CN107459629A - A kind of waste PET material decolourizes to reclaim the method for preparing high-purity PET sections - Google Patents
A kind of waste PET material decolourizes to reclaim the method for preparing high-purity PET sections Download PDFInfo
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- CN107459629A CN107459629A CN201610388201.2A CN201610388201A CN107459629A CN 107459629 A CN107459629 A CN 107459629A CN 201610388201 A CN201610388201 A CN 201610388201A CN 107459629 A CN107459629 A CN 107459629A
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- 239000002699 waste material Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 title claims abstract description 10
- QPKOBORKPHRBPS-UHFFFAOYSA-N bis(2-hydroxyethyl) terephthalate Chemical compound OCCOC(=O)C1=CC=C(C(=O)OCCO)C=C1 QPKOBORKPHRBPS-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000002425 crystallisation Methods 0.000 claims abstract description 15
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 10
- 238000011084 recovery Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000004821 distillation Methods 0.000 claims abstract description 6
- 230000008025 crystallization Effects 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 42
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 3
- 229910052787 antimony Inorganic materials 0.000 claims description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229920003023 plastic Polymers 0.000 abstract description 5
- 239000004033 plastic Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000008367 deionised water Substances 0.000 abstract 1
- 229910021641 deionized water Inorganic materials 0.000 abstract 1
- 239000000835 fiber Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 4
- 238000000053 physical method Methods 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000000126 substance Substances 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
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/18—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material
- C08J11/22—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic oxygen-containing compounds
- C08J11/24—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic oxygen-containing compounds containing hydroxyl groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/09—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis
- C07C29/095—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of esters of organic acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/03—Preparation of carboxylic acid esters by reacting an ester group with a hydroxy group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
- C08G63/86—Germanium, antimony, 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
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Decolourize to reclaim the method for preparing high-purity PET sections the invention discloses a kind of waste PET material.By the waste PET material after kneader is handled, it is dissolved in propylene glycol solution, by filtering, crystallisation by cooling, again by squeezing, dissolving, crystallization twice, obtain BHET essence cakes, the BHET powder of high-purity is obtained using deionized water dissolving, crystallization, distillation afterwards, high-purity PET, which is prepared, through polycondensation reaction cuts into slices.The present invention solve traditional handicraft can only to cleaning up, the bottleneck that dried bottle piece, the clean waste silk of fiber factory are reclaimed, greatly reduce the complexity of equipment requirement, reduce solvent acquisition amount, reduce energy consumption, recovery yield rate and product purity are improved, reduces cost, non-secondary pollution, the height recycling of waste or used plastics is realized, and industrialization production can be carried out.
Description
Technical field
The present invention relates to useless PET recovery and utilization technologies, more particularly to a kind of waste PET material decolourizes back
Receive the method for preparing high-purity PET sections.
Background technology
At present, China's method main to waste PET closed matereial cycle is the method and thing of chemical degradation
Reason method.Chemical method is to allow PET material that degradation reaction, shape occurs in the presence of thermally and chemically reagent
Into low molecule product, product can be utilized further, and as monomer can polymerize again, oil product can carry out deep processing,
But this method needs HTHP, require appointed condition high, power consumption is high, condition is harsh, it is difficult to real
Existing large-scale operation；Physical method is by cutting off, crushing, heating and the process such as dissolve to waste PET
The recycle utilization reprocessed, but the performance of regenerative PET is greatly lowered than virgin material, and containing big
Impurity is measured, application value reduces a lot.To printing PET film due to that can go out in the processing of physical method
Now easily foaming, takes out a broken strip, color blackening and situation about giving an offensive smell and lead to not processing recovery,
Still belong to technical clear area.
The content of the invention
The present invention is to make up the deficiencies in the prior art, there is provided a kind of waste PET material decolouring recovery prepares high
The method of pure PET sections.Concrete technical scheme step of the present invention is as follows：
(1) PET low molecule solution is prepared
By the useless film of the waste and old polyethylene terephtalate of collection and BHET powder in mass ratio
Added for 3: 2-8: 1 ratio in kneader, temperature control is blended, blend, disperse at 180-240 DEG C
30-900min, it can obtain PET low molecule solution；
(2) PET primary solutions are prepared
By propane diols and gained PET low molecules solution in mass ratio for 1-4: 1 ratio put into it is closed
In container, under conditions of 180-240 DEG C, 0.1-0.5Mpa, after stirring and being incubated 1-5 hours, obtain
To PET primary solutions；
(3) filtering, crystallisation by cooling
Gained PET primary solutions are added into aperture as in the filter of 10-200 mesh, at 100-140 DEG C and
Under normal pressure, filtering, remove impurity, obtain initial soln；After crystallisation by cooling at 20-50 DEG C, analysis
Go out to obtain bishydroxyethyl terephthalate BHET just cake and propane diols；
(4) squeeze, dissolve, crystallization
Cake at the beginning of BHET is placed in squeezer after strong force squeezing, obtains the clear cakes of BHET；Backward gained
The 50-250% of its volume propane diols is added in the clear cakes of BHET, 90-130 DEG C is heated to, obtains BHET
Clear cake solution；Afterwards by the clear cake solution of BHET crystallisation by cooling at 20-100 DEG C, separate out, obtain BHET
Thick cake and propylene glycol solution；
(5) squeeze, dissolve, crystallize, rectifying again
The thick cakes of BHET are placed in squeezer after strong force squeezing, obtain bis- clear cakes of BHET, Ran Houyong
Evaporator distillation obtains BHET essence cakes to remove the whole propane diols remained in the clear cake；Afterwards by institute
BHET essence cakes dissolve in 70-90 DEG C of hot water, isolate insoluble matter, then crystallized, dehydration,
Dry, obtain purity 97-99% BHET powder；Obtained BHET powder is continued with into rectifying
Device carries out rectifying and obtains high-purity BHET powder that purity is more than 99.5%；
(6) polycondensation reaction, PET sections are prepared
By high-purity BHET powder obtained by step (5) and ethylene glycol according to the ratio that mass ratio is 5-13: 1
Example is added in polycondensation vessel, while adds antimony-based catalyst, is carried out polycondensation reaction under vacuo, is finally given
The PET that inherent viscosity is 0.63-0.70dl/g cuts into slices.
The advantage of the invention is that：Realize and substitute the technology of traditional distillation mode to dash forward in a manner of squeezing
It is broken, the complexity of equipment requirement is greatly reduced, simplifies flow, reduces solvent acquisition amount, is reduced
Energy consumption, recovery yield rate and product purity are improved, while the cost recovery of waste plastics is saved not
Secondary pollution can be caused to environment, realize the height recycling of waste or used plastics and industrialization can be carried out
Production.
Embodiment
The embodiment of the present invention is further described with reference to embodiment, following examples are only
For clearly illustrating technical scheme, and the protection model of the present invention can not be limited with this
Enclose.
A kind of waste PET material provided by the invention decolourizes to reclaim the method bag for preparing high-purity PET sections
Include following steps：
Embodiment 1
(1) PET low molecule solution is prepared
By the useless film of the waste and old polyethylene terephtalate of collection and BHET powder in mass ratio
Added for 3: 2-8: 1 ratio in kneader, temperature control is blended, blend, disperse at 180-240 DEG C
30-900min, it can obtain PET low molecule solution；
(2) PET primary solutions are prepared
By propane diols and gained PET low molecules solution in mass ratio for 1-4: 1 ratio put into it is closed
In container, under conditions of 180-240 DEG C, 0.1-0.5Mpa, after stirring and being incubated 1-5 hours, obtain
To PET primary solutions；
(3) filtering, crystallisation by cooling
Gained PET primary solutions are added into aperture as in the filter of 10-200 mesh, at 100-140 DEG C and
Under normal pressure, filtering, remove impurity, obtain initial soln；After crystallisation by cooling at 20-50 DEG C, analysis
Go out to obtain bishydroxyethyl terephthalate BHET just cake and propane diols；
(4) squeeze, dissolve, crystallization
Cake at the beginning of BHET is placed in squeezer after strong force squeezing, obtains the clear cakes of BHET；Backward gained
The 50-250% of its volume propane diols is added in the clear cakes of BHET, 90-130 DEG C is heated to, obtains BHET
Clear cake solution；Afterwards by the clear cake solution of BHET crystallisation by cooling at 20-100 DEG C, separate out, obtain BHET
Thick cake and propylene glycol solution；
(5) squeeze, dissolve, crystallize, rectifying again
The thick cakes of BHET are placed in squeezer after strong force squeezing, obtain bis- clear cakes of BHET, Ran Houyong
Evaporator distillation obtains BHET essence cakes to remove the whole propane diols remained in the clear cake；Afterwards by institute
BHET essence cakes dissolve in 70-90 DEG C of hot water, isolate insoluble matter, then crystallized, dehydration,
Dry, obtain purity 97-99% BHET powder；Obtained BHET powder is continued with into rectifying
Device carries out rectifying and obtains high-purity BHET powder that purity is more than 99.5%；
(6) polycondensation reaction, PET sections are prepared
By high-purity BHET powder obtained by step (5) and ethylene glycol according to the ratio that mass ratio is 5-13: 1
Example is added in polycondensation vessel, while adds antimony-based catalyst, is carried out polycondensation reaction under vacuo, is finally given
The PET that inherent viscosity is 0.63-0.70dl/g cuts into slices.
The advantage of the invention is that：Realize and substitute the technology of traditional distillation mode to dash forward in a manner of squeezing
It is broken, the complexity of equipment requirement is greatly reduced, simplifies flow, reduces solvent acquisition amount, is reduced
Energy consumption, recovery yield rate and product purity are improved, while the cost recovery of waste plastics is saved not
Secondary pollution can be caused to environment, realize the height recycling of waste or used plastics and industrialization can be carried out
Production.
One embodiment of the present of invention is described in detail above, but the content is only the present invention's
Preferred embodiment, it is impossible to be considered as the practical range for limiting the present invention.It is all according to the present patent application scope
The equivalent change made and improvement etc., all should still be belonged within the patent covering scope of the present invention.
Claims (1)
- A kind of method that recovery prepares high-purity PET sections 1. waste PET material decolourizes, it is characterised in that Concrete technical scheme step of the present invention is as follows：(1) PET low molecule solution is preparedBy the useless film of the waste and old polyethylene terephtalate of collection and BHET powder in mass ratio Added for 3: 2-8: 1 ratio in kneader, temperature control is blended, blend, disperse at 180-240 DEG C 30-900min, it can obtain PET low molecule solution；(2) PET primary solutions are preparedBy propane diols and gained PET low molecules solution in mass ratio for 1-4: 1 ratio put into it is closed In container, under conditions of 180-240 DEG C, 0.1-0.5Mpa, after stirring and being incubated 1-5 hours, obtain To PET primary solutions；(3) filtering, crystallisation by coolingGained PET primary solutions are added into aperture as in the filter of 10-200 mesh, at 100-140 DEG C and Under normal pressure, filtering, remove impurity, obtain initial soln；After crystallisation by cooling at 20-50 DEG C, analysis Go out to obtain bishydroxyethyl terephthalate BHET just cake and propane diols；(4) squeeze, dissolve, crystallizationCake at the beginning of BHET is placed in squeezer after strong force squeezing, obtains the clear cakes of BHET；Backward gained The 50-250% of its volume propane diols is added in the clear cakes of BHET, 90-130 DEG C is heated to, obtains BHET Clear cake solution；Afterwards by the clear cake solution of BHET crystallisation by cooling at 20-100 DEG C, separate out, obtain BHET Thick cake and propylene glycol solution；(5) squeeze, dissolve, crystallize, rectifying againThe thick cakes of BHET are placed in squeezer after strong force squeezing, obtain bis- clear cakes of BHET, Ran Houyong Evaporator distillation obtains BHET essence cakes to remove the whole propane diols remained in the clear cake；Afterwards by institute BHET essence cakes dissolve in 70-90 DEG C of hot water, isolate insoluble matter, then crystallized, dehydration, Dry, obtain purity 97-99% BHET powder；Obtained BHET powder is continued with into rectifying Device carries out rectifying and obtains high-purity BHET powder that purity is more than 99.5%；(6) polycondensation reaction, PET sections are preparedBy high-purity BHET powder obtained by step (5) and ethylene glycol according to the ratio that mass ratio is 5-13: 1 Example is added in polycondensation vessel, while adds antimony-based catalyst, is carried out polycondensation reaction under vacuo, is finally given The PET that inherent viscosity is 0.63-0.70dl/g cuts into slices.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610388201.2A CN107459629A (en) | 2016-06-06 | 2016-06-06 | A kind of waste PET material decolourizes to reclaim the method for preparing high-purity PET sections |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610388201.2A CN107459629A (en) | 2016-06-06 | 2016-06-06 | A kind of waste PET material decolourizes to reclaim the method for preparing high-purity PET sections |
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| CN107459629A true CN107459629A (en) | 2017-12-12 |
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| CN201610388201.2A Pending CN107459629A (en) | 2016-06-06 | 2016-06-06 | A kind of waste PET material decolourizes to reclaim the method for preparing high-purity PET sections |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110128635A (en) * | 2019-06-10 | 2019-08-16 | 中塑联新材料科技湖北有限公司 | A kind of method that useless PET film electronation prepares PBT raw material |
| WO2021028695A1 (en) * | 2019-08-13 | 2021-02-18 | Poseidon Plastics Limited | Polymer recycling |
-
2016
- 2016-06-06 CN CN201610388201.2A patent/CN107459629A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110128635A (en) * | 2019-06-10 | 2019-08-16 | 中塑联新材料科技湖北有限公司 | A kind of method that useless PET film electronation prepares PBT raw material |
| WO2021028695A1 (en) * | 2019-08-13 | 2021-02-18 | Poseidon Plastics Limited | Polymer recycling |
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Application publication date: 20171212 |