CN109467740A - Recovery method of waste polyester-cotton blended fabric - Google Patents
Recovery method of waste polyester-cotton blended fabric Download PDFInfo
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- CN109467740A CN109467740A CN201710807076.9A CN201710807076A CN109467740A CN 109467740 A CN109467740 A CN 109467740A CN 201710807076 A CN201710807076 A CN 201710807076A CN 109467740 A CN109467740 A CN 109467740A
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- terylene
- recovery method
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- cotton
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- 238000000034 method Methods 0.000 title claims abstract description 84
- 229920000742 Cotton Polymers 0.000 title claims abstract description 67
- 238000011084 recovery Methods 0.000 title claims abstract description 60
- 239000002699 waste material Substances 0.000 title claims abstract description 29
- 239000004744 fabric Substances 0.000 title abstract description 7
- 229920004933 Terylene® Polymers 0.000 claims abstract description 79
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 79
- 239000007787 solid Substances 0.000 claims abstract description 39
- 229920000728 polyester Polymers 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 150000002148 esters Chemical class 0.000 claims description 34
- 239000002904 solvent Substances 0.000 claims description 32
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 20
- 235000019441 ethanol Nutrition 0.000 claims description 20
- 150000002191 fatty alcohols Chemical class 0.000 claims description 17
- 238000004090 dissolution Methods 0.000 claims description 14
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 14
- -1 isopropyl ester One Chemical compound 0.000 claims description 13
- 230000020764 fibrinolysis Effects 0.000 claims description 12
- 229920003043 Cellulose fiber Polymers 0.000 claims description 10
- 239000003963 antioxidant agent Substances 0.000 claims description 10
- 230000003078 antioxidant effect Effects 0.000 claims description 10
- ZTHYODDOHIVTJV-UHFFFAOYSA-N Propyl gallate Chemical compound CCCOC(=O)C1=CC(O)=C(O)C(O)=C1 ZTHYODDOHIVTJV-UHFFFAOYSA-N 0.000 claims description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 8
- 229940074391 gallic acid Drugs 0.000 claims description 7
- 235000004515 gallic acid Nutrition 0.000 claims description 7
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 claims description 6
- UDEWPOVQBGFNGE-UHFFFAOYSA-N benzoic acid n-propyl ester Natural products CCCOC(=O)C1=CC=CC=C1 UDEWPOVQBGFNGE-UHFFFAOYSA-N 0.000 claims description 6
- XSIFPSYPOVKYCO-UHFFFAOYSA-N butyl benzoate Chemical compound CCCCOC(=O)C1=CC=CC=C1 XSIFPSYPOVKYCO-UHFFFAOYSA-N 0.000 claims description 6
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims description 6
- 238000009987 spinning Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- MTZQAGJQAFMTAQ-UHFFFAOYSA-N ethyl benzoate Chemical compound CCOC(=O)C1=CC=CC=C1 MTZQAGJQAFMTAQ-UHFFFAOYSA-N 0.000 claims description 4
- OLXYLDUSSBULGU-UHFFFAOYSA-N methyl pyridine-4-carboxylate Chemical compound COC(=O)C1=CC=NC=C1 OLXYLDUSSBULGU-UHFFFAOYSA-N 0.000 claims description 4
- 235000010388 propyl gallate Nutrition 0.000 claims description 4
- 239000000473 propyl gallate Substances 0.000 claims description 4
- 229940075579 propyl gallate Drugs 0.000 claims description 4
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 claims description 4
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 3
- FEXQDZTYJVXMOS-UHFFFAOYSA-N Isopropyl benzoate Chemical compound CC(C)OC(=O)C1=CC=CC=C1 FEXQDZTYJVXMOS-UHFFFAOYSA-N 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 3
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 claims description 3
- 229960001826 dimethylphthalate Drugs 0.000 claims description 3
- DUAYDERMVQWIJD-UHFFFAOYSA-N 2-n,2-n,6-trimethyl-1,3,5-triazine-2,4-diamine Chemical compound CN(C)C1=NC(C)=NC(N)=N1 DUAYDERMVQWIJD-UHFFFAOYSA-N 0.000 claims description 2
- KYZHGEFMXZOSJN-UHFFFAOYSA-N benzoic acid isobutyl ester Natural products CC(C)COC(=O)C1=CC=CC=C1 KYZHGEFMXZOSJN-UHFFFAOYSA-N 0.000 claims description 2
- VNGOYPQMJFJDLV-UHFFFAOYSA-N dimethyl benzene-1,3-dicarboxylate Chemical compound COC(=O)C1=CC=CC(C(=O)OC)=C1 VNGOYPQMJFJDLV-UHFFFAOYSA-N 0.000 claims description 2
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical compound O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 claims description 2
- GOKQOZYJEDDDOC-UHFFFAOYSA-N C(=O)OC.C1=CC=CC=C1 Chemical compound C(=O)OC.C1=CC=CC=C1 GOKQOZYJEDDDOC-UHFFFAOYSA-N 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 21
- 229920002678 cellulose Polymers 0.000 abstract description 7
- 239000001913 cellulose Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 6
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 2
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 abstract description 2
- 230000007794 irritation Effects 0.000 abstract description 2
- 231100000086 high toxicity Toxicity 0.000 abstract 1
- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 description 12
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 6
- 238000004064 recycling Methods 0.000 description 6
- 238000002166 wet spinning Methods 0.000 description 5
- 238000004821 distillation Methods 0.000 description 4
- QPJVMBTYPHYUOC-UHFFFAOYSA-N methyl benzoate Chemical compound COC(=O)C1=CC=CC=C1 QPJVMBTYPHYUOC-UHFFFAOYSA-N 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- 239000005711 Benzoic acid Substances 0.000 description 3
- 235000010233 benzoic acid Nutrition 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010297 mechanical methods and process Methods 0.000 description 2
- 229940095102 methyl benzoate Drugs 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 150000007942 carboxylates Chemical group 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 229940079877 pyrogallol Drugs 0.000 description 1
- 239000012492 regenerant Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000012163 sequencing technique Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 239000010784 textile waste Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- 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
- C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
- C08J11/08—Recovery or working-up of waste materials of polymers without chemical reactions using selective solvents for polymer components
-
- 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
- C08J11/02—Recovery or working-up of waste materials of solvents, plasticisers or unreacted monomers
-
- 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
-
- 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
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture 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
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
-
- 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
-
- 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)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention provides a method for recovering waste polyester-cotton blended fabrics, which comprises the steps of heating the waste polyester-cotton blended fabrics in an ester solvent with a submerged structure (1) to perform a polyester dissolving reaction, and then performing solid-liquid separation on the obtained mixture to obtain a polyester solution and insoluble substances containing cotton fibers; and then respectively recovering the terylene solution and the insoluble substance containing the cotton fiber to obtain terylene solid and cellulose regenerated fiber. The recovery method of the invention can completely and thoroughly separate the terylene and the cotton fibersThe method avoids the use of chemical reagents with high toxicity and high irritation, and the used reagents can be recycled. The recovery method provided by the invention has the advantages of high efficiency, low cost, environmental friendliness, wide application range and the like, and has the potential of industrial application.
Description
Technical field
The invention belongs to resource regeneration fields of weaving, and in particular to a kind of recovery method of waste and old polyester cotton.
Background technique
The textile waste weight that generates every year of China reaches 2,6,000,000 tons (Chinese Resources utilize association, 2013), only fragrant
In 2012, there are about 106,945 tons of textiles to be sent to landfill (Hong Kong Environmental Protection Administration, 2013) at port.According to PCI Wood
Mackenzie reports that in consumption textile material in 2015, terylene occupies 55%, ranks first place, followed by cotton, occupies
27%.The 82% of consumption textile material is accounted for altogether with cotton that is, washing.Estimate the year two thousand twenty, need of the whole world to both fibers
The amount of asking will be 90,000,000 tons (Global Fiber Overview, 2014).On the other hand, annual to use from energy consumption
In production fibre natural resources about 13, trillion liters of water of 2,000,000 tons of coals and 6-9 (weaving the world, 2008 11/
12 monthly magazines).Specific on terylene, according to middle petrochemical industry, the terephthalic acid (TPA) that one ton of terylene needs 0.85-0.86 tons is produced
(PTA) and 0.33-0.34 tons of ethylene glycol (EG), and the CO2 emission for producing a PTA is 4.2 tons.For cotton,
Cultivate 1 ton of raw cotton, need 8,000-18,000 square kilometre farmland, 8.3-13.8 kilograms of pesticide, 5700 cubic metres of water and
The energy (Waste:A handbook for management.2011) of 36-55GJ.From above data, it is not difficult to find out that, recycling is useless
Old polyester-cotton blend textile fabric, especially clothing have very big market potential, economic benefit and environment protection significance.
The recovery method of polyester cotton mainly has Mechanical Method and chemical method.What Mechanical Method obtained is mixed staple fiber
Aggregate, and since terylene is bigger than the intensity of cotton fiber, so it is serious by mechanical cotton fiber damage after the recovery, it also tends to
With other kinds of fiber, it can only finally be used as packing material or engineering reinforcing material.Chemical method is ideal method,
It can be by different chemical treatment technologies by terylene, cotton fiber and other fiber separations, convenient for the recycling of high added value.
In existing research, the solvent that chemical method uses is mostly the higher type of toxicity, at high cost and endanger environment, in addition, existing
Method is difficult to realize being completely separated for regenerant mostly, influences to recycle purity, thus seriously constrains returning for polyester cotton
It receives and recycles.
Summary of the invention
To overcome defect present in existing waste and old polyester cotton recovery technology, the object of the present invention is to provide one kind
The recovery method of efficient waste and old polyester cotton.
The recovery method of waste and old polyester cotton provided by the invention the following steps are included:
S1: waste and old polyester cotton is immersed in esters solvent, carries out terylene in 150~210 DEG C of at a temperature of heating
Dissolution reaction, then resulting mixture is separated by solid-liquid separation, obtains terylene solution and the insoluble matter containing cotton fiber；
S2: the fatty alcohol of C1~C3 is added into the terylene solution that step S1 is obtained to be precipitated terylene solid, described in filtering
Terylene solid repeats the operation until resulting terylene solid recycles after being free of the esters solvent；And
S3: the insoluble matter containing cotton fiber that step S1 is obtained carries out Fibrinolysis, and recycle obtain it is cellulose regenerated
Fiber；
Wherein, esters solvent used in the step S1 has formula (1) structure:
In formula (1), R indicates the linear or branched alkyl group of C1~C5, and n indicates 1~3 integer.
In recovery method of the invention, the waste and old polyester cotton is 10%~90% containing the amount of washing by weight.
In recovery method of the invention, esters solvent used in the step S1 is selected from methyl benzoate, benzoic acid second
Ester, propyl benzoate, isopropyl benzoate, butyl benzoate, isobutyl benzoate, dimethyl terephthalate (DMT), isophthalic diformazan
One of dimethyl phthalate or a variety of combinations.
In recovery method of the invention, in the waste and old polyester cotton, the weight of terylene and the esters solvent
Weight ratio is 1 ﹕, 10~1 ﹕ 90.
In recovery method of the invention, in the step S1, the reaction time of the dissolution reaction of terylene is 5~60 minutes.
In recovery method of the invention, in the step S2, the volume ratio of the terylene solution and fatty alcohol be 1 ﹕ 15~
1 ﹕ 50 after the fatty alcohol is added, is cooled to 45~65 DEG C so that terylene solid is precipitated.
In recovery method of the invention, the fatty alcohol is selected from one of methanol, ethyl alcohol, propyl alcohol, isopropanol or a variety of
Combination.
In recovery method of the invention, the step S2 further includes being viscosified resulting terylene solid to reaching spinning
The requirement of slice.
In recovery method of the invention, the step S2 further includes filtering out to be separately recovered after the terylene solid and again
Utilize the fatty alcohol and the esters solvent.
In recovery method of the invention, the step S3 include: into the insoluble matter containing cotton fiber be added antioxidant,
The mixture of hydrogen peroxide and 4- methyhnorpholine-N-oxide carries out Fibrinolysis, and cellulose is made again using wet spinning
It is recycled after raw fiber.
In recovery method of the invention, the weight ratio of the insoluble matter containing cotton fiber and the mixture be 1 ﹕ 99~
14 ﹕ 86.
In recovery method of the invention, the antioxidant is selected from catechol, Pyrogallol acid, gallic acid third
Ester, 2,6-di-tert-butyl p-cresol, gallic acid, the first, second of gallic acid, third or one of isopropyl ester or a variety of groups
It closes, the weight of the antioxidant is the 0.5%~3% of the mixture weight.
In recovery method of the invention, the weight of the hydrogen peroxide is the 3%~8% of the mixture weight.
In recovery method of the invention, the Fibrinolysis process include: prior to 70~85 DEG C at be swollen 10~30min,
It is warming up to 90~100 DEG C of 60~90min of dissolution later.
The recovery method of waste and old polyester cotton of the invention has the advantage that
(1) recovery method of the invention can completely, thoroughly separate terylene and cotton fiber, recycling resulting terylene solid can
Further reach the requirement of spinning chips, and recycles resulting tModified Cellulose Fibers also and can be directly used for spinning manufacture, it is economical
It is with the obvious advantage.
(2) recovery method of the invention avoids chemical reagent big using toxicity, that irritation is big, and used examination
Agent is also recyclable, further reduces process costs, and alleviates the harm to environment.
In short, recovery method provided by the invention has many advantages, such as that high efficiency, low cost, environmental-friendly, applicability is wide, tool
There are the potentiality of industrial applications.
Detailed description of the invention
Fig. 1 is the process flow chart of waste and old polyester cotton recovery method of the present invention.
Specific embodiment
The present invention provides a kind of recovery methods of waste and old polyester cotton, comprising the following steps:
S1: waste and old polyester cotton is immersed in esters solvent, carries out terylene in 150~210 DEG C of at a temperature of heating
Dissolution reaction, then resulting mixture is separated by solid-liquid separation, obtains terylene solution and the insoluble matter containing cotton fiber；
S2: the fatty alcohol of C1~C3 is added into the terylene solution that step S1 is obtained terylene solid is precipitated, filters terylene
Solid repeats the operation until resulting terylene solid recycles after being free of esters solvent；And
S3: the insoluble matter containing cotton fiber that step S1 is obtained carries out Fibrinolysis, and recycle obtain it is cellulose regenerated
Fiber；
Wherein, esters solvent used in step S1 has formula (1) structure:
In formula (1), R indicates the linear or branched alkyl group of C1~C5, and n indicates 1~3 integer.
Referring to Fig.1, the recovery method of waste and old polyester cotton of the invention uses chemical method, uses esters solvent first
Terylene is dissolved, reaches the mesh for being completely separated polyester fiber (being dissolved in solution) and cotton fiber (insoluble matter) by being separated by solid-liquid separation
, specific aim recovery processing then is carried out to resulting terylene solution and cotton fiber insoluble matter again.Recovery method of the invention makes
Esters solvent is the solvent of benzoic acid derived ester, and small toxicity is at low cost, and is convenient to recycling and reusing.
Further, terylene solution is handled using the lower aliphatic alcohols of C1~C3, so that terylene solid is precipitated, by its mistake
Filter is repeated several times until resulting terylene solid is free of esters solvent to may be recovered.Insoluble matter containing cotton fiber can
By the processing of Fibrinolysis to obtain tModified Cellulose Fibers.In practical applications, step S2, S3 can be according to the actual situation
It is handled by different sequencings, sequence is unlimited, can also be handled simultaneously.
In recovery method of the invention, waste and old polyester cotton can be the waste and old polyester-cotton blend of arbitrary proportion terylene content
Blended fabric.In one embodiment according to the present invention, waste and old polyester cotton can be by weight containing the amount of washing
10%~90%, in one preferred embodiment, waste and old polyester cotton can be 30%~70% containing the amount of washing.It removes
Outside terylene, the other compositions of waste and old polyester cotton are cotton fiber, also may include other except a small amount of terylene, cotton fiber
Fibre types, these other kinds of fibers are finally separated from system in the form of insoluble matter in removal process.
In recovery method of the invention, the esters solvent that step S1 is used has above-mentioned formula (1) structure, wherein R can table
Show methyl, ethyl, propyl, isopropyl, normal-butyl, isobutyl group, sec-butyl, tert-butyl, n-pentyl, isopentyl, neopentyl, uncle penta
Base etc. preferably can be methyl, ethyl, propyl, isopropyl, normal-butyl.N can indicate 1,2 or 3 integer, preferably 1 or 2
Integer has one or two carboxylate groups that is, on phenyl ring, when n indicates not to be 1 integer, two or more substitutions
Group can be located at any possible the position of substitution on phenyl ring.In one embodiment according to the present invention, esters solvent packet
Include but be not limited to methyl benzoate, ethyl benzoate, propyl benzoate, isopropyl benzoate, butyl benzoate, anhydride
Ester, dimethyl terephthalate (DMT), dimethyl isophthalate etc. can also be the combination of any kind.
In recovery method of the invention, calculated according to the weight of terylene in waste and old polyester cotton, it is molten with esters
The dosage of agent can be the weight ratio of 1 ﹕, 10~1 ﹕ 90, can also be adjusted according to the actual situation by those skilled in the art.?
In a preferred embodiment according to the present invention, the weight ratio of terylene and esters solvent can be 1 ﹕, 20~1 ﹕ 50.
In recovery method of the invention, the dissolution reaction of the terylene in step S1 should generally make terylene dissolution completely, can
By those skilled in the art adjusting reaction time and temperature according to the actual situation.In one embodiment according to the present invention,
Reaction time can be 5~60 minutes, and in one preferred embodiment, the reaction time can be 10~30 minutes.In root
According in an embodiment of the invention, reaction temperature can be 160~190 DEG C.
In recovery method of the invention, C1~C3 fatty alcohol in step S2 can be methanol, ethyl alcohol, propyl alcohol, isopropyl
The common lower aliphatic alcohols such as alcohol, can be heated to boiling before addition.In one embodiment according to the present invention, fatty alcohol can
Think methanol or ethyl alcohol.In one embodiment according to the present invention, the lower aliphatic alcohols such as terylene solution and methanol, ethyl alcohol
Volume ratio can be 1 ﹕, 15~1 ﹕ 50, and in one preferred embodiment, the volume ratio of terylene solution and lower aliphatic alcohols can
Think 1 ﹕, 20~1 ﹕ 40.It is added after the lower aliphatic alcohols such as methanol, ethyl alcohol, terylene solution can be cooled to 45~65 DEG C to be precipitated
Terylene solution can be cooled to 55~65 DEG C in one preferred embodiment terylene solid is precipitated by terylene solid.
In recovery method of the invention, step S2's plus alcohol, be precipitated solid, the techniques such as filtering can according to the actual situation into
Row repeats, including but not limited to more than once.By reprocessing, until pure terylene solid is obtained, wherein not containing ester
Class solvent.In one embodiment according to the present invention, to reach higher recycling requirement, also for obtained terylene solid
It can be handled by granulation, pre-crystallized, dry, solid-phase tack producing etc., to improve the number-average molecular weight of terylene up to 20000 or more, thus
Reach the requirement of spinning chips.
In recovery method of the invention, as shown in Figure 1, collecting the lower aliphatic alcohols after processing terylene solid, may be used also
It is recycled or is purified to recycle respectively for esters solvent and fatty alcohol itself contained therein.Since the present invention makes
Esters solvent boiling point is much higher than lower aliphatic alcohols, therefore can pass through this fields normal methods such as cooling crystallization, distillation, rectifying
Recycle esters solvent and fatty alcohol.In one embodiment according to the present invention, after isolating terylene solid, then will be remaining
Fatty alcohol solution continues to be cooled to 20~40 DEG C so that esters solvent crystal is precipitated, and in one preferred embodiment, is cooled to
20~25 DEG C to be precipitated esters solvent crystal, after recycling esters solvent crystal, remaining fatty alcohol is purified by modes such as distillations
After can be recycled.In an alternative embodiment of the process according to the invention, distillation can also be used or ester is separately recovered in rectifying mode
Class solvent and fatty alcohol.
In recovery method of the invention, the insoluble matter containing cotton fiber can pass through existing method or reagent reclaiming
Fiber, since cotton fiber insoluble matter and polyester fiber have obtained comprehensively, thoroughly separating, even if can also using existing method
To achieve the purpose that recycle high-purity cotton fiber.In one embodiment according to the present invention, step S3 can further comprise
Following treatment process: antioxidant, hydrogen peroxide and 4- methyhnorpholine-N-oxide are added in the insoluble matter of Xiang Hanyou cotton fiber
Mixture carry out Fibrinolysis, recycled after tModified Cellulose Fibers are made using wet spinning.
In one embodiment according to the present invention, antioxidant includes but is not limited to catechol, 1,2,3- benzene three
Phenol, propylgallate, 2,6-di-tert-butyl p-cresol, gallic acid, the first, second of gallic acid, third or isopropyl ester etc., can also
For the combination of any kind, in one preferred embodiment, the weight of antioxidant can be the 0.5% of mixture weight
~3%, in a preferred embodiment, the weight of antioxidant can be the 1%~2% of mixture weight.
In one embodiment according to the present invention, the hydrogen peroxide concentration in mixture can be 3%~8%, one
In a preferred embodiment, hydrogen peroxide concentration can be 5%~7%.Hydrogen peroxide can play certain bleaching, decolorization.
In one embodiment according to the present invention, the insoluble matter containing cotton fiber and 4- methyhnorpholine-N-oxide
The weight ratio of equal mixtures can be 1 ﹕, 99~14 ﹕ 86, in one preferred embodiment, the insoluble matter containing cotton fiber with
The weight ratio of mixture can be 9 ﹕, 91~12 ﹕ 88.In one embodiment according to the present invention, Fibrinolysis can add
It is carried out under heat condition, such as following procedure: being swollen 10~30min at prior to 70~85 DEG C, be warming up to 90~100 DEG C of dissolutions later
60~90min, in one preferred embodiment, Fibrinolysis can also be following procedure: be swollen at prior to 75~85 DEG C
20~25min is warming up to 90~95 DEG C of 60~75min of dissolution later.After Fibrinolysis, by other insoluble fibres in acquired solution
The solid impurities such as dimension filter out, and the methods of common recovery method such as wet spinning recycled fiber can be selected in remaining fiber solution
Plain regenerated fiber.
In recovery method of the invention, it is common that this field can be selected in the operation of the separating steps such as separation of solid and liquid, filtering
Operation, including but not limited to suction method, (high speed) centrifugal process, the precipitation method or their combination.
To make the object, technical solutions and advantages of the present invention clearer, it will be further described below example of the invention
The technical solution of property embodiment.
Chemical reagent used in following embodiment is then commercial goods and is that analysis is pure unless otherwise instructed, is implemented below
Operation or instrument used in example are then this field common operation or instrument unless otherwise instructed.Described in following embodiment
Ratio, ratio, content etc. are then weight ratio unless otherwise instructed.
Embodiment 1
The waste and old blue denim fabric 2g for being 50/50 by polyester cotton blending rate, immerses and 25g terephthalic acid (TPA) diformazan is housed
In the flask of ester, 25min is heated at a temperature of 170 DEG C.After terylene is completely dissolved, the insoluble matters such as cotton fiber are filtered to take
Out, and by resulting terylene solution it puts into the 1L methanol of heat, temperature is down to 50 DEG C, collects the terylene solid being precipitated by suction method
Body later puts into the terylene solid in fresh methanol again, repeats the above process the terylene solid several times, made not
Solvent containing dimethyl terephthalate (DMT) again, and so that its molecular weight is reached the requirements of spinning-grade terylene chips using thickening machine.
Continue above-mentioned collected methanol solution to cool to 25 DEG C, the terephthaldehyde being precipitated is collected using supercentrifuge
Dimethyl phthalate solid, and remaining methanol solution is reusable after distilation.
The insoluble matters such as the cotton fiber of taking-up are then added in the 4- methyhnorpholine-N-oxide mixture of 230ml, wherein also
Containing 2% propylgallate and 6% hydrogen peroxide, and it first is swollen 20min at 80 DEG C, then is warming up to 95 DEG C of dissolutions
60min makes cellulose filter out the impurity such as other insoluble fibers after completely dissolution, and be made through wet spinning connect it is subdiaphanous
TModified Cellulose Fibers.
Obtained terylene solid and tModified Cellulose Fibers are subjected to cleaning and the drying in 80 DEG C of convection oven respectively
It weighs after 6h, the rate of recovery of terylene solid is 90%, and the rate of recovery of tModified Cellulose Fibers is 94%.
Embodiment 2
The waste and old blended fabric 2g for being 65/35 by polyester cotton blending rate immerses in the flask equipped with 60g propyl benzoate,
15min is heated at a temperature of 180 DEG C.After terylene is completely dissolved, the insoluble matters such as cotton fiber are taken out, and by resulting terylene
Solution is put into the 1.2L ethyl alcohol of heat, and temperature is down to 55 DEG C, the terylene solid being precipitated is collected by suction method, later by the terylene
Solid is put into again in fresh ethyl alcohol, is repeated the above process several times, until obtained terylene solid no longer contains benzoic acid third
Ester solvent, and so that its molecular weight is reached the requirements of spinning-grade terylene chips using thickening machine.
Above-mentioned collected ethanol solution is subjected to distilation, obtained distillation is ethyl alcohol, and residue is benzoic acid
Propyl ester.
The insoluble matters such as the cotton fiber of taking-up are then added in the mixture of 4- methyhnorpholine-N-oxide of 220ml, wherein
Containing 1% Propylgallate and 7% hydrogen peroxide, and it first is swollen 15min at 75 DEG C, then is warming up to 90 DEG C of dissolution 70min, made
Cellulose filters out insoluble other types fiber after completely dissolution, and be made through wet spinning connect it is subdiaphanous cellulose regenerated
Fiber.
Obtained terylene solid and tModified Cellulose Fibers are subjected to cleaning and the drying in 80 DEG C of convection oven respectively
It weighs after 6h, the rate of recovery of obtained terylene solid is 92%, and the rate of recovery of tModified Cellulose Fibers is 93%.
Although the preferred embodiments of the invention, those skilled in the art has been disclosed in order to illustrate the present invention
Member can be the present invention it should be appreciated that in the case where not departing from present inventive concept defined by claims and range
Various modifications, addition and replacement out.
Claims (14)
1. a kind of recovery method of waste and old polyester cotton, which comprises the following steps:
S1: waste and old polyester cotton is immersed in esters solvent, carries out the molten of terylene in 150~210 DEG C of at a temperature of heating
Resulting mixture, is then separated by solid-liquid separation, obtains terylene solution and the insoluble matter containing cotton fiber by solution reaction；
S2: the fatty alcohol of C1~C3 is added into the terylene solution that step S1 is obtained terylene solid is precipitated, filters the terylene
Solid repeats the operation until resulting terylene solid recycles after being free of the esters solvent；And
S3: the insoluble matter containing cotton fiber that step S1 is obtained carries out Fibrinolysis, and recycles and obtain tModified Cellulose Fibers；
Wherein, esters solvent used in the step S1 has formula (1) structure:
In formula (1), R indicates the linear or branched alkyl group of C1~C5, and n indicates 1~3 integer.
2. recovery method according to claim 1, which is characterized in that the waste and old polyester cotton contains the amount of washing by weight
Amount is than being 10%~90%.
3. recovery method according to claim 1, which is characterized in that esters solvent used in the step S1 is selected from benzene
Methyl formate, ethyl benzoate, propyl benzoate, isopropyl benzoate, butyl benzoate, isobutyl benzoate, terephthaldehyde
One of dimethyl phthalate, dimethyl isophthalate or a variety of combinations.
4. recovery method according to claim 3, which is characterized in that in the waste and old polyester cotton, the weight of terylene
Amount and the weight ratio of the esters solvent are 1 ﹕, 10~1 ﹕ 90.
5. recovery method according to claim 1, which is characterized in that in the step S1, the dissolution of terylene reacts anti-
It is 5~60 minutes between seasonable.
6. recovery method according to claim 1, which is characterized in that in the step S2, the terylene solution and fat
The volume ratio of alcohol is 1 ﹕, 15~1 ﹕ 50, after the fatty alcohol is added, is cooled to 45~65 DEG C so that terylene solid is precipitated.
7. recovery method according to claim 6, which is characterized in that the fatty alcohol is selected from methanol, ethyl alcohol, propyl alcohol, different
One of propyl alcohol or a variety of combinations.
8. recovery method according to claim 1, which is characterized in that the step S2 further includes by resulting terylene solid
It is viscosified to the requirement for reaching spinning chips.
9. recovery method according to claim 1, which is characterized in that the step S2 further includes filtering out the terylene solid
It is separately recovered after body and recycles the fatty alcohol and the esters solvent.
10. recovery method according to claim 1, which is characterized in that the step S3 include: to containing cotton fiber not
The mixture that antioxidant, hydrogen peroxide and 4- methyhnorpholine-N-oxide are added in molten object carries out Fibrinolysis, using wet
Method spinning is recycled after tModified Cellulose Fibers are made.
11. recovery method according to claim 10, which is characterized in that the insoluble matter containing cotton fiber is mixed with described
The weight ratio for closing object is 1 ﹕, 99~14 ﹕ 86.
12. recovery method according to claim 10, which is characterized in that the antioxidant be selected from catechol, 1,2,
3- benzenetriol, propylgallate, 2,6-di-tert-butyl p-cresol, gallic acid, the first, second of gallic acid, third or isopropyl ester
One of or a variety of combinations, the weight of the antioxidant be the 0.5%~3% of the mixture weight.
13. recovery method according to claim 10, which is characterized in that the weight of the hydrogen peroxide is the mixture weight
The 3%~8% of amount.
14. recovery method according to claim 10, which is characterized in that the Fibrinolysis process include: prior to 70~
It is swollen 10~30min at 85 DEG C, is warming up to 90~100 DEG C of 60~90min of dissolution later.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020252683A1 (en) * | 2019-06-19 | 2020-12-24 | The Hong Kong Research Institute Of Textiles And Apparel Limited | Method and system for recovering fibers from fibrous products |
| WO2021165531A3 (en) * | 2020-02-21 | 2021-10-14 | DTNW Deutsches Textilforschungszentrum Nord-West gemeinnützige GmbH | Method for recycling mixed fabrics |
| CN113717433A (en) * | 2021-09-13 | 2021-11-30 | 福建赛隆科技有限公司 | Process for recovering chinlon from waste chinlon blended fabric and recovered product |
| WO2023076210A3 (en) * | 2021-10-25 | 2023-06-08 | Eastman Chemical Company | Processes for recovering polyesters from feedstocks |
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| CN102061005A (en) * | 2010-11-19 | 2011-05-18 | 绍兴中纺院江南分院有限公司 | Polyester fiber or polyester fabric waste recycling method |
| CN102199310A (en) * | 2011-05-17 | 2011-09-28 | 东华大学 | Method for recycling cotton-containing components in waste cotton-polyester blended fabrics |
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| CN1252823A (en) * | 1997-04-18 | 2000-05-10 | 纳幕尔杜邦公司 | Method for recovering polyester from contaminated polyester waste |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2020252683A1 (en) * | 2019-06-19 | 2020-12-24 | The Hong Kong Research Institute Of Textiles And Apparel Limited | Method and system for recovering fibers from fibrous products |
| WO2021165531A3 (en) * | 2020-02-21 | 2021-10-14 | DTNW Deutsches Textilforschungszentrum Nord-West gemeinnützige GmbH | Method for recycling mixed fabrics |
| CN113717433A (en) * | 2021-09-13 | 2021-11-30 | 福建赛隆科技有限公司 | Process for recovering chinlon from waste chinlon blended fabric and recovered product |
| CN113717433B (en) * | 2021-09-13 | 2023-08-11 | 福建赛隆科技有限公司 | Process for recovering chinlon from waste chinlon blended fabric and recovered product |
| WO2023076210A3 (en) * | 2021-10-25 | 2023-06-08 | Eastman Chemical Company | Processes for recovering polyesters from feedstocks |
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