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A kind of preparation method of polyester polyol

A technology of polyester polyol and polyol, applied in the field of preparation of polymer compounds, can solve the problems of long unit operation time, unfavorable biological utilization, easy oxidation and blackening, etc., and achieves shortened production time, reduced viscosity and low degree of coloring Effect

Active Publication Date: 2020-07-10
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] CN101168592A discloses a polyester polyol and its preparation method and application. The patented three-step method for preparing caprolactone-modified polyester polyol requires multiple operations of heating, cooling, and feeding. The steps are cumbersome and the unit operation time is Long, using transition metal compounds such as tin and pickaxe as catalysts, transition metal catalysts are easy to oxidize and blacken, causing material discoloration, and at the same time, transition metal catalysts have certain toxicity, which is not conducive to biological utilization

Method used

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  • A kind of preparation method of polyester polyol
  • A kind of preparation method of polyester polyol
  • A kind of preparation method of polyester polyol

Examples

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Effect test

Embodiment 1

[0035] Step 1: Weigh succinic acid (235g, 1.99mol), ethylene glycol (129.7g, 2.089mol) and ε-caprolactone (45.65g, 0.4mol), and add them under nitrogen protection until the The four-neck flask of the device, thermometer, gas inlet, and water-splitting condenser. Step 1: Heat the reaction mixture under the protection of nitrogen. When the temperature rises to 140°C, the water separator starts to discharge water. At this time, it is considered that the polycondensation reaction has started, so the rate of water discharge is controlled, and the temperature at the top of the container is 98-102°C to prevent The reaction was too intense, and the temperature was raised to about 160°C for 4 hours. Step 2: Add the catalyst BEMP with a total mass of 100ppm of the mixture and slowly raise the temperature to about 210°C, increase the stirring rate, and react for 2 hours. After the acid value is determined to be qualified, vacuumize and cool down, stop the water flow, and obtain the modif...

Embodiment 2

[0037] In the first step, weigh glutaric acid (216.6g, 1.617mol), propylene glycol (147.63g, 1.940mol) and ε-caprolactone (68.48g, 0.6mol) and add to an electric stirrer under nitrogen protection, Four flasks with thermometer, gas inlet, and separatory condenser. Step 1: Heat the reaction mixture under the protection of nitrogen. When the temperature rises to about 130°C, the water separator starts to discharge water. At this time, it is considered that the polycondensation reaction starts, and the water discharge rate is controlled. The temperature at the top of the container is 98-102°C. Avoid overreacting. Raise the temperature to about 165°C for 4.5 hours. The second step: add the catalyst P of mixture total mass 70ppm 1 -t-Bu slowly heat up to about 200°C, increase the stirring rate, and react for 1.5h. After the acid value is determined to be qualified, vacuumize and cool down, stop the water flow, and obtain the modified polyester polyol. The prepared caprolactone-mo...

Embodiment 3

[0039] The first step, weigh adipic acid (204g, 1.396mol), 1,4-butanediol (176.12g, 1.954mol) and ε-caprolactone (79.90g, 0.7mol), add to Four flasks equipped with electric stirrer, thermometer, gas inlet, and water separator condenser. Step 1: Heat the reaction mixture under the protection of nitrogen. When the temperature rises to about 140°C, the water separator starts to discharge water. At this time, it is considered that the polycondensation reaction starts, and the water discharge rate is controlled. The temperature at the top of the container is 98-102°C. To prevent the reaction from being too intense, raise the temperature to about 170°C for 2 hours. The second step: add the total mass of the mixture 50ppm catalyst P 1 -t-Oct, slowly raise the temperature to about 220°C, increase the stirring speed, and react for 2 hours. After the acid value is determined to be qualified, vacuumize and cool down, stop the water flow, and obtain the modified polyester polyol. The pr...

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Abstract

The invention discloses a preparation method of polyester polyol. The preparation method comprises the following steps of: (1) mixing at least one kind of dicarboxylic acid with at least one kind of polyol under the protection of inert gas, and performing an esterification reaction; and (2) then under an inert gas atmosphere and under the condition of an organic catalyst, heating the reaction liquid obtained in the step (1) and at least one kind of cyclic ester to 200-230 DEG C, and performing a transesterification reaction to obtain the polyester polyol. Compared with the prior art, a one-potcooking method is adopted to prepare the polyester polyol, operation steps of heating, cooling and feeding are reduced, the reaction is simplified, and the operation time is saved; through adoption of the metal-free catalyst, high catalytic activity is maintained, the reaction time is shortened, and the method is more environmentally friendly.

Description

technical field [0001] The invention relates to a preparation method of a polymer compound, in particular to a preparation method of polyester polyol. Background technique [0002] Polyester polyol is one of the important raw materials for the synthesis of polyurethane (PU), and it acts as a flexible soft segment in the synthesis of polyurethane. The polyester polyol required in polyurethane has a relatively low molecular weight, generally 1000-3000 g / mol. Polyester polyols are usually linear polymers prepared by polycondensation of dibasic acids and diols. The polycondensation reaction is a reversible reaction. Since the viscosity of the system increases in the later stage of the reaction, the water generated is not easy to discharge from the system. Measures such as raising the temperature, increasing the stirring rate and applying vacuum are required to maintain the reaction in the positive direction. However, if the reaction time at this stage is too long, it will not ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/60C08G63/78C08G63/91
CPCC08G63/60C08G63/78C08G63/916
Inventor 郭凯高晗朱宁胡欣李振江方正孟晶晶
Owner CHINA PETROLEUM & CHEM CORP
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