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Preparation method of polyester polyol

A polyester polyol and polyol technology, applied in the field of polymer synthesis, can solve the problems of poor heat resistance and difficult application, and achieve the effect of high heat resistance

Active Publication Date: 2020-05-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Traditional polyester polyols are all obtained with organic acids, anhydrides or organic acid esters as raw materials, and have poor heat resistance, and the initial decomposition temperature is generally lower than 300°C (CN106660252A; Synthesis of acrylic pimaric acid polyester polyols and Research on its properties [J]. Forest Products Chemistry and Industry, 1999, (02): 63-67.), it is difficult to apply in the field requiring high heat resistance

Method used

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  • Preparation method of polyester polyol
  • Preparation method of polyester polyol

Examples

Experimental program
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Effect test

Embodiment approach

[0074] According to an embodiment of the present application, the polyester polyol polymer and its synthesis method are characterized in that the method comprises the following steps:

[0075] a) Mix inorganic oxyester, polyol and transesterification reaction catalyst in a three-necked flask evenly, carry out transesterification reaction under agitation, connect a distillation device, pass nitrogen protection, and the reaction temperature is between 80-180°C. The time ranges from 2 to 10 hours, and the conversion rate of the transesterification reaction ranges from 60% to 80%.

[0076] b) Connect the device after the reaction in step a) to a water pump or an oil pump for vacuum distillation to make the transesterification reaction more complete. The vacuum degree of the control system is 0.01-5KPa, the reaction temperature is between 170-230°C, and the reaction time is between After 0.5 to 5 hours, the conversion rate of the transesterification reaction is greater than 90%.

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Embodiment 1

[0088] Add 10g 1,3-propanediol, 6.84g ethyl orthosilicate and 5g methyl orthosilicate to a three-neck flask, connect to a distillation device, add 0.12g concentrated sulfuric acid as a catalyst dropwise under stirring, and raise the temperature under nitrogen protection to 100°C, the reaction time is 6 hours, a large amount of methanol and ethanol are distilled out during this process, and the conversion rate of the transesterification reaction is 75%; The vacuum degree is 1KPa, and the temperature is raised to 170°C. After one hour of reaction, the reaction is stopped, and after the temperature is naturally cooled to room temperature, the sample is taken out. The conversion rate of the transesterification reaction is 93%.

Embodiment 2

[0090] Add 5g of ethylene glycol and 8.7g of aluminum triethoxide into the three-necked flask, wherein the aluminum triethoxide is used not only as an inorganic oxo acid salt raw material, but also as a transesterification catalyst, connected to a distillation device, under the condition of stirring and nitrogen protection The temperature was raised to 175°C, and the reaction time was 5 hours. During this process, a large amount of ethanol was distilled out, and the conversion rate of the transesterification reaction was 73%; then a vacuum device was connected, and the reaction was carried out under reduced pressure distillation conditions, and the vacuum of the system was controlled. The temperature was 0.1KPa, and the temperature was raised to 210° C. After one hour of reaction, the reaction was stopped, and after cooling down to room temperature naturally, a sample was taken out, and the conversion rate of the transesterification reaction was 92%.

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Abstract

The invention discloses a preparation method of polyester polyol. The method comprises the following steps: carrying out a transesterification reaction on raw materials containing inorganic oxacid ester and polyol to obtain the polyester polyol. The polyester polyol obtained by the method provided by the invention has high heat resistance.

Description

technical field [0001] The application relates to a preparation method of polyester polyol, which belongs to the field of polymer synthesis. Background technique [0002] Polyester polyol is obtained by polycondensation of dibasic organic carboxylic acid, carboxylic anhydride and polyol, and its relative molecular mass is generally less than 4500. Among them, the dibasic acid includes phthalic acid or phthalic anhydride or its ester, adipic acid, halogenated phthalic acid, etc., and the polyols include ethylene glycol, propylene glycol, diethylene glycol, trimethylolpropane, Pentaerythritol, etc. The types of polyester polyols are generally classified by carboxylic acids, usually as follows: adipic acid-based polyester polyols, alkyd-based polyester polyols, caprolactone-based polyester polyols, acrylic-based polyester polyols . The production methods of polyester polyols include vacuum dehydration method and high temperature nitrogen dehydration method. Vacuum dehydrati...

Claims

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Application Information

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IPC IPC(8): C08G63/698C08G63/68C08G63/692C08G63/00
CPCC08G63/00C08G63/681C08G63/692C08G63/698
Inventor 袁丹华邢嘉成徐云鹏刘中民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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