CN106750212A - The synthetic method of castor oil acid based polyester polyol - Google Patents
The synthetic method of castor oil acid based polyester polyol Download PDFInfo
- Publication number
- CN106750212A CN106750212A CN201611140172.4A CN201611140172A CN106750212A CN 106750212 A CN106750212 A CN 106750212A CN 201611140172 A CN201611140172 A CN 201611140172A CN 106750212 A CN106750212 A CN 106750212A
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- CN
- China
- Prior art keywords
- castor oil
- polyester polyol
- acid based
- based polyester
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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
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/68—Unsaturated polyesters
-
- 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
- C08G63/46—Polyesters chemically modified by esterification
- C08G63/48—Polyesters chemically modified by esterification by unsaturated higher fatty oils or their acids; by resin acids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The synthetic method of castor oil acid based polyester polyol of the present invention is related to polyurethane industrial field, and in particular to the synthetic method of castor oil acid based polyester polyol, comprises the following steps：The preparation of castor oil methyl esters, in the 500mL three-neck flasks equipped with electric mixer, reflux condenser and thermometer, adds the castor oil 250g processed by predrainage, after being heated to 35 degree through water bath with thermostatic control, adds the KOH CH of 54g5%30H solution, after stirring reaction 2h, adds 10%HCl to be neutralized to pH value 4 4.5, reaction solution is poured into separatory funnel, stratification, separate lower floor's glycerine methanol solution, supernatant liquid is washed 3 times to neutral, vacuum distillation water removal with 100mL deionized waters, obtains the castor oil methyl esters of 247g clears；The present invention is simple to operate, convenient processing, and can guarantee that product quality, enhances product performance, with preferable film forming, hardness higher, excellent adhesive force and preferable water-fast, oil resistivity.
Description
Technical field
The present invention relates to polyurethane industrial field, and in particular to the synthetic method of castor oil acid based polyester polyol.
Background technology
PEPA is the primary raw material for preparing polyurethane material, can be used to preparing polyurethane rubber, elastomer, gluing
The materials such as agent, coating, foam.PEPA type polyurethane resin has excellent wear-resisting, resistance to gentle oil resistance, wherein with
Adipate polyester polyalcohol is the formation series of products of representative.Current PEPA is raw materials used to be coming substantially from
Oil product, with the increasingly consumption of petroleum resources, produces polyurethane material and gets over using renewable resource replacement petroleum resources
It is valued by people to get over.
Castor oil is a kind of reproducible polyalcohol with three-functionality-degree, but because its relative molecular mass is smaller, no
Current industrialized polyalcohol can be completely substituted to use, and because as a kind of alcohol of polyfunctionality, in use,
Can cause to prepare polyurethane reaction and cause cross-linking reaction and limit its large-scale application.Using castor oil, PPG,
Diformazan phenylisocyanate and dihydromethyl propionic acid have been synthesized the aqueous polyurethane with certain degree of cross linking, with preferably into
Film, hardness higher, excellent adhesive force and preferable water-fast, oil resistivity.
The content of the invention
It is a kind of simple to operate present invention aim at providing, convenient processing, and product quality is can guarantee that, improve product
Can, gather with preferable film forming, hardness higher, excellent adhesive force and preferable water-fast, oil resistivity castor oil acidic group
The synthetic method of ester polyol.
The synthetic method of castor oil acid based polyester polyol of the present invention, comprises the following steps：
The first step, the preparation of castor oil methyl esters
In the 500mL three-neck flasks equipped with electric mixer, reflux condenser and thermometer, add what is processed by predrainage
Castor oil 250g, after being heated to 35 degree through water bath with thermostatic control, adds the KOH-CH of 54g5%30H solution, after stirring reaction 2h, adds
10%HCl is neutralized to pH value 4-4.5, and reaction solution is poured into separatory funnel, stratification, separates lower floor's glycerine-methanol solution,
Supernatant liquid is washed 3 times to neutral, vacuum distillation water removal with 100mL deionized waters, obtains the castor oil first of 247g clears
Ester；
Second step, the synthesis of castor oil acid based polyester polyol dihydroxylic alcohols
Castor oil methyl esters obtained above, adipic acid, ethylene glycol are added to equipped with agitator, thermometer, logical nitrogen, condenser pipe
In the 500mL four-hole boiling flasks of discharging device, lead to nitrogen 30min with the air in exclusion system, heating under nitrogen protection rises
140 degree beginning polycondensation reactions of temperature, temperature reaches 180-185 degree in question response system, then after being incubated 1.5h, adds catalyst, guarantor
Temperature 3 h of reaction, stop logical nitrogen, and vacuum decompression under 180 degree, 6.7kPa after 2 h of reaction, is cooled to 120 degree, obtains castor oil
Acid based polyester polyol.
Preferably, catalyst is tetra-n-butyl titanate.
The present invention is simple to operate, convenient processing, and can guarantee that product quality, enhances product performance, with preferable film forming
Property, hardness higher, excellent adhesive force and preferably water-fast, oil resistivity.
Specific embodiment
Embodiment one：
The synthetic method of castor oil acid based polyester polyol of the present invention, comprises the following steps：
The first step, the preparation of castor oil methyl esters
In the 500mL three-neck flasks equipped with electric mixer, reflux condenser and thermometer, add what is processed by predrainage
Castor oil 250g, after being heated to 35 degree through water bath with thermostatic control, adds the KOH-CH of 54g5%30H solution, after stirring reaction 2h, adds
10%HCl is neutralized to pH value 4-4.5, and reaction solution is poured into separatory funnel, stratification, separates lower floor's glycerine-methanol solution,
Supernatant liquid is washed 3 times to neutral, vacuum distillation water removal with 100mL deionized waters, obtains the castor oil first of 247g clears
Ester；
Second step, the synthesis of castor oil acid based polyester polyol dihydroxylic alcohols
Castor oil methyl esters obtained above, adipic acid, ethylene glycol are added to equipped with agitator, thermometer, logical nitrogen, condenser pipe
In the 500mL four-hole boiling flasks of discharging device, lead to nitrogen 30min with the air in exclusion system, heating under nitrogen protection rises
140 degree beginning polycondensation reactions of temperature, temperature reaches 180-185 degree in question response system, then after being incubated 1.5h, adds catalyst, guarantor
Temperature 3 h of reaction, stop logical nitrogen, and vacuum decompression under 180 degree, 6.7kPa after 2 h of reaction, is cooled to 120 degree, obtains castor oil
Acid based polyester polyol.
Embodiment two：
The synthetic method of castor oil acid based polyester polyol of the present invention, comprises the following steps：
The first step, the preparation of castor oil methyl esters
In the 500mL three-neck flasks equipped with electric mixer, reflux condenser and thermometer, add what is processed by predrainage
Castor oil 250g, after being heated to 35 degree through water bath with thermostatic control, adds the KOH-CH of 54g5%30H solution, after stirring reaction 2h, adds
10%HCl is neutralized to pH value 4-4.5, and reaction solution is poured into separatory funnel, stratification, separates lower floor's glycerine-methanol solution,
Supernatant liquid is washed 3 times to neutral, vacuum distillation water removal with 100mL deionized waters, obtains the castor oil first of 247g clears
Ester；
Second step, the synthesis of castor oil acid based polyester polyol dihydroxylic alcohols
Castor oil methyl esters obtained above, adipic acid, ethylene glycol are added to equipped with agitator, thermometer, logical nitrogen, condenser pipe
In the 500mL four-hole boiling flasks of discharging device, lead to nitrogen 30min with the air in exclusion system, heating under nitrogen protection rises
140 degree beginning polycondensation reactions of temperature, temperature reaches 180-185 degree in question response system, then after being incubated 1.5h, adds catalyst, guarantor
Temperature 3 h of reaction, stop logical nitrogen, and vacuum decompression under 180 degree, 6.7kPa after 2 h of reaction, is cooled to 120 degree, obtains castor oil
Acid based polyester polyol.
Catalyst is tetra-n-butyl titanate.
Embodiment three：
The synthetic method of castor oil acid based polyester polyol of the present invention, comprises the following steps：
The first step, the preparation of castor oil methyl esters
In the 500mL three-neck flasks equipped with electric mixer, reflux condenser and thermometer, add what is processed by predrainage
Castor oil 250g, after being heated to 35 degree through water bath with thermostatic control, adds the KOH-CH of 54g5%30H solution, after stirring reaction 2h, adds
10%HCl is neutralized to pH value 4-4.5, and reaction solution is poured into separatory funnel, stratification, separates lower floor's glycerine-methanol solution,
Supernatant liquid is washed 3 times to neutral, vacuum distillation water removal with 100mL deionized waters, obtains the castor oil first of 247g clears
Ester；
Second step, the synthesis of castor oil acid based polyester polyol dihydroxylic alcohols
Castor oil methyl esters obtained above, adipic acid, ethylene glycol are added to equipped with agitator, thermometer, logical nitrogen, condenser pipe
In the 500mL four-hole boiling flasks of discharging device, lead to nitrogen 30min with the air in exclusion system, heating under nitrogen protection rises
140 degree beginning polycondensation reactions of temperature, temperature reaches 180-185 degree in question response system, then after being incubated 1.5h, adds catalyst, guarantor
Temperature 3 h of reaction, stop logical nitrogen, and vacuum decompression under 180 degree, 6.7kPa after 2 h of reaction, is cooled to 120 degree, obtains castor oil
Acid based polyester polyol.
Catalyst is tetra-n-butyl titanate.
The present invention is simple to operate, convenient processing, and can guarantee that product quality, enhances product performance, with preferable film forming
Property, hardness higher, excellent adhesive force and preferably water-fast, oil resistivity.
Claims (2)
1. a kind of synthetic method of castor oil acid based polyester polyol, it is characterised in that comprise the following steps：
The first step, the preparation of castor oil methyl esters
In the 500mL three-neck flasks equipped with electric mixer, reflux condenser and thermometer, add what is processed by predrainage
Castor oil 250g, after being heated to 35 degree through water bath with thermostatic control, adds the KOH-CH of 54g5%30H solution, after stirring reaction 2h, adds
10%HCl is neutralized to pH value 4-4.5, and reaction solution is poured into separatory funnel, stratification, separates lower floor's glycerine-methanol solution,
Supernatant liquid is washed 3 times to neutral, vacuum distillation water removal with 100mL deionized waters, obtains the castor oil first of 247g clears
Ester；
Second step, the synthesis of castor oil acid based polyester polyol dihydroxylic alcohols
Castor oil methyl esters obtained above, adipic acid, ethylene glycol are added to equipped with agitator, thermometer, logical nitrogen, condenser pipe
In the 500mL four-hole boiling flasks of discharging device, lead to nitrogen 30min with the air in exclusion system, heating under nitrogen protection rises
140 degree beginning polycondensation reactions of temperature, temperature reaches 180-185 degree in question response system, then after being incubated 1.5h, adds catalyst, guarantor
Temperature 3 h of reaction, stop logical nitrogen, and vacuum decompression under 180 degree, 6.7kPa after 2 h of reaction, is cooled to 120 degree, obtains castor oil
Acid based polyester polyol.
2. the synthetic method of castor oil acid based polyester polyol as claimed in claim 1, it is characterised in that the catalyst is titanium
Sour four N-butyls.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611140172.4A CN106750212A (en) | 2016-12-12 | 2016-12-12 | The synthetic method of castor oil acid based polyester polyol |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611140172.4A CN106750212A (en) | 2016-12-12 | 2016-12-12 | The synthetic method of castor oil acid based polyester polyol |
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| CN106750212A true CN106750212A (en) | 2017-05-31 |
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| CN201611140172.4A Pending CN106750212A (en) | 2016-12-12 | 2016-12-12 | The synthetic method of castor oil acid based polyester polyol |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109721715A (en) * | 2018-12-13 | 2019-05-07 | 南京长江涂料有限公司 | A kind of decompression technique is for alkyd resin and preparation method thereof |
| CN111662634A (en) * | 2020-06-24 | 2020-09-15 | 广东达尔新型材料有限公司 | Thin-coating type water-based anti-static polyurethane mortar floor coating and preparation method thereof |
| CN113980637A (en) * | 2021-11-01 | 2022-01-28 | 烟台德邦科技股份有限公司 | Low-viscosity low-density polyurethane pouring sealant |
| CN114854475A (en) * | 2022-06-06 | 2022-08-05 | 广州润泰新材料科技有限公司 | Vegetable oil-based biodegradable lubricating oil with good stability and preparation method thereof |
-
2016
- 2016-12-12 CN CN201611140172.4A patent/CN106750212A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109721715A (en) * | 2018-12-13 | 2019-05-07 | 南京长江涂料有限公司 | A kind of decompression technique is for alkyd resin and preparation method thereof |
| CN111662634A (en) * | 2020-06-24 | 2020-09-15 | 广东达尔新型材料有限公司 | Thin-coating type water-based anti-static polyurethane mortar floor coating and preparation method thereof |
| CN111662634B (en) * | 2020-06-24 | 2021-12-07 | 广东达尔新型材料有限公司 | Thin-coating type water-based anti-static polyurethane mortar floor coating and preparation method thereof |
| CN113980637A (en) * | 2021-11-01 | 2022-01-28 | 烟台德邦科技股份有限公司 | Low-viscosity low-density polyurethane pouring sealant |
| CN114854475A (en) * | 2022-06-06 | 2022-08-05 | 广州润泰新材料科技有限公司 | Vegetable oil-based biodegradable lubricating oil with good stability and preparation method thereof |
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Application publication date: 20170531 |