CN114426663B - Titanium dioxide removal method for circulating EG in polyester production - Google Patents
Titanium dioxide removal method for circulating EG in polyester production Download PDFInfo
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- CN114426663B CN114426663B CN202011182529.1A CN202011182529A CN114426663B CN 114426663 B CN114426663 B CN 114426663B CN 202011182529 A CN202011182529 A CN 202011182529A CN 114426663 B CN114426663 B CN 114426663B
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- solution
- titanium dioxide
- circulating
- esterification
- glycol
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 36
- 229920000728 polyester Polymers 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 71
- 239000012528 membrane Substances 0.000 claims abstract description 47
- 238000005886 esterification reaction Methods 0.000 claims abstract description 37
- 230000032050 esterification Effects 0.000 claims abstract description 29
- 239000000919 ceramic Substances 0.000 claims abstract description 25
- 238000001914 filtration Methods 0.000 claims abstract description 22
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 230000008569 process Effects 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 239000002002 slurry Substances 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims description 14
- 230000004907 flux Effects 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 230000001172 regenerating effect Effects 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000012982 microporous membrane Substances 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 230000007704 transition Effects 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims 1
- 229910001928 zirconium oxide Inorganic materials 0.000 claims 1
- 238000004064 recycling Methods 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 3
- 230000000153 supplemental effect Effects 0.000 abstract description 3
- 238000000605 extraction Methods 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000012466 permeate Substances 0.000 description 9
- 239000012141 concentrate Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical group COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- -1 polyethylene terephthalate Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002216 antistatic agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000003381 stabilizer 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
- C08G63/88—Post-polymerisation treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention provides a method for removing titanium dioxide of circulating EG in polyester production, which comprises the following steps: firstly, enabling glycol mixed steam generated in the esterification process to pass through a process tower to form recovered EG solution; an external ceramic membrane is adopted on a glycol extraction pipeline of a process tower to treat and recycle EG solution, so as to obtain circulating EG solution to a clear liquid tank, and water insoluble matters such as titanium dioxide and the like are intercepted to become concentrated solution to a circulating tank; finally, the circulating EG solution is obtained after filtering, one part of the circulating EG solution is sent to a first esterification kettle for regulating esterification reaction, and the other part of the circulating EG solution is sent to a recycling glycol collecting tank for being mixed with external pure supplemental glycol to prepare slurry. The invention utilizes specific filtering separation equipment, and the filter mainly filters out titanium dioxide impurities to realize the recycling of EG; by adopting the removal process, the titanium dioxide removal rate is more than 99.5%.
Description
Technical Field
The invention relates to the technical field of recycling of polyester EG, in particular to a method for removing titanium dioxide of recycled EG in polyester production.
Background
Polyester (PET), particularly polyethylene terephthalate, is widely used in the field of various molded articles such as fibers, films, and resins. In the conventional process for producing polyethylene terephthalate, dimethyl terephthalate or terephthalic acid and ethylene glycol are reacted in the presence of a catalyst, and in order to satisfy the characteristics required for the application, only a characteristic imparting agent such as a stabilizer, a colorant, or an antistatic agent may be used.
The adding amount of titanium dioxide in the production process is larger than that in the production process of semi-dull PET, the solvent for preparing the titanium dioxide is fresh glycol, the titanium dioxide is added in a second esterification kettle, and excessive glycol is extracted from a process tower. Because the ethylene glycol is continuously recycled in a production system, various impurities are mixed in each section, especially titanium dioxide impurities are continuously increased, and the prepared slurry is unstable and affects the esterification reaction, so that the quality of polyester products is directly affected. The invention aims to ensure the pure and stable purpose of the recovered glycol for preparing slurry by adding a filtering system again so as to obtain an effective method for removing titanium dioxide in the circulating EG.
Disclosure of Invention
The technical problem solved by the invention is to provide a method for removing titanium dioxide of circulating EG in polyester production.
In view of this, the present invention provides a process for the removal of titania from recycled EG in the production of polyester, comprising the steps of:
1) Adding a titanium dioxide solution into a second esterification kettle for producing full-dull polyester PET, generating glycol mixed steam under the conditions that the esterification temperature is 258+/-2 ℃ and the liquid level of the esterification kettle is 70+/-2% and the esterification pressure is normal pressure in the esterification process, and spraying the glycol mixed steam at 25+/-1 ℃ to obtain a recovered EG solution; wherein the recovered EG solution comprises ethylene glycol, and titanium dioxide impurities;
2) Filtering the recovered EG solution in a ceramic membrane, allowing the recovered EG solution to flow in a membrane tube at a high speed as raw material liquid under the conditions of a filtering pressure of 0.2Mpa and a filtering temperature of 23+/-1 ℃, allowing clear permeate liquid containing small molecular components to permeate the membrane outwards along a direction perpendicular to the clear permeate liquid under the driving of pressure, and trapping turbid concentrate containing large molecular components by the membrane, so that the fluid achieves the purposes of separation, concentration and purification, the recycled EG solution is obtained to a clear liquid tank, and water insoluble matters such as titanium dioxide impurities are trapped to form concentrate to a circulating tank;
3) The 40% -50% circulating EG solution in the clear solution tank is returned to the first esterification kettle for esterification reaction; the remaining solution was sent to a recycle EG collection tank and mixed with external pure make-up ethylene glycol for slurry preparation.
Further, in the step (1), the solvent for preparing the titanium dioxide solution is fresh ethylene glycol EG, the concentration of the titanium dioxide solution is 25-35wt%, and the adding amount of the titanium dioxide solution is controlled according to the titanium dioxide content of 3.0% +/-0.02% in the polyester chip.
Further, the ceramic membrane in the step (2) is an inorganic ceramic membrane, and is a precision ceramic filter material with a porous structure formed by sintering alumina, titania, zirconia and the like at high temperature (a set of ceramic membrane purification treatment systems manufactured by Jiangsu Jiuwu corporation, membrane element models JW-CMF-U-005-19X 30X 1016, JW-CMF-U-002-19X 30X 1100).
Furthermore, the inorganic ceramic membrane finished product structure in the step (2) is that the inner porous supporting layer, the transition layer and the microporous membrane layer are in asymmetric distribution.
Further, when the membrane flux of the ceramic membrane in the step (2) is lower than 1500L/hr, the ceramic membrane is determined to be low in flux, the ceramic membrane is cleaned, and is cleaned and regenerated by adopting a water cleaning mode, and the ceramic membrane is continuously used after the membrane flux is recovered.
Further, the water cleaning mode is adopted, and the washing time is 30-60 min.
Further, the water cleaning adopts hot water at 60-80 ℃.
The invention provides a method for removing titanium dioxide of circulating EG in polyester production, which comprises the steps of firstly evaporating glycol mixed steam generated in an esterification process to obtain a recovered EG solution; then, carrying out ceramic membrane treatment on the recovered EG solution, and filtering to obtain the recycled EG solution; and (3) circulating a part of EG solution to a first esterification kettle to adjust esterification reaction, and mixing a large part of EG solution with external pure supplemental glycol after reaching a recycling glycol collecting tank to prepare slurry. The invention utilizes specific filtering separation equipment, and the filter mainly filters out titanium dioxide impurities to realize the recycling of EG; by adopting the removal process, the titanium dioxide removal rate is more than 99.5%.
Drawings
FIG. 1 is a schematic diagram of the polyester production process of the present invention.
FIG. 2 is a schematic flow chart of the removal of titania from recycled EG in the production of polyester according to the present invention.
Detailed Description
For a further understanding of the present invention, preferred embodiments of the invention are described below in conjunction with the examples, but it should be understood that these descriptions are merely intended to illustrate further features and advantages of the invention, and are not limiting of the claims of the invention.
The following examples were conducted to carry out the titania removal process of circulating EG in the polyester production, the specific flow is shown in FIGS. 1 and 2, and firstly, the glycol mixed steam generated in the esterification process is passed through a process tower to become a recovered EG solution; an external ceramic membrane is adopted on a glycol extraction pipeline of a process tower to treat and recycle EG solution, so as to obtain circulating EG solution to a clear liquid tank, and water insoluble matters such as titanium dioxide and the like are intercepted to become concentrated solution to a circulating tank; finally, the circulating EG solution is obtained after filtering, one part of the circulating EG solution is sent to a first esterification kettle for regulating esterification reaction, and the other part of the circulating EG solution is sent to a recycling glycol collecting tank for being mixed with external pure supplemental glycol to prepare slurry.
Example 1
1) The method comprises the steps of (1) generating ethylene glycol mixed steam under the conditions that the capacity of the full-extinction PET is 500t, the adding amount of a titanium dioxide solution with the concentration of 30wt% is about 5000kg/h, the esterification temperature is 258+/-2 ℃, the liquid level of an esterification kettle is 70+/-2% and the esterification pressure is normal pressure in the esterification process, and obtaining recovered EG solution containing 0.5% of titanium dioxide under the spraying condition of 25+/-1 ℃ through a process tower;
2) Filtering the recovered EG solution in a ceramic membrane under the conditions of the filtering pressure of 0.2Mpa and the filtering temperature of 23+/-1 ℃, filtering by a ceramic membrane purification treatment system produced by Jiangsu Jiuwu corporation, wherein the membrane element model JW-CMF-U-005-19X 30X 1016 is used as raw material liquid, the recovered EG solution flows in a membrane tube at a high speed, clear permeate containing small molecular components is driven by pressure to permeate the membrane outwards along the direction perpendicular to the clear permeate, and turbid concentrate containing large molecular components is intercepted by the membrane, so that the circulating EG solution is obtained to a clear liquid tank. Intercepting water insoluble matters such as titanium dioxide and the like into concentrated solution to a circulating tank;
when the membrane flux of the ceramic membrane is reduced, and when the membrane flux is lower than 1500L/hr, the membrane flux is determined to be low, and cleaning is required. And cleaning and regenerating by adopting a water cleaning mode. Washing with 65deg.C hot water for 30min, and continuing use after membrane flux is recovered;
3) The 40% -50% circulating EG solution in the clear solution tank is returned to the first esterification kettle for esterification reaction; the remaining solution was sent to a recycle EG collection tank and mixed with external pure make-up ethylene glycol for slurry preparation.
Experimental results show that the circulating EG solution prepared in this example has a titanium dioxide content of about 0.027% and a filtration efficiency of 94.6%.
Example 2
1) The method comprises the steps of (1) generating ethylene glycol mixed steam under the conditions that the capacity of the full-extinction PET is 500t, the adding amount of titanium dioxide solution with the concentration of 35wt% is about 5000kg/h, the esterification temperature is 258+/-2 ℃, the liquid level of an esterification kettle is 70+/-2% and the esterification pressure is normal pressure in the esterification process, and obtaining recovered EG solution containing 0.5% of titanium dioxide under the spraying condition of 25+/-1 ℃ through a process tower;
2) Filtering the recovered EG solution in a ceramic membrane under the conditions of the filtering pressure of 0.2Mpa and the filtering temperature of 23+/-1 ℃, filtering by a ceramic membrane purification treatment system produced by Jiangsu Jiuwu corporation, wherein the membrane element model JW-CMF-U-002-19X 30X 1100 is used as raw material liquid, the recovered EG solution flows in a membrane tube at a high speed, clear permeate containing small molecular components is driven by pressure to permeate the membrane outwards along the direction perpendicular to the clear permeate, and turbid concentrate containing large molecular components is intercepted by the membrane, so that the circulating EG solution is obtained to a clear liquid tank. Intercepting water insoluble matters such as titanium dioxide and the like into concentrated solution to a circulating tank;
when the membrane flux of the ceramic membrane is reduced, and when the membrane flux is lower than 1500L/hr, the membrane flux is determined to be low, and cleaning is required. And cleaning and regenerating by adopting a water cleaning mode. Cleaning with hot water at 75deg.C for 30min, and continuing to use when membrane flux is recovered;
3) The 40% -50% circulating EG solution in the clear solution tank is returned to the first esterification kettle for esterification reaction; the remaining solution was sent to a recycle EG collection tank and mixed with external pure make-up ethylene glycol for slurry preparation.
Experimental results show that the circulating EG solution prepared in this example has a titanium dioxide content of about 0.007% and a filtration efficiency of 98.6%.
The above description of the embodiments is only for aiding in the understanding of the method of the present invention and its core ideas. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
Claims (7)
1. A method for removing titania from recycled EG in the production of polyester, comprising:
1) Adding a titanium dioxide solution into a second esterification kettle for producing full-dull polyester PET, generating glycol mixed steam under the conditions that the esterification temperature is 258+/-2 ℃ and the liquid level of the esterification kettle is 70+/-2% and the esterification pressure is normal pressure in the esterification process, and spraying the glycol mixed steam at 25+/-1 ℃ to obtain a recovered EG solution; wherein the recovered EG solution comprises ethylene glycol and titanium dioxide impurities;
2) Filtering the recovered EG solution by a ceramic membrane, and obtaining the circulating EG solution to a clear liquid tank under the condition that the filtering pressure is 0.2Mpa and the filtering temperature is 23+/-1 ℃, wherein titanium dioxide impurities are intercepted to become concentrated solution to the circulating tank;
3) The 40% -50% circulating EG solution in the clear solution tank is returned to the first esterification kettle for esterification reaction; the remaining solution was sent to a recycle EG collection tank and mixed with external pure make-up ethylene glycol for slurry preparation.
2. The removal method according to claim 1, wherein: in the step (1), the solvent for preparing the titanium dioxide solution is fresh glycol EG, the concentration of the titanium dioxide solution is 25-35wt%, and the adding amount of the titanium dioxide solution is controlled according to the titanium dioxide content of 3.0% +/-0.02% in the polyester chip.
3. The removal method according to claim 1, wherein: the ceramic membrane in the step (2) is an inorganic ceramic membrane, and is a precise ceramic filter material with a porous structure, which is formed by sintering alumina, titanium oxide or zirconium oxide at high temperature.
4. The removal method according to claim 1, wherein: the inorganic ceramic membrane in the step (2) is internally provided with a porous supporting layer, a transition layer and a microporous membrane layer which are asymmetrically distributed.
5. The removal method according to claim 1, wherein: and (3) when the membrane flux of the ceramic membrane in the step (2) is lower than 1500L/hr, judging that the flux is low, cleaning and regenerating in a water cleaning mode, and continuing to use after the membrane flux is recovered.
6. The removal method according to claim 5, wherein: the water cleaning mode is adopted, and the washing time is 30-60 min.
7. The removal method according to claim 5, wherein: the water cleaning adopts hot water at 60-80 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011182529.1A CN114426663B (en) | 2020-10-29 | 2020-10-29 | Titanium dioxide removal method for circulating EG in polyester production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011182529.1A CN114426663B (en) | 2020-10-29 | 2020-10-29 | Titanium dioxide removal method for circulating EG in polyester production |
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| Publication Number | Publication Date |
|---|---|
| CN114426663A CN114426663A (en) | 2022-05-03 |
| CN114426663B true CN114426663B (en) | 2024-04-02 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1250405A (en) * | 1997-03-20 | 2000-04-12 | 伊斯曼化学公司 | Process for continuously producing polyester articles with scrap recycle in a continuous melt-to-preform process |
| CN1362448A (en) * | 1996-06-28 | 2002-08-07 | 东丽株式会社 | Titanium dioxide-contained resin composition |
| JP2006290910A (en) * | 2005-04-05 | 2006-10-26 | Toyobo Co Ltd | Polyester manufacturing method, polyester and polyester molded item |
| CN104479168A (en) * | 2014-11-18 | 2015-04-01 | 广东树业环保科技股份有限公司 | Waste PET (polyethylene terephthalate) decolorization recovery method, product and application |
| CN107445802A (en) * | 2017-08-21 | 2017-12-08 | 上海聚友化工有限公司 | A kind of method that ethylene glycol and acetaldehyde are reclaimed in polyester waste water |
-
2020
- 2020-10-29 CN CN202011182529.1A patent/CN114426663B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1362448A (en) * | 1996-06-28 | 2002-08-07 | 东丽株式会社 | Titanium dioxide-contained resin composition |
| CN1250405A (en) * | 1997-03-20 | 2000-04-12 | 伊斯曼化学公司 | Process for continuously producing polyester articles with scrap recycle in a continuous melt-to-preform process |
| JP2006290910A (en) * | 2005-04-05 | 2006-10-26 | Toyobo Co Ltd | Polyester manufacturing method, polyester and polyester molded item |
| CN104479168A (en) * | 2014-11-18 | 2015-04-01 | 广东树业环保科技股份有限公司 | Waste PET (polyethylene terephthalate) decolorization recovery method, product and application |
| CN107445802A (en) * | 2017-08-21 | 2017-12-08 | 上海聚友化工有限公司 | A kind of method that ethylene glycol and acetaldehyde are reclaimed in polyester waste water |
Non-Patent Citations (1)
| Title |
|---|
| PET装置EG降耗的措施;倪剑菁;张晓静;;聚酯工业;20110115(第01期);第25-27页 * |
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| CN114426663A (en) | 2022-05-03 |
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