CN106554488A - A kind of PEPA production technology - Google Patents
A kind of PEPA production technology Download PDFInfo
- Publication number
- CN106554488A CN106554488A CN201610477538.0A CN201610477538A CN106554488A CN 106554488 A CN106554488 A CN 106554488A CN 201610477538 A CN201610477538 A CN 201610477538A CN 106554488 A CN106554488 A CN 106554488A
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- CN
- China
- Prior art keywords
- reaction
- pepa
- acid number
- different
- reactor
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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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
- C08G63/78—Preparation processes
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4244—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups
- C08G18/4247—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polyols containing at least one ether group and polycarboxylic acids
- C08G18/425—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polyols containing at least one ether group and polycarboxylic acids the polyols containing one or two ether groups
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
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- 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
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The present invention relates to chemical products production field, especially PEPA field.PEPA, Organic substance, typically by Dicarboxylic Acids（Anhydride or ester）With polyhydric alcohol（Including glycol）Condensation（Or ester exchange）Or formed with polymerization by lactone.Binary acid has phthalic acid or phthalate anhydride or its ester, adipic acid, halo phthalic acid etc..Polyhydric alcohol has ethylene glycol, Propylene Glycol, diglycol, trimethylolpropane, tetramethylolmethane etc.., as species is different or preparation technology is different, property is also different, and the several indexs important for PEPA are hydroxyl value, acid number, moisture, viscosity, molecular weight, density and colourity etc. for the PEPA of different cultivars.
Description
Technical field
The present invention relates to chemical products production field, especially PEPA field.
Background technology
PEPA, Organic substance, typically by Dicarboxylic Acids（Anhydride or ester）With polyhydric alcohol（Including glycol）Contracting
Close（Or ester exchange）Or formed with polymerization by lactone.Binary acid have phthalic acid or phthalate anhydride or its ester, oneself two
Acid, halo phthalic acid etc..Polyhydric alcohol has ethylene glycol, Propylene Glycol, diglycol, trimethylolpropane, tetramethylolmethane etc..
, as species is different or preparation technology is different, property is also different, for PEPA for the PEPA of different cultivars
Important several indexs are hydroxyl value, acid number, moisture, viscosity, molecular weight, density and colourity etc..The spy of PEPA
Property and purposes：The PAUR ester group more because intramolecular contains, amino isopolarity group, cohesive strength and adhesive force
By force, with higher intensity, wearability.Technological transformation project PEPA production technology is identical with existing engineering, is batch (-type)
Condensation process.Liquid material diethylene glycol, glycerol Jing gears are pumped into into reactor, solid-state PET material, terephthaldehyde first
Acid, catalyst are added by batching hole, close feeding hole and feeding valve, open blender, are heated up by heat-conducting oil heating, when
Kettle temperature adds p-phthalic acid when rising to 190 DEG C, is continuously heating to 210 DEG C, is incubated 3 hours, then proceedes to be warming up to 230 DEG C,
And be incubated.
The content of the invention
Technological process：
This reaction is carried out in closing jacket reactor, as reaction temperature is higher, is reacted to avoid reaction mass vaporization from escaping
Kettle, opens the condensing units on kettle top during heating, will boil the moisture content condensation of the polyhydric alcohol and reaction generation for, and Jing shuntings
Post is shunted, and alcohols is returned, and the moisture content for condensing out is reclaimed into material collection tank.Reaction about 24 hours
Complete, acid number is measured by sampling, as acid number≤10mgKOH/g, show that normal pressure esterification reaction is basically completed, stop upper heating.To make ester
Changing reaction is carried out completely, and vacuum pump is opened after stopping heating carrying out evacuation dehydration, and reaction is further reacted under condition of negative pressure,
Vacuum is gradually stepped up, and finally reaches 0.08 ~ 0.09Mpa, is maintained 1 hour or so, a small amount of moisture that reaction is generated is distillated, is taken
Sample determines acid number, and as acid number≤1.0mgKOH/g, reaction carries out completely, is then passed through cooling water to reacting kettle jacketing and dropped
Temperature, is down to 120 DEG C of dischargings.Product Jing kieselguhr is filtered, and after going the removal of impurity, Jing is cooled to room temperature, loads the packaging of plastic lining film
In bucket, sealing.
Project raw materials consumption catalog
Reaction equation：
Claims (2)
1. the present invention relates to material composition and proportioning.
2. the present invention relates to technological process：This reaction closing jacket reactor in carry out, due to reaction temperature it is higher, to avoid
Reaction mass vaporization effusion reactor, opens the condensing units on kettle top during heating, will boil the polyhydric alcohol and the reaction life that
Into moisture content condensation, and Jing shunting post shunting, alcohols return synthesis reactor in continue reaction, the moisture content for condensing out enter material receipts
Collection tank is reclaimed；Reaction is completed for about 24 hours, and acid number is measured by sampling, and as acid number≤10mgKOH/g, shows that normal pressure esterification reaction is basic
Complete, stop upper heating；To make esterification carry out completely, vacuum pump is opened after stopping heating carrying out evacuation dehydration, reacts
Further react under condition of negative pressure, vacuum is gradually stepped up, finally reach 0.08 ~ 0.09Mpa, maintain 1 hour or so, will reaction
The a small amount of moisture for generating is distillated, and acid number is measured by sampling, and as acid number≤1.0mgKOH/g, reaction is carried out completely, then to reactor
Chuck is passed through cooling water and is lowered the temperature, and is down to 120 DEG C of dischargings；Product Jing kieselguhr is filtered, and after going the removal of impurity, Jing is cooled to room temperature,
Load in the pail pack of plastic lining film, sealing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610477538.0A CN106554488A (en) | 2016-06-28 | 2016-06-28 | A kind of PEPA production technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610477538.0A CN106554488A (en) | 2016-06-28 | 2016-06-28 | A kind of PEPA production technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106554488A true CN106554488A (en) | 2017-04-05 |
Family
ID=58417312
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610477538.0A Pending CN106554488A (en) | 2016-06-28 | 2016-06-28 | A kind of PEPA production technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106554488A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114602399A (en) * | 2022-02-17 | 2022-06-10 | 苏州奥斯汀新材料科技有限公司 | Process method for shortening polyester polyol manufacturing time |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803878A (en) * | 2005-12-22 | 2006-07-19 | 辽阳东辰聚氨酯有限公司 | Polyester polyol for preparation of polyurethane foam, polyisocyanurate foam and polyurethane adhesive and preparation process thereof |
| CN102653589A (en) * | 2011-03-02 | 2012-09-05 | 上海诺科生物科技有限公司 | Water soluble or water dispersible polyester synthesized by utilizing waste polyester and application thereof in textile processing |
| CN104262596A (en) * | 2014-09-23 | 2015-01-07 | 四川东材科技集团股份有限公司 | High-functionality degree polyester polyol and preparation method thereof |
| CN104736599A (en) * | 2012-05-30 | 2015-06-24 | 巴斯夫欧洲公司 | Polyesterols for producing rigid polyurethane foams |
-
2016
- 2016-06-28 CN CN201610477538.0A patent/CN106554488A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803878A (en) * | 2005-12-22 | 2006-07-19 | 辽阳东辰聚氨酯有限公司 | Polyester polyol for preparation of polyurethane foam, polyisocyanurate foam and polyurethane adhesive and preparation process thereof |
| CN102653589A (en) * | 2011-03-02 | 2012-09-05 | 上海诺科生物科技有限公司 | Water soluble or water dispersible polyester synthesized by utilizing waste polyester and application thereof in textile processing |
| CN104736599A (en) * | 2012-05-30 | 2015-06-24 | 巴斯夫欧洲公司 | Polyesterols for producing rigid polyurethane foams |
| CN104262596A (en) * | 2014-09-23 | 2015-01-07 | 四川东材科技集团股份有限公司 | High-functionality degree polyester polyol and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114602399A (en) * | 2022-02-17 | 2022-06-10 | 苏州奥斯汀新材料科技有限公司 | Process method for shortening polyester polyol manufacturing time |
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| PB01 | Publication | ||
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170405 |
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| WD01 | Invention patent application deemed withdrawn after publication |