CN107652422B - A kind of method that Waste Polyester alcoholysis method prepares cation regenerant dyeable polyester - Google Patents
A kind of method that Waste Polyester alcoholysis method prepares cation regenerant dyeable polyester Download PDFInfo
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- CN107652422B CN107652422B CN201710841873.9A CN201710841873A CN107652422B CN 107652422 B CN107652422 B CN 107652422B CN 201710841873 A CN201710841873 A CN 201710841873A CN 107652422 B CN107652422 B CN 107652422B
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- 229920000728 polyester Polymers 0.000 title claims abstract description 138
- 238000006136 alcoholysis reaction Methods 0.000 title claims abstract description 72
- 239000002699 waste material Substances 0.000 title claims abstract description 63
- 150000001768 cations Chemical class 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 51
- 239000012492 regenerant Substances 0.000 title claims abstract description 44
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 229
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 34
- 150000007942 carboxylates Chemical class 0.000 claims abstract description 25
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 23
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 23
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 239000000835 fiber Substances 0.000 claims abstract description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 33
- 230000035484 reaction time Effects 0.000 claims description 22
- 238000005886 esterification reaction Methods 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 11
- 239000003381 stabilizer Substances 0.000 claims description 11
- 239000003963 antioxidant agent Substances 0.000 claims description 10
- 230000003078 antioxidant effect Effects 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000000654 additive Substances 0.000 claims description 8
- 230000000996 additive effect Effects 0.000 claims description 8
- 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
- 230000006641 stabilisation Effects 0.000 claims description 7
- 238000011105 stabilization Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 150000002148 esters Chemical class 0.000 claims description 4
- 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 4
- 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
- 238000007599 discharging 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
- 238000004806 packaging method and process Methods 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
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 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 9
- 239000000047 product Substances 0.000 description 46
- 238000004519 manufacturing process Methods 0.000 description 14
- 239000012452 mother liquor Substances 0.000 description 14
- 230000032050 esterification Effects 0.000 description 11
- 239000002994 raw material Substances 0.000 description 9
- 239000000975 dye Substances 0.000 description 8
- 230000034659 glycolysis Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000006227 byproduct Substances 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 6
- LZFNKJKBRGFWDU-UHFFFAOYSA-N 3,6-dioxabicyclo[6.3.1]dodeca-1(12),8,10-triene-2,7-dione Chemical compound O=C1OCCOC(=O)C2=CC=CC1=C2 LZFNKJKBRGFWDU-UHFFFAOYSA-N 0.000 description 5
- -1 Polyethylene terephthalate Polymers 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000004043 dyeing Methods 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 5
- 239000000155 melt Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 230000008929 regeneration Effects 0.000 description 4
- 238000011069 regeneration method Methods 0.000 description 4
- 230000000717 retained effect Effects 0.000 description 4
- LLLVZDVNHNWSDS-UHFFFAOYSA-N 4-methylidene-3,5-dioxabicyclo[5.2.2]undeca-1(9),7,10-triene-2,6-dione Chemical compound C1(C2=CC=C(C(=O)OC(=C)O1)C=C2)=O LLLVZDVNHNWSDS-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 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
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 229920000229 biodegradable polyester Polymers 0.000 description 2
- 239000004622 biodegradable polyester Substances 0.000 description 2
- 125000002091 cationic group Chemical group 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
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229920001634 Copolyester Polymers 0.000 description 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 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
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 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
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000006140 methanolysis reaction Methods 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 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
- 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
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/688—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur
- C08G63/6884—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/6886—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
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/83—Alkali metals, alkaline earth metals, beryllium, magnesium, copper, silver, gold, zinc, cadmium, mercury, manganese, or compounds thereof
-
- 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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- 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)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Polyesters Or Polycarbonates (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention discloses a kind of methods that Waste Polyester alcoholysis method prepares cation regenerant dyeable polyester, include the following steps: the pretreatment of 1) Waste Polyester；2) alcoholysis of Waste Polyester；3) controlling of quality of carboxylate and the addition of 5-sodium sulfo isophthalate and polyethylene glycol as comonomer；4) preparation of polycondensation and slice；The inherent viscosity of finally obtained cation regenerant dyeable polyester be 0.55 ~ 0.65 dl/g, 220 ~ 230 DEG C of fusing point, diethylene glycol content in 5.5 ± 0.3%, coloration b value less than 8.Cation regenerant dyeable polyester produced by the present invention can be used for the preparation of cation dyeable polyester long filament, short fibre, realize the high-valued recycling of Waste Polyester.
Description
Technical field
The present invention relates to a kind of methods that Waste Polyester alcoholysis method prepares cation regenerant dyeable polyester, belong to Waste Polyester
Recycling field.
Background technique
Polyethylene terephthalate (PET, abbreviation polyester) is widely used in beverage bottle, fibre as important raw material
The production of dimension, film, sheet material etc..Processing, use process with the rapid development of polyester industrial, in production of polyester and product
In, the polyester waste material of generation is also skyrocketed through.Since polyester has very strong chemical inertness, natural storage is difficult degradation or micro-
Biological decomposition not only causes the huge wasting of resources, but also generates serious environmental pollution.Therefore, by recycling with reality
Existing resource benign cycle, improves environmental quality, becomes the important topic of current polyester industrial.
Utilizing at present to Reclaim of PET Scrap mainly has physical method and chemical method.Physical method 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 generally 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.For this purpose, publication number CN106113319A is disclosed
" containing waste textile reclaiming technique is washed " polyester waste material, spent glycol will complete alcoholysis, ester in alcoholysis kettle after processing
Change, after polycondensation and multistage filtering, obtains recycled polyester.In order to enrich the kind of recycled polyester, publication number CN102153734A is public
Opened " a method of Biodegradable polyester is prepared by post-consumer polyester ", oligomer is 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 method of prepare composite fibre water-soluble polyester with Waste Polyester ", by Waste Polyester second two
Alcohol carries out alcoholysis and obtains ethylene glycol terephthalate, and the 5-sodium sulfo isophthalate of certain mass percent is then added
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 cationic dye capable of dyeing recycled polyester ", wherein the cationic dye capable of dyeing recycled polyester of cortex is with recycled polyester
It is made in degradation of ethylene glycol method by adding specific comonomer for raw material.
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, there are recycled polyester form and aspect to be deteriorated, the big, fusing point of by-product diethylene glycol (DEG) (DEG) content fluctuation
The problems such as not easy to control, decline product quality.
Therefore, how to solve the problems, such as Waste Polyester alcoholysis method regenerative process, and according to obtaining after Waste Polyester alcoholysis
Oligomer characteristic, carry out copolyesters research preparation, be the emphasis of recycled polyester area research and breakthrough.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of Waste Polyester alcoholysis methods to prepare cation regenerant dye capable of dyeing
The method of polyester, cation regenerant dyeable polyester produced by the present invention can be used for cation dyeable polyester long filament, short
Fine preparation, realizes the high-valued recycling of Waste Polyester.
In order to solve the above-mentioned technical problem used technical solution is the present invention:
A kind of method that Waste Polyester alcoholysis method prepares cation regenerant dyeable polyester includes the following steps: 1) to give up poly-
Clean Waste Polyester block is directly smashed into feed bin in the pretreatment of ester, and clean Waste Polyester fiber 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, in Waste Polyester: the ratio of molar percentage 1:2~6 of ethylene glycol puts into alcoholysis kettle, wherein in alcoholysis kettle
It is (following containing the ethylene glycol terephthalate (BHET) and oligomer for accounting for investment 20~40% mass percent of Waste Polyester total amount
Claim mother liquor), and add alcoholysis catalysts；190~210 DEG C of reaction temperature, 2~6 hours reaction time are controlled, is obtained containing to benzene two
The alcoholysate of formic acid glycol ester (BHET) and oligomer, is sent into esterifying kettle after filtering；3) controlling of quality of carboxylate is together
The addition of polycondensation monomer controls 220~240 DEG C of esterification reaction temperature, 1~2 hour reaction time in esterifying kettle, while adding isophthalic
Dioctyl phthalate -5- sodium sulfonate (SIPA) and polyethylene glycol (PEG) are used as comonomer, stabilizer, antioxidant；According in alcoholysate two
The actual content of glycol (DEG) adds diethylene glycol (DEG) (DEG), and diethylene glycol (DEG) (DEG) stable content in carboxylate is made to account for gained production
5.0 ± 0.3% range of amount of substance percentage, obtained carboxylate enter precondensation kettle after filtering again；4) polycondensation and slice
The carboxylate that step 3) enters precondensation kettle is successively entered polycondensation-I and polycondensation-II, controls 240~260 DEG C of temperature by preparation,
1~100Kpa of vacuum degree, the inherent viscosity 0.2~0.4 of prepolymer；Subsequently into vertical whole polycondensation vessel, reaction temperature 260 is controlled
~270 DEG C, 0.1~1Kpa of vacuum degree, the reaction time 1.0~2.0 hours, then pass through Melt Pump discharging, filtering, pelletizing, packet
Dress；The inherent viscosity of finally obtained cation regenerant dyeable polyester be 0.55~0.65dl/g, 220~230 DEG C of fusing point,
DEG content is in 5.5 ± 0.3%, coloration b value less than 8.
The additional amount of the 5-sodium sulfo isophthalate (SIPA) accounts for the 2~5% of products therefrom mass percent；
The additional amount of the polyethylene glycol (PEG) accounts for the 4~10% of products therefrom mass percent.
The additive amount of the alcoholysis catalysts accounts for the 2 ‰ of products therefrom mass percent；The addition of the stabilizer
Amount accounts for the 0.2 ‰ of products therefrom mass percent；The additive amount of the antioxidant accounts for products therefrom mass percent
0.5‰；The alcoholysis catalysts use acetic acid saline catalyst；The stabilizer uses triphenyl phosphate, phosphorous acid, phosphorus
One of sour trimethyl；The antioxidant uses the antioxidant of hindered phenolic.
The alcoholysis catalysts preferably use zinc acetate；The stabilizer preferably uses triphenyl phosphate；Described
Antioxidant preferably uses antioxidant 1010 (being purchased from beneficial (Guangzhou) the chemical materials Co., Ltd in day).
The invention has the benefit that 1) retain a certain amount of mother liquor in alcoholysis kettle, alcoholysis efficiency, stabilization 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 system is introduced in object, ensure that the stabilization of DEG content；3) using after glycolysis alcoholysis, DEG content is higher
Characteristic realizes that cation regenerant dye capable of dyeing is poly- by adding 5-sodium sulfo isophthalate (SIPA), polyethylene glycol (PEG)
The production of ester.Simultaneously because in carboxylate EG content it is higher, so using the method for directly addition SIPA esterification, change it is general positive from
When sub- dyeable polyester produces, need SIPA to be reacted with EG in advance obtained ethylene isophthalate -5- sodium sulfonate
(SIPE) method reduces auxiliary material and deploys link；4) from alcoholysis to esterification, again to polycondensation, using lower reaction temperature, effectively
Reduce the generation of by-product；5) lower precondensation inherent viscosity is controlled, using efficient vertical liquid-phase tackifying kettle as final minification
Poly- reaction kettle reduces residence time and reaction temperature of the melt in final polycondensation reaction kettle, overcomes general horizontal final polycondensation reaction kettle
The shortcomings that existing reaction time is long, reaction temperature is high and melt is detained, the form and aspect of product are preferable, cation regenerant dye capable of dyeing
Polyester items product quality indicator is stablized.Cation regenerant dyeable polyester produced by the present invention can be used for the dye of positive ion can
The preparation for contaminating polyester filament, short fibre, realizes the high-valued recycling of Waste Polyester.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Illustrate with reference to embodiments, but does not limit the present invention.
The performance indexes of cation regenerant dyeable polyester slice, is cut by GBT 14190-2008 fiber-grade polyester
Piece (PET) test method executes.
Embodiment 1
The method that a kind of Waste Polyester alcoholysis method of the present embodiment prepares cation regenerant dyeable polyester, as shown in Figure 1,
Clean Waste Polyester block is directly smashed into feed bin in the pretreatment for including the following steps: 1) Waste Polyester, and clean Waste Polyester is fine
Dimension is sent into feed bin after being cut off, waste polyester bottle piece sorted, cleaned, being cleaned, being crushed, cut off after be sent into feed bin, then mix
Ingredient is closed, for next procedure；2) alcoholysis of Waste Polyester, by pretreated Waste Polyester, by Waste Polyester, (Waste Polyester is added in mouth 7
It is added) ratio investment alcoholysis kettle 1 with the molar percentage 1:2 of ethylene glycol (ethylene glycol be added mouth 6 in be added), in alcoholysis kettle 1
Containing ethylene glycol terephthalate and oligomer (mother liquor) (the first additive is added in mouth 8 and is added), wherein terephthalic acid (TPA)
The additional amount of glycol ester and oligomer (mother liquor) accounts for the 40% of investment Waste Polyester gross mass percentage, alcoholysis catalysts zinc acetate
Additive amount be 2 ‰ (accounting for products therefrom mass percent) (the first additive be added mouth 8 in be added).Control reaction temperature 210
DEG C, the reaction time 6 hours, obtain the alcoholysate containing BHET and oligomer, after filtering be sent into esterifying kettle 2；3) matter of carboxylate
The addition of amount regulation and comonomer, controls and controls 240 DEG C of esterification reaction temperature, 2 hours reaction time in esterifying kettle 2, simultaneously
The 5-sodium sulfo isophthalate (SIPA) and 10% of 2% (accounting for products therefrom mass percent) of addition (accounts for products therefrom quality
Percentage) polyethylene glycol (PEG) (comonomer be added mouth 9 in be added), the phosphorus of 0.2 ‰ (accounting for products therefrom mass percent)
Triphenyl phosphate ester stabilizer (Second addition is added in mouth 10 and is added) and 0.5 ‰ (accounting for products therefrom mass percent) antioxidant
1010 (Second addition is added in mouth 10 and is added), and according to the content of DEG in alcoholysate, addition 0.4% (accounts for products therefrom matter
Amount percentage) DEG (Second addition be added mouth 10 in be added), so that the DEG content in carboxylate (is accounted for products therefrom quality hundred
Divide ratio) it is 5.1%, obtained carboxylate enters precondensation kettle after filtering again；4) preparation of polycondensation and slice, by step 3) into
The carboxylate for entering precondensation kettle successively enters polycondensation-I and polycondensation-II (prepolymerization reaction kettle-I 3 and prepolymerization reaction kettle-II 4),
The temperature for controlling polycondensation-I and polycondensation-II is respectively 240,250 DEG C, 1~100Kpa of vacuum degree, the inherent viscosity 0.4 of prepolymer；
Subsequently into vertical whole polycondensation vessel 5,270 DEG C of reaction temperature, 0.1~1Kpa of vacuum degree, the reaction time 1.0 hours are controlled, then
Pass through Melt Pump discharging, filtering, pelletizing, packaging；The inherent viscosity of finally obtained cation regenerant dyeable polyester is
0.648dl/g, 228.9 DEG C of fusing point, DEG content 5.4%, coloration b value 7.1 (the results are shown in Table 1, table 1 is that cation regenerant dyestuff can
Contaminate polyester synthesis condition and table of performance indicators).
1) cation regenerant dyeable polyester manufactured in the present embodiment has a characteristic that be retained centainly in alcoholysis kettle
The mother liquor of amount can be improved alcoholysis efficiency, stablize alcoholysis product quality；2) due to the uncertainty of Waste Polyester raw material, alcoholysis is produced
The DEG content fluctuation of object is larger, by introducing DEG controlling of quality system in carboxylate, ensure that the stabilization of DEG content；3)
After glycolysis alcoholysis, the higher characteristic of DEG content, by adding 5-sodium sulfo isophthalate (SIPA), polyethylene glycol
(PEG), the production of cation regenerant dyeable polyester is realized.Simultaneously because in carboxylate EG content it is higher, so using direct
Add SIPA esterification method, change general cation dyeable polyester production when, need in advance SIPA with EG the system of reacting
The method for obtaining ethylene isophthalate -5- sodium sulfonate (SIPE) reduces auxiliary material and deploys link；4) from alcoholysis to esterification, again
The generation of by-product is effectively reduced using lower reaction temperature to polycondensation；5) lower precondensation inherent viscosity is controlled, is adopted
It uses efficient vertical liquid-phase tackifying kettle as final polycondensation reaction kettle, reduces residence time and reaction of the melt in final polycondensation reaction kettle
Temperature overcomes the shortcomings that reaction time existing for general horizontal final polycondensation reaction kettle is long, reaction temperature is high and melt is detained, product
Form and aspect it is preferable, cation regenerant dyeable polyester items product quality indicator stablize.The present embodiment regeneration sun obtained from
Sub- dyeable polyester can be used for the preparation of cation dyeable polyester long filament, short fibre, realize the high-valued recycling of Waste Polyester
It utilizes.
Embodiment 2
As described in Example 1, except that: the molar percentage 1:4 of Waste Polyester and ethylene glycol, in alcoholysis kettle containing pair
Ethylene terephthalate and oligomer (mother liquor), wherein the additional amount of ethylene glycol terephthalate and oligomer (mother liquor) accounts for
Put into the 30% of Waste Polyester gross mass percentage, 200 DEG C of reaction temperature, 4 hours reaction time.It is added 0.2 ‰ and (accounts for products therefrom
Mass percent) phosphorous acid stabilizer；230 DEG C of esterification reaction temperature, 1.5 hours reaction time, while adding 3% and (accounting for institute
Product quality percentage) SIPA and 8% (accounting for products therefrom mass percent) PEG, 0.3% (accounts for products therefrom quality hundred
Point ratio) DEG, making DEG content (accounting for products therefrom mass percent) in carboxylate is 5.0%.Control polycondensation-I and polycondensation-
II temperature is respectively 250,260 DEG C, the inherent viscosity 0.2 of prepolymer；Vertical whole polycondensation vessel, 265 DEG C of reaction temperature, when reaction
Between 1.5 hours.The inherent viscosity of finally obtained cation regenerant dyeable polyester be 0.617dl/g, 225.3 DEG C of fusing point,
DEG content 5.5%, coloration b value 7.3.(it the results are shown in Table 1, table 1 is cation regenerant dyeable polyester synthesis condition and performance
Index table).
1) cation regenerant dyeable polyester manufactured in the present embodiment has a characteristic that be retained centainly in alcoholysis kettle
The mother liquor of amount can be improved alcoholysis efficiency, stablize alcoholysis product quality；2) due to the uncertainty of Waste Polyester raw material, alcoholysis is produced
The DEG content fluctuation of object is larger, by introducing DEG controlling of quality system in carboxylate, ensure that the stabilization of DEG content；3)
After glycolysis alcoholysis, the higher characteristic of DEG content, by adding 5-sodium sulfo isophthalate (SIPA), polyethylene glycol
(PEG), the production of cation regenerant dyeable polyester is realized.Simultaneously because in carboxylate EG content it is higher, so using direct
Add SIPA esterification method, change general cation dyeable polyester production when, need in advance SIPA with EG the system of reacting
The method for obtaining ethylene isophthalate -5- sodium sulfonate (SIPE) reduces auxiliary material and deploys link；4) from alcoholysis to esterification, again
The generation of by-product is effectively reduced using lower reaction temperature to polycondensation；5) lower precondensation inherent viscosity is controlled, is adopted
It uses efficient vertical liquid-phase tackifying kettle as final polycondensation reaction kettle, reduces residence time and reaction of the melt in final polycondensation reaction kettle
Temperature overcomes the shortcomings that reaction time existing for general horizontal final polycondensation reaction kettle is long, reaction temperature is high and melt is detained, product
Form and aspect it is preferable, cation regenerant dyeable polyester items product quality indicator stablize.The present embodiment regeneration sun obtained from
Sub- dyeable polyester can be used for the preparation of cation dyeable polyester long filament, short fibre, realize the high-valued recycling of Waste Polyester
It utilizes.
Embodiment 3
As described in Example 1, except that: the molar percentage 1:6 of Waste Polyester and ethylene glycol, in alcoholysis kettle containing pair
Ethylene terephthalate and oligomer (mother liquor), wherein the additional amount of ethylene glycol terephthalate and oligomer (mother liquor) accounts for
Put into the 20% of Waste Polyester gross mass percentage, 190 DEG C of reaction temperature, 2 hours reaction time.It is added 0.2 ‰ and (accounts for products therefrom
Mass percent) tripotassium phosphate ester stabilizer；220 DEG C of esterification reaction temperature, 1 hour reaction time, while adding 4% and (accounting for
Products therefrom mass percent) SIPA and 6% (accounting for products therefrom mass percent) PEG, 0.2% (accounts for products therefrom quality
Percentage) DEG, making DEG content (accounting for products therefrom mass percent) in carboxylate is 5.2%.Control polycondensation-I and contracting
Poly- II temperature is respectively 245,255 DEG C, the inherent viscosity 0.3 of prepolymer；Vertical whole polycondensation vessel, 260 DEG C of reaction temperature, instead
Answer time 2 h.The inherent viscosity of finally obtained cation regenerant dyeable polyester is 0.589dl/g, fusing point 223.8
DEG C, DEG content 5.6%, coloration b value 7.4 (the results are shown in Table 1, table 1 is cation regenerant dyeable polyester synthesis condition and property
Energy index table).
1) cation regenerant dyeable polyester manufactured in the present embodiment has a characteristic that be retained centainly in alcoholysis kettle
The mother liquor of amount can be improved alcoholysis efficiency, stablize alcoholysis product quality；2) due to the uncertainty of Waste Polyester raw material, alcoholysis is produced
The DEG content fluctuation of object is larger, by introducing DEG controlling of quality system in carboxylate, ensure that the stabilization of DEG content；3)
After glycolysis alcoholysis, the higher characteristic of DEG content, by adding 5-sodium sulfo isophthalate (SIPA), polyethylene glycol
(PEG), the production of cation regenerant dyeable polyester is realized.Simultaneously because in carboxylate EG content it is higher, so using direct
Add SIPA esterification method, change general cation dyeable polyester production when, need in advance SIPA with EG the system of reacting
The method for obtaining ethylene isophthalate -5- sodium sulfonate (SIPE) reduces auxiliary material and deploys link；4) from alcoholysis to esterification, again
The generation of by-product is effectively reduced using lower reaction temperature to polycondensation；5) lower precondensation inherent viscosity is controlled, is adopted
It uses efficient vertical liquid-phase tackifying kettle as final polycondensation reaction kettle, reduces residence time and reaction of the melt in final polycondensation reaction kettle
Temperature overcomes the shortcomings that reaction time existing for general horizontal final polycondensation reaction kettle is long, reaction temperature is high and melt is detained, product
Form and aspect it is preferable, cation regenerant dyeable polyester items product quality indicator stablize.The present embodiment regeneration sun obtained from
Sub- dyeable polyester can be used for the preparation of cation dyeable polyester long filament, short fibre, realize the high-valued recycling of Waste Polyester
It utilizes.
Embodiment 4
As described in Example 1, except that: the molar percentage 1:4 of Waste Polyester and ethylene glycol, in alcoholysis kettle containing pair
Ethylene terephthalate and oligomer (mother liquor), wherein the additional amount of ethylene glycol terephthalate and oligomer (mother liquor) accounts for
Put into the 30% of Waste Polyester gross mass percentage, 200 DEG C of reaction temperature, 4 hours reaction time.It is 230 DEG C of esterification reaction temperature, anti-
1.5 hours between seasonable, while the SIPA and 4% for adding 5% (accounting for products therefrom mass percent) (accounts for products therefrom quality percentage
Than) PEG, according to the content of DEG in alcoholysate, the DEG of 0.1% (accounting for products therefrom mass percent) of addition makes in carboxylate
DEG content (accounting for products therefrom mass percent) be 5.1%.Vertical whole polycondensation vessel, 265 DEG C of reaction temperature, the reaction time 1.5
Hour.The inherent viscosity of finally obtained cation regenerant dyeable polyester is 0.554dl/g, 221.1 DEG C of fusing point, DEG contain
Measure 5.7%, coloration b value 7.5.(it the results are shown in Table 1, table 1 is cation regenerant dyeable polyester synthesis condition and performance indicator
Table).
1) cation regenerant dyeable polyester manufactured in the present embodiment has a characteristic that be retained centainly in alcoholysis kettle
The mother liquor of amount can be improved alcoholysis efficiency, stablize alcoholysis product quality；2) due to the uncertainty of Waste Polyester raw material, alcoholysis is produced
The DEG content fluctuation of object is larger, by introducing DEG controlling of quality system in carboxylate, ensure that the stabilization of DEG content；3)
After glycolysis alcoholysis, the higher characteristic of DEG content, by adding 5-sodium sulfo isophthalate (SIPA), polyethylene glycol
(PEG), the production of cation regenerant dyeable polyester is realized.Simultaneously because in carboxylate EG content it is higher, so using direct
Add SIPA esterification method, change general cation dyeable polyester production when, need in advance SIPA with EG the system of reacting
The method for obtaining ethylene isophthalate -5- sodium sulfonate (SIPE) reduces auxiliary material and deploys link；4) from alcoholysis to esterification, again
The generation of by-product is effectively reduced using lower reaction temperature to polycondensation；5) lower precondensation inherent viscosity is controlled, is adopted
It uses efficient vertical liquid-phase tackifying kettle as final polycondensation reaction kettle, reduces residence time and reaction of the melt in final polycondensation reaction kettle
Temperature overcomes the shortcomings that reaction time existing for general horizontal final polycondensation reaction kettle is long, reaction temperature is high and melt is detained, product
Form and aspect it is preferable, cation regenerant dyeable polyester items product quality indicator stablize.The present embodiment regeneration sun obtained from
Sub- dyeable polyester can be used for the preparation of cation dyeable polyester long filament, short fibre, realize the high-valued recycling of Waste Polyester
It utilizes.
Comparative example 1
As described in Example 1, except that: using conventional horizontal whole polycondensation vessel, control 275 DEG C of reaction temperature, very
0.1~1Kpa of reciprocal of duty cycle, the reaction time 2.5 hours.The inherent viscosity of finally obtained cation regenerant dyeable polyester is
0.647dl/g, 224.9 DEG C of fusing point, DEG content 6.5%, coloration b value 10.5 (the results are shown in Table 1, table 1 is cation regenerant dyestuff
Dyeable polyester synthesis condition and table of performance indicators).
It can be seen that, in order to make cation regenerant dyeable polyester reach identical inherent viscosity, adopted by comparing example 1
When with conventional horizontal whole polycondensation vessel, reaction temperature is higher, the reaction time is longer, so that DEG content is higher, coloration b value increases,
It is unable to reach the quality index of the cation regenerant dyeable polyester of embodiment.
Table 1
Claims (4)
1. a kind of method that Waste Polyester alcoholysis method prepares cation regenerant dyeable polyester, which is characterized in that including walking as follows
Rapid: 1) clean Waste Polyester block is directly smashed into feed bin in the pretreatment of Waste Polyester, and clean Waste Polyester fiber is cut off
After 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, under
Procedure；2) alcoholysis of Waste Polyester, in Waste Polyester: the ratio of molar percentage 1:2~6 of ethylene glycol puts into alcoholysis kettle, wherein
Containing the ethylene glycol terephthalate and oligomer for accounting for investment 20~40% mass percent of Waste Polyester total amount in alcoholysis kettle, and
Add alcoholysis catalysts；190~210 DEG C of reaction temperature, 2~6 hours reaction time are controlled, is obtained containing terephthalate
The alcoholysate of ester and oligomer, is sent into esterifying kettle after filtering；3) addition of the controlling of quality and comonomer of carboxylate, control
220~240 DEG C of esterification reaction temperature, 1~2 hour reaction time in esterifying kettle, at the same add 5-sodium sulfo isophthalate,
Polyethylene glycol, stabilizer, antioxidant, wherein 5-sodium sulfo isophthalate and polyethylene glycol are as comonomer；According to alcoholysis
The actual content of diethylene glycol (DEG) in object adds diethylene glycol (DEG), and the diethylene glycol content stabilization in carboxylate is made to account for products therefrom quality
5.0 ± 0.3% ranges, obtained carboxylate enter precondensation kettle after filtering again；4) preparation of polycondensation and slice, by step 3)
Carboxylate into precondensation kettle successively enters polycondensation-I and polycondensation-II, controls 240~260 DEG C of temperature, and vacuum degree 1~
100Kpa, the inherent viscosity 0.2~0.4 of prepolymer；Subsequently into vertical whole polycondensation vessel, 260~270 DEG C of reaction temperature are controlled,
0.1~1Kpa of vacuum degree the reaction time 1.0~2.0 hours, then passes through Melt Pump discharging, filtering, pelletizing, packaging；Final
To cation regenerant dyeable polyester inherent viscosity be 0.55~0.65dl/g, 220~230 DEG C of fusing point, diethylene glycol (DEG) contain
Amount is in 5.5 ± 0.3%, coloration b value less than 8.
2. a kind of method that Waste Polyester alcoholysis method prepares cation regenerant dyeable polyester as described in claim 1, special
Sign is that the additional amount of the 5-sodium sulfo isophthalate accounts for the 2~5% of products therefrom mass percent；Described is poly-
The additional amount of ethylene glycol accounts for the 4~10% of products therefrom quality.
3. a kind of method that Waste Polyester alcoholysis method prepares cation regenerant dyeable polyester as described in claim 1, special
Sign is that the additive amount of the alcoholysis catalysts accounts for the 2 ‰ of products therefrom quality；The additive amount of the stabilizer accounts for gained
The 0.2 ‰ of product quality；The additive amount of the antioxidant accounts for the 0.5 ‰ of products therefrom quality；The alcoholysis catalysts are adopted
With acetic acid saline catalyst；The stabilizer uses one of triphenyl phosphate, phosphorous acid, trimethyl phosphate；Described
Antioxidant uses the antioxidant of hindered phenolic.
4. a kind of method that Waste Polyester alcoholysis method prepares cation regenerant dyeable polyester as claimed in claim 3, special
Sign is that the alcoholysis catalysts use zinc acetate；The stabilizer uses triphenyl phosphate；The antioxidant uses
Antioxidant 1010.
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| WO2021038512A1 (en) * | 2019-08-28 | 2021-03-04 | Sanjay Tammaji Kulkarni | A process for manufacturing specialty polyesters & co-polyesters from recycled bis 2-hydroxyethyl terephthalate (rbhet) and product thereof |
| CN110964188B (en) * | 2019-11-25 | 2022-10-28 | 浙江佳人新材料有限公司 | Production method of cyclic regeneration cation slice |
| CN111088545B (en) * | 2019-12-12 | 2022-05-06 | 浙江恒逸石化研究院有限公司 | Preparation method of cationic dye dyeable regenerated cotton-like polyester fiber |
| CN115141363A (en) * | 2021-03-30 | 2022-10-04 | 科泽新材料股份有限公司 | Method for preparing regenerated cationic polyester by using waste polyester |
| CN115232298A (en) * | 2021-04-22 | 2022-10-25 | 浙江安吉华逸化纤有限公司 | Method for preparing regenerated cationic dyeable polyester chip from waste polyester material and product |
| CN113214458B (en) * | 2021-04-30 | 2022-02-08 | 东华大学 | Method for preparing regenerated polyester by efficiently alcoholysis of waste polyester |
| CN113550022B (en) * | 2021-09-22 | 2021-12-07 | 苏州宝丽迪材料科技股份有限公司 | Preparation method of cation-dyeable regenerated polyester fiber and product thereof |
| CN114835885A (en) * | 2022-06-21 | 2022-08-02 | 绍兴九洲化纤有限公司 | Method for preparing normal-pressure dyeable polyester and producing superfine fiber by using polyester reclaimed material |
| CN118007260B (en) * | 2024-04-10 | 2024-07-02 | 安徽保尔盈新材料科技有限公司 | Method for producing composite low-melting-point polyester filaments by using regenerated polyester bottle flakes |
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