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Method for synthesizing linear and multifunctional polyester polyol by using double epoxy compound

A technology of diepoxy compound and polyester polyol, applied in the direction of adhesive type, polyurea/polyurethane adhesive, adhesive, etc., can solve the problem of unadjusted alkyd ratio and limited increase of polyester functionality problems, to avoid the problem of metal residues, increase the yield of polyester, and shorten the reaction time.

Pending Publication Date: 2020-04-28
无锡博锦高分子研究发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The methods for synthesizing high-functionality polyesters such as CN101851328B, CN1649931A, CN103360588A, and CN104262596B cannot avoid producing branched chain polyesters, and the functionality of polyesters is all limited within a certain range to avoid product gelation.
[0003] In addition, the use of diepoxy or polyepoxides to extend the chain of polyester polyols has also been reported, indicating that the use of epoxy compounds to react with carboxyl or hydroxyl groups in polyester can extend the chain and increase viscosity of PET. There is no description on the increase of polyester functionality by diepoxy compounds, and the existing public information and research on the increase of polyester functionality are limited (the average functionality is in the range of 2-4)
Patents CN110256657A and CN110156970A synthesize polyester polyols with different properties by using monoepoxy compounds, and WO2015127276A1 terminates the esterification reaction by end-capping polyester with monoepoxy compounds, indicating that epoxy compounds are important in the synthesis of polyester polyols. Alcohols have great application prospects, but none of them have made specific reports on the synthesis of linear, multifunctional polyesters from diepoxy compounds by adjusting the alkyd-acid ratio

Method used

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  • Method for synthesizing linear and multifunctional polyester polyol by using double epoxy compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Example 1: Add 721.33g (6.10mol) of 1,6-hexanediol, 1278.67g (6.32mol) of sebacic acid, and 6g of antioxidant into a 2L four-necked flask, heat up and blow in nitrogen, and the system reaches Water began to flow out at 150°C, and the temperature was gradually raised to 230°C. After a period of heat preservation, 0.28 g of tetrabutyl titanate was added to continue the reaction. After a period of time, gradient vacuuming was started, and the temperature at the top of the reflux tower was maintained at a maximum of 90°C until the vacuum degree reached -0.095Mbar, keep vacuuming around 230°C, monitor the acid value and hydroxyl value, after about 13 hours, the measured AV=19.5mgKOH / g, release the vacuum, blow nitrogen, reduce the reaction temperature to 190-200°C, add bisphenol F-diglycidyl ether 74.0g, after 1h (AN=7.5mgKOH / g, OHV=12.52), add bisphenol F-diglycidyl ether 38.6g again, continue to react for 2h, measured AN=3.6mgKOH / g, The reaction was stopped, and the reacti...

Embodiment 2

[0060] Example 2: Add 721.33g (6.10mol) of 1,6-hexanediol, 1278.67g (6.32mol) of sebacic acid, and 6g of antioxidant into a 2L four-necked flask, heat up and blow in nitrogen, and the system reaches Water began to flow out at 150°C, and the temperature was gradually raised to 230°C. After a period of heat preservation, 0.28 g of tetrabutyl titanate was added to continue the reaction. After a period of time, gradient vacuuming was started, and the temperature at the top of the reflux tower was maintained at a maximum of 90°C until the vacuum degree reached -0.095Mbar, keep vacuuming at around 230°C, monitor the acid value and hydroxyl value, after about 13 hours, measure AV=19.1mgKOH / g, release the vacuum, blow nitrogen, reduce the reaction temperature to 190-200°C, add bisphenol F-diglycidyl ether 59.1g, after 1h (AN=11.7mgKOH / g, OHV=10.79), add bisphenol F-diglycidyl ether 45.2g again, continue to react for 2h (AN=4.6mgKOH / g, OHV= 16.98), add 9.7g of bisphenol F-diglycidyl et...

Embodiment 3

[0062]Embodiment 3: In order to make the acid value of the polyester in the embodiment 1 smaller, and no gel phenomenon occurs, a single epoxy compound is then added for end-capping. Take 1000.54g of the polyester of Example 1 into a 2L four-neck flask, add 15.08g of monoepoxy Cardura E10P, and react with nitrogen gas at 190-200°C for 2 hours to obtain a polyester product with an acid value of less than 2mgKOH / g. The test results are shown in Table 1 . Comparing this example with Example 1 and Example 2, it can be seen that the use of a single epoxy compound to end-cap the polyester polyol can effectively reduce the acid value (increase the reaction process), and maintain the functionality of the polyester polyol, The basic indicators of viscosity and molecular weight are equivalent to those after the diepoxy reaction, which effectively expands the application range of the polyester polyol. This example obtained the polyester product with acid value lower than 1 while obtaini...

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Abstract

The invention relates to the technical field of polyester polyol preparation, in particular to a method for synthesizing linear and multifunctional polyester polyol by using a double epoxy compound. Specifically, the method is characterized by adjusting the feeding ratio of dihydric alcohol to binary acid, when the reaction is carried out to a certain degree (acid value), a diepoxy compound is added, the functionality of the linear polyester polyol can be greater than any value (such as 2-10) of 2, and the product does not have a gel phenomenon in the synthesis process, which cannot be realized by synthesizing the polyfunctional polyester polyol by using trihydric alcohol or tribasic acid small molecules as an initiator. Particularly, only when the OH / COOH ratio (1.0 (i.e., COOH / OH is greater than 1), high-hydroxyl-value polyester polyol with the functionality of more than 4 can be synthesized, and linear polyol which cannot be gelled can be obtained. The product is widely applied to adhesives, synthetic leather, rubber and composite material products, and has practical application value.

Description

technical field [0001] The invention relates to the technical field of preparation of polyester polyols, in particular to a method for synthesizing linear and multifunctional polyester polyols using diepoxides. Background technique [0002] Polyester polyol is one of the important basic chemical raw materials. Its temperature resistance, wear resistance, oil resistance and mechanical strength are very outstanding. It is widely used in the fields of adhesives, synthetic leather, rubber, composite materials and other product manufacturing and modification. . Among them, the industrial bifunctional polyester polyol is obtained by gradual polymerization of diols and dibasic acids, while the synthesis of industrial multifunctional polyester polyols generally requires the use of polyacids or polyols as initiators. It is obtained by esterification and polycondensation reaction. This method not only makes the polyester branched, but even has the risk of gelation, and the functional...

Claims

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Application Information

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IPC IPC(8): C08G63/672C08G63/78C08L75/06C09J175/06
CPCC08G63/672C08G63/78C08L75/06C09J175/06
Inventor 陈旨进卓聪聪
Owner 无锡博锦高分子研究发展有限公司
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