Waste Polyester.
Embodiment 5
As described in Example 2, except that：The 1 of 10% (accounting for products therefrom mass percent) is added in esterifying kettle,
4 cyclohexane dimethyl carbinols, and according to the content of DEG in alcoholysate, add the DEG of 0.2% (accounting for products therefrom mass percent), make
DEG content (accounting for products therefrom mass percent) in carboxylate is 2.5%.The characteristic of the regeneration high-contraction polyester finally given
Viscosity is 0.649dl/g, 219.0 DEG C of fusing point, DEG content 3.1%, colourity b values 5.4 (the results are shown in Table 1, table 1 is regeneration high convergency
Polyester synthesis condition and performance indications table).
Regeneration high-contraction polyester manufactured in the present embodiment has following features：1) a certain amount of mother is retained in alcoholysis kettle
Liquid, alcoholysis efficiency, stable alcoholysis product quality can be improved；2) due to the uncertainty of Waste Polyester raw material, the DEG of alcoholysis product
Content fluctuation is larger, by introducing DEG controlling of quality systems in carboxylate, ensure that the stabilization of DEG content；3) second two is utilized
After alcohol alcoholysis, the higher characteristic of DEG content, it is used as comonomer by adding Isosorbide-5-Nitrae cyclohexane dimethyl carbinol, realizes regeneration high convergency
The production of polyester.4) from alcoholysis to esterification, again to polycondensation, using relatively low reaction temperature, the generation of accessory substance is effectively reduced；5)
Relatively low precondensation inherent viscosity is controlled, using efficient vertical liquid-phase tackifying kettle as final polycondensation reaction kettle, melt is reduced and exists
The residence time of final polycondensation reaction kettle and reaction temperature, overcome the reaction time existing for general horizontal final polycondensation reaction kettle long, anti-
The shortcomings that answering temperature high with melt delay, the form and aspect of product are preferable, and regeneration high-contraction polyester items product quality indicator is stable.This
The obtained regeneration high-contraction polyester of embodiment can be used for high-shrinkage polyester filaments, short fine and high-contraction polyester film preparation, realize
The high-valued recycling of Waste Polyester.
Embodiment 6
As described in Example 3, except that：The 1 of 15% (accounting for products therefrom mass percent) is added in esterifying kettle,
4 cyclohexane dimethyl carbinols, and according to the content of DEG in alcoholysate, add the DEG of 0.1% (accounting for products therefrom mass percent), make
DEG content (accounting for products therefrom mass percent) in carboxylate is 2.4%.The characteristic of the regeneration high-contraction polyester finally given
Viscosity is 0.603dl/g, 212.3 DEG C of fusing point, DEG content 2.9%, colourity b values 5.6 (the results are shown in Table 1, table 1 is regeneration high convergency
Polyester synthesis condition and performance indications table).
Regeneration high-contraction polyester manufactured in the present embodiment has following features：1) a certain amount of mother is retained in alcoholysis kettle
Liquid, alcoholysis efficiency, stable alcoholysis product quality can be improved；2) due to the uncertainty of Waste Polyester raw material, the DEG of alcoholysis product
Content fluctuation is larger, by introducing DEG controlling of quality systems in carboxylate, ensure that the stabilization of DEG content；3) second two is utilized
After alcohol alcoholysis, the higher characteristic of DEG content, it is used as comonomer by adding Isosorbide-5-Nitrae cyclohexane dimethyl carbinol, realizes regeneration high convergency
The production of polyester.4) from alcoholysis to esterification, again to polycondensation, using relatively low reaction temperature, the generation of accessory substance is effectively reduced；5)
Relatively low precondensation inherent viscosity is controlled, using efficient vertical liquid-phase tackifying kettle as final polycondensation reaction kettle, melt is reduced and exists
The residence time of final polycondensation reaction kettle and reaction temperature, overcome the reaction time existing for general horizontal final polycondensation reaction kettle long, anti-
The shortcomings that answering temperature high with melt delay, the form and aspect of product are preferable, and regeneration high-contraction polyester items product quality indicator is stable.This
The obtained regeneration high-contraction polyester of embodiment can be used for high-shrinkage polyester filaments, short fine and high-contraction polyester film preparation, realize
The high-valued recycling of Waste Polyester.
Comparative example 1
As described in Example 1, except that：Using routine horizontal whole polycondensation vessel, 275 DEG C of controlling reaction temperature, very
0.1~1Kpa of reciprocal of duty cycle, 2.5 hours reaction time.Finally give regeneration high-contraction polyester inherent viscosity for 0.702dl/g,
227.1 DEG C of fusing point, DEG content 3.7%, colourity b values 6.8 (the results are shown in Table 1, table 1 is regeneration high-contraction polyester synthesis condition and property
Energy index table).
Comparative example 2
As described in Example 4, except that：Using routine horizontal whole polycondensation vessel, 275 DEG C of controlling reaction temperature, very
0.1~1Kpa of reciprocal of duty cycle, 2.5 hours reaction time.Finally give regeneration high-contraction polyester inherent viscosity for 0.695dl/g,
228.3 DEG C of fusing point, DEG content 3.6%, colourity b values 7.1 (the results are shown in Table 1, table 1 is regeneration high-contraction polyester synthesis condition and property
Energy index table).
It can see by comparative example 1,2, in order that regeneration high-contraction polyester reaches identical inherent viscosity, using routine
Horizontal whole polycondensation vessel when, reaction temperature is higher, the reaction time is longer so that DEG content is higher, colourity b values increase, Wu Fada
To the quality index of the regeneration high-contraction polyester of embodiment.
Table 1
Claims (4)
1. a kind of method that Waste Polyester alcoholysis method prepares regeneration high-contraction polyester, it is characterised in that comprise the following steps：1) give up poly-
The pretreatment of ester, the Waste Polyester block of cleaning is directly smashed into feed bin, the Waste Polyester fiber of cleaning is sent into material after being cut off
Storehouse, waste polyester bottle piece sorted, cleaned, being cleaned, being crushed, cut off after be sent into feed bin, then mix, for next procedure；
2) alcoholysis of Waste Polyester, by Waste Polyester：The molar percentage 1 of ethylene glycol:2~6 ratio input alcoholysis kettle, wherein in alcoholysis kettle
Containing accounting for the ethylene glycol terephthalate and oligomer of the mass percent of input Waste Polyester total amount 20~40%, and add alcoholysis
Catalyst；190~210 DEG C of controlling reaction temperature, 2~6 hours reaction time, obtain containing ethylene glycol terephthalate and oligomerisation
The alcoholysate of thing, is sent into esterifying kettle after filtering；3) addition of the controlling of quality and comonomer of carboxylate, control in esterifying kettle
220~240 DEG C of esterification reaction temperature, 1~2 hour reaction time, while add M-phthalic acid or Isosorbide-5-Nitrae cyclohexane dimethyl carbinol is total to
Polycondensation monomer, stabilizer, antioxidant；According to the actual content of diethylene glycol (DEG) in alcoholysate, diethylene glycol (DEG) is added, is made two in carboxylate sweet
Alcohol content is stable to account for 2.5 ± 0.3% scopes of products therefrom mass percent, and obtained carboxylate enters pre- after filtering again
Polycondensation vessel；4) preparation of polycondensation and section, by step 3) enter precondensation kettle carboxylate successively enter polycondensation-I and polycondensation-
II, control 240~260 DEG C, 1~100Kpa of vacuum of temperature, the inherent viscosity 0.2~0.4 of prepolymer；Subsequently into vertical end
Polycondensation vessel, 260~270 DEG C, 0.1~1Kpa of vacuum of controlling reaction temperature, 1.0~2.0 hours reaction time, then by molten
Body pumps out material, filtering, pelletizing, packaging；The inherent viscosity of the regeneration high-contraction polyester finally given is 0.60~0.70dl/g, melted
210~230 DEG C of point, diethylene glycol content are less than 6 in 3.0 ± 0.3%, colourity b values.
2. the method that a kind of Waste Polyester alcoholysis method as claimed in claim 1 prepares regeneration high-contraction polyester, it is characterised in that institute
The addition for the M-phthalic acid stated accounts for the 5~15% of products therefrom mass percent；Described Isosorbide-5-Nitrae cyclohexane dimethyl carbinol adds
Enter amount accounts for products therefrom mass percent 5~15%.
3. the method that a kind of Waste Polyester alcoholysis method as claimed in claim 1 prepares regeneration high-contraction polyester, it is characterised in that institute
The addition for the alcoholysis catalysts stated accounts for the 2 ‰ of products therefrom mass percent；The addition of described stabilizer accounts for gained and produced
The 0.2 ‰ of amount of substance percentage；The addition of described antioxidant accounts for the 0.5 ‰ of products therefrom mass percent；Described alcohol
Solution catalyst uses acetic acid saline catalyst；Described stabilizer is using one in triphenyl phosphate, phosphorous acid, trimethyl phosphate
Kind；Described antioxidant uses the antioxidant of hindered phenolic.
4. the method that a kind of Waste Polyester alcoholysis method as claimed in claim 3 prepares regeneration high-contraction polyester, it is characterised in that institute
The alcoholysis catalysts stated use zinc acetate；Described stabilizer uses triphenyl phosphate；Described antioxidant uses antioxidant
1010。
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