CN107879895A - A kind of EG kettles are residual and purify the method that EG is recycled - Google Patents
A kind of EG kettles are residual and purify the method that EG is recycled Download PDFInfo
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- CN107879895A CN107879895A CN201711158043.2A CN201711158043A CN107879895A CN 107879895 A CN107879895 A CN 107879895A CN 201711158043 A CN201711158043 A CN 201711158043A CN 107879895 A CN107879895 A CN 107879895A
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- Prior art keywords
- kettles
- residual
- ethylene glycol
- pet
- additive
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- 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
- C07C29/128—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by alcoholysis
- C07C29/1285—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by alcoholysis of esters of organic acids
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- 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
Abstract
The present invention relates to a kind of method that EG kettles are residual and purify EG recyclings, it is characterised in that it is concretely comprised the following steps：(1) ethylene glycol EG kettles is residual, ethylene glycol EG, PET PET and additive carry out alcoholysis reaction and obtain alcoholysate；(2) alcoholysate, methanol, additive three carry out ester exchange reaction, obtain dimethyl terephthalate (DMT) DMT and thick ethylene glycol EG, (3) are purified EG, and it is residual to obtain purification EG and EG kettles；It is residual in first step alcoholysis reaction, realizing reusing for waste that purification EG and EG kettles will be obtained.The EG kettles of the present invention are residual or containing the useful material such as a certain amount of EG, BHET, catalyst, and bigger reduction is had to production cost if it can be reused.
Description
Technical field
The present invention relates to the residual reutilization technology field of EG kettles, is that a kind of EG kettles are residual and purification EG is recycled specifically
Method.
Background technology
Polyester, the polymer general name as obtained by polyalcohol and polyacid polycondensation.Refer mainly to PET
(PET) linear thermoplastic's resins such as polybutylene terephthalate (PBT) and polyarylate, are traditionally also included.It is a kind of performance
Excellent, widely used engineering plastics.It may be made as polyester fiber and polyester film.Polyester includes polyester resin and polyester
Body.Polyester resin includes PET (PET), polybutylene terephthalate (PBT) again) and polyarylate
(PAR) etc..Polyester elastomer (TPEE) is typically polymerized by dimethyl terephthalate (DMT), BDO and poly- butanol, chain
Section includes hard section part and soft segment part, is thermoplastic elastomer (TPE).
It is residual in a large amount of EG kettles of polyester production process generation, the cost of enterprise how is utilized and reduced, turns into current one
Individual trend.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of residual side recycled with purification EG of EG kettles
Method.
The purpose of the present invention is achieved through the following technical solutions：
A kind of EG kettles are residual and purify the method that EG is recycled, and it is concretely comprised the following steps：
(1) ethylene glycol EG kettles is residual, ethylene glycol EG, PET PET and additive progress alcoholysis are anti-
Alcoholysate should be obtained；
Proportioning between ethylene glycol EG, PET (PET) and three parts of additive is：EG dosages
7-6 tons, amount of PET 2-3 tons, catalyst amount 120-125kg.
The specific material of additive is potassium carbonate
The concrete technology condition of alcoholysis reaction is：Material is heated to 200-230 DEG C with conduction oil and carries out alcoholysis reaction, instead
Kettle Stress control is answered hour in reaction time 4-6, to steam excessive moisture and EG, ultimately generate BHET to benzene two in 0.1-0.15Mpa
Formic acid glycol ester monomer；
(2) alcoholysate, methanol, additive three carry out ester exchange reaction, obtain dimethyl terephthalate (DMT) DMT and thick
Ethylene glycol EG,
Alcoholysate volume is 7-15m3, the volume of methanol is 9-16m3, the quality of catalyst is 110-210kg.
The specific material of additive is potassium carbonate and silicon carbide composite,
Silicon carbide composite is for the mixture of nanometer silicon carbide and titanium dioxide using grinding distribution in 1- butyl -3- methyl
In limidazolium hexafluorophosphate；Three's mass of nanometer silicon carbide, titanium dioxide and 1- butyl -3- methylimidazole hexafluorophosphates
Than for 1:1:5.TiO 2 particles are adsorbed using the loose structure of nanometer silicon carbide, are then redispersed in 1- butyl -3- methyl
In limidazolium hexafluorophosphate, formed and be sustained the porous performance such as hole cored structure, the gloss spinnability so as to increase product.
The concrete technology condition of ester exchange reaction is：Material is heated to 70-90 DEG C with 0.6Mpa steams, is being catalyzed
BHET (ethylene glycol terephthalate) is set to carry out ester exchange reaction with methanol under the catalytic action of agent, the reaction time is controlled 5
Hour or so, ultimately generate DMT (dimethyl terephthalate (DMT)) and EG (ethylene glycol).
(3) EG is purified, it is residual obtains purification EG and EG kettles；Purification will be obtained, and EG and EG kettles are residual is used for first step alcoholysis
In reaction, reusing for waste is realized.
Compared with prior art, the positive effect of the present invention is：
In RD processes, methanol and BHET (ethylene glycol terephthalate) carry out ester exchange chemical reaction generation DMT and
EG, wherein the DMT generated, by raw material of the process such as filtering, decolouring as production section, the EG generated in addition is due to containing face
Other impurities such as color are, it is necessary to further decolourize and purify, then purify and left part of decolourizing is exactly that kettle is residual.EG kettles
Residual the reason for needing to recycle and benefit：
Because EG kettles are residual or containing the useful material such as a certain amount of EG, BHET, catalyst, if it can be repeated
Bigger reduction is had using the production cost to us.
Embodiment
A kind of EG kettles of the present invention presented below are residual and purify the embodiment for the method that EG is recycled.
Embodiment 1
A kind of EG kettles are residual and purify the method that EG is recycled, and it is concretely comprised the following steps：
(1) ethylene glycol EG kettles is residual, ethylene glycol EG, PET PET and additive progress alcoholysis are anti-
Alcoholysate should be obtained；
Proportioning between ethylene glycol EG, PET (PET) and three parts of additive is：EG dosages
7 tons, 2 tons of amount of PET, catalyst amount 120kg.
The specific material of additive is potassium carbonate.
The concrete technology condition of alcoholysis reaction is：Material is heated to 200-230 DEG C with conduction oil and carries out alcoholysis reaction, instead
Kettle Stress control is answered hour in reaction time 4-6, to steam excessive moisture and EG, ultimately generate BHET to benzene two in 0.1-0.15Mpa
Formic acid glycol ester monomer；
(2) alcoholysate, methanol, additive three carry out ester exchange reaction, obtain dimethyl terephthalate (DMT) DMT and thick
Ethylene glycol EG,
Alcoholysate volume is 7m3, the volume of methanol is 9m3, the quality of catalyst is 110kg.
The specific material of additive is potassium carbonate and silicon carbide composite；Silicon carbide composite is nanometer silicon carbide and dioxy
The mixture for changing titanium uses grinding distribution in 1- butyl -3- methylimidazole hexafluorophosphates；Nanometer silicon carbide, titanium dioxide with
And three's mass ratio of 1- butyl -3- methylimidazole hexafluorophosphates is 1:1:7；
The concrete technology condition of ester exchange reaction is：Material is heated to 70-90 DEG C with 0.6Mpa steams, is being catalyzed
BHET (ethylene glycol terephthalate) is set to carry out ester exchange reaction with methanol under the catalytic action of agent, the reaction time is controlled 5
Hour or so, ultimately generate DMT (dimethyl terephthalate (DMT)) and EG (ethylene glycol).
(3) EG is purified, it is residual obtains purification EG and EG kettles；Purification will be obtained, and EG and EG kettles are residual is used for first step alcoholysis
In reaction, reusing for waste is realized.
Embodiment 2
A kind of EG kettles are residual and purify the method that EG is recycled, and it is concretely comprised the following steps：
(1) ethylene glycol EG kettles is residual, ethylene glycol EG, PET PET and additive progress alcoholysis are anti-
Alcoholysate should be obtained；
Proportioning between ethylene glycol EG, PET (PET) and three parts of additive is：EG dosages
7-6 tons, amount of PET 2-3 tons, catalyst amount 120-125kg.
The specific material of additive is potassium carbonate.
The concrete technology condition of alcoholysis reaction is：Material is heated to 200-230 DEG C with conduction oil and carries out alcoholysis reaction, instead
Kettle Stress control is answered hour in reaction time 4-6, to steam excessive moisture and EG, ultimately generate BHET to benzene two in 0.1-0.15Mpa
Formic acid glycol ester monomer；
(2) alcoholysate, methanol, additive three carry out ester exchange reaction, obtain dimethyl terephthalate (DMT) DMT and thick
Ethylene glycol EG,
Alcoholysate volume is 10m3, the volume of methanol is 12m3, the quality of catalyst is 150kg.
The specific material of additive is potassium carbonate and silicon carbide composite；Silicon carbide composite is nanometer silicon carbide and dioxy
The mixture for changing titanium uses grinding distribution in 1- butyl -3- methylimidazole hexafluorophosphates；Nanometer silicon carbide, titanium dioxide with
And three's mass ratio of 1- butyl -3- methylimidazole hexafluorophosphates is 1:1:7；
The concrete technology condition of ester exchange reaction is：Material is heated to 70-90 DEG C with 0.6Mpa steams, is being catalyzed
BHET (ethylene glycol terephthalate) is set to carry out ester exchange reaction with methanol under the catalytic action of agent, the reaction time is controlled 5
Hour or so, ultimately generate DMT (dimethyl terephthalate (DMT)) and EG (ethylene glycol).
(3) EG is purified, it is residual obtains purification EG and EG kettles；Purification will be obtained, and EG and EG kettles are residual is used for first step alcoholysis
In reaction, reusing for waste is realized.
Embodiment 3
A kind of EG kettles are residual and purify the method that EG is recycled, and it is concretely comprised the following steps：
(1) ethylene glycol EG kettles is residual, ethylene glycol EG, PET PET and additive progress alcoholysis are anti-
Alcoholysate should be obtained；
Proportioning between ethylene glycol EG, PET (PET) and three parts of additive is：EG dosages
6 tons, 3 tons of amount of PET, catalyst amount 125kg.
The specific material of additive is potassium carbonate.
The concrete technology condition of alcoholysis reaction is：Material is heated to 200-230 DEG C with conduction oil and carries out alcoholysis reaction, instead
Kettle Stress control is answered hour in reaction time 4-6, to steam excessive moisture and EG, ultimately generate BHET to benzene two in 0.1-0.15Mpa
Formic acid glycol ester monomer；
(2) alcoholysate, methanol, additive three carry out ester exchange reaction, obtain dimethyl terephthalate (DMT) DMT and thick
Ethylene glycol EG,
Alcoholysate volume is 15m3, the volume of methanol is 16m3, the quality of catalyst is 210kg.
The specific material of additive is potassium carbonate and silicon carbide composite；Silicon carbide composite is nanometer silicon carbide and dioxy
The mixture for changing titanium uses grinding distribution in 1- butyl -3- methylimidazole hexafluorophosphates；Nanometer silicon carbide, titanium dioxide with
And three's mass ratio of 1- butyl -3- methylimidazole hexafluorophosphates is 1:1:7；
The concrete technology condition of ester exchange reaction is：Material is heated to 70-90 DEG C with 0.6Mpa steams, is being catalyzed
BHET (ethylene glycol terephthalate) is set to carry out ester exchange reaction with methanol under the catalytic action of agent, the reaction time is controlled 5
Hour or so, ultimately generate DMT (dimethyl terephthalate (DMT)) and EG (ethylene glycol).
(3) EG is purified, it is residual obtains purification EG and EG kettles；Purification will be obtained, and EG and EG kettles are residual is used for first step alcoholysis
In reaction, reusing for waste is realized.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
Member, without departing from the inventive concept of the premise, can also make some improvements and modifications, these improvements and modifications also should be regarded as
In protection scope of the present invention.
Claims (6)
1. a kind of EG kettles are residual and purify the method that EG is recycled, it is characterised in that it is concretely comprised the following steps：
(1) ethylene glycol EG kettles is residual, ethylene glycol EG, PET PET and additive carry out alcoholysis reaction and obtained
To alcoholysate；
(2) alcoholysate, methanol, additive three carry out ester exchange reaction, obtain dimethyl terephthalate (DMT) DMT and thick second two
Alcohol EG, the specific material of additive is potassium carbonate and silicon carbide composite；Silicon carbide composite is nanometer silicon carbide and titanium dioxide
The mixture of titanium is using grinding distribution in 1- butyl -3- methylimidazole hexafluorophosphates；Nanometer silicon carbide, titanium dioxide and
Three's mass ratio of 1- butyl -3- methylimidazole hexafluorophosphates is 1:1:7；
(3) EG is purified, it is residual obtains purification EG and EG kettles；Purification will be obtained, and EG and EG kettles are residual is used for first step alcoholysis reaction
In, realize reusing for waste.
2. a kind of EG kettles as claimed in claim 1 are residual and purify the method that EG is recycled, it is characterised in that in step 1,
Proportioning between ethylene glycol EG, PET (PET) and three parts of additive is：EG dosage 7-6 tons,
Amount of PET 2-3 tons, catalyst amount 120-125kg.
3. a kind of EG kettles as claimed in claim 1 are residual and purify the method that EG is recycled, it is characterised in that in step 1,
The specific material of additive is potassium carbonate.
4. a kind of EG kettles as claimed in claim 1 are residual and purify the method that EG is recycled, it is characterised in that in step 1,
The concrete technology condition of alcoholysis reaction is：Material is heated to 200-230 DEG C with conduction oil and carries out alcoholysis reaction, reactor pressure
Control in 0.1-0.15Mpa, hour in reaction time 4-6, steam excessive moisture and EG, ultimately generate BHET terephthalic acid (TPA)s second two
Ester monomer.
5. a kind of EG kettles as claimed in claim 1 are residual and purify the method that EG is recycled, it is characterised in that in step 2,
Alcoholysate volume is 7-15m3, the volume of methanol is 9-16m3, the quality of catalyst is 110-210kg.
6. a kind of EG kettles as claimed in claim 1 are residual and purify the method that EG is recycled, it is characterised in that in step 2,
The concrete technology condition of ester exchange reaction is：Material is heated to 70-90 DEG C with 0.6Mpa steams, in the catalysis of catalyst
BHET (ethylene glycol terephthalate) is set to carry out ester exchange reaction with methanol under effect, the reaction time is controlled at 5 hours or so,
Ultimately generate DMT (dimethyl terephthalate (DMT)) and EG (ethylene glycol).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711158043.2A CN107879895A (en) | 2017-11-20 | 2017-11-20 | A kind of EG kettles are residual and purify the method that EG is recycled |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711158043.2A CN107879895A (en) | 2017-11-20 | 2017-11-20 | A kind of EG kettles are residual and purify the method that EG is recycled |
Publications (1)
| Publication Number | Publication Date |
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| CN107879895A true CN107879895A (en) | 2018-04-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711158043.2A Pending CN107879895A (en) | 2017-11-20 | 2017-11-20 | A kind of EG kettles are residual and purify the method that EG is recycled |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023076217A1 (en) * | 2021-10-25 | 2023-05-04 | Eastman Chemical Company | Processes for recovering dialkyl terephthalates from polyester compositions |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5051528A (en) * | 1990-04-24 | 1991-09-24 | Eastman Kodak Company | Recovery process for ethylene glycol and dimethylterephthalate |
| JP2002060536A (en) * | 2000-08-22 | 2002-02-26 | Teijin Ltd | Method for recovering valuable component from polyester waste |
| CN1413178A (en) * | 1999-10-22 | 2003-04-23 | 帝人株式会社 | Method for separating and recovering dimethyl terephthalate and ethylene glycol from polyester waste |
| CN102153443A (en) * | 2011-02-23 | 2011-08-17 | 合肥工业大学 | Method for degrading polyethylene terephthalate |
| CN102225994A (en) * | 2011-05-10 | 2011-10-26 | 浙江比例包装股份有限公司 | Nanometer composite catalyst for synthesis of polyester and copolyester, and synthetic method for polyester and copolyester |
-
2017
- 2017-11-20 CN CN201711158043.2A patent/CN107879895A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5051528A (en) * | 1990-04-24 | 1991-09-24 | Eastman Kodak Company | Recovery process for ethylene glycol and dimethylterephthalate |
| CN1413178A (en) * | 1999-10-22 | 2003-04-23 | 帝人株式会社 | Method for separating and recovering dimethyl terephthalate and ethylene glycol from polyester waste |
| JP2002060536A (en) * | 2000-08-22 | 2002-02-26 | Teijin Ltd | Method for recovering valuable component from polyester waste |
| CN102153443A (en) * | 2011-02-23 | 2011-08-17 | 合肥工业大学 | Method for degrading polyethylene terephthalate |
| CN102225994A (en) * | 2011-05-10 | 2011-10-26 | 浙江比例包装股份有限公司 | Nanometer composite catalyst for synthesis of polyester and copolyester, and synthetic method for polyester and copolyester |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023076217A1 (en) * | 2021-10-25 | 2023-05-04 | Eastman Chemical Company | Processes for recovering dialkyl terephthalates from polyester compositions |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20191202 Address after: 312071 building 7, No. 5, Paojiang Haitang Road, Shaoxing, Zhejiang Province Applicant after: Zhejiang beauty New Material Co., Ltd. Address before: 312071 Zhejiang city of Shaoxing Province on economic and Technological Development Zone Paojiang Road No. 5 Applicant before: Zhejiang beauty New Material Co., Ltd. Applicant before: Zhejiang Jiabao New Fiber Group Co., Ltd. Applicant before: ZHEJIANG JIABAO POLYESTER CO., LTD. |
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| TA01 | Transfer of patent application right | ||
| CB02 | Change of applicant information |
Address after: Building 7, No.5, Haitang Road, Yuecheng District, Shaoxing City, Zhejiang Province Applicant after: ZHEJIANG JIAREN NEW MATERIALS Co.,Ltd. Address before: 312071 building 7, No. 5, Paojiang Haitang Road, Shaoxing, Zhejiang Province Applicant before: ZHEJIANG JIAREN NEW MATERIALS Co.,Ltd. |
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Application publication date: 20180406 |
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| RJ01 | Rejection of invention patent application after publication |