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Preparation method of light-colored polycaprolactone and product prepared from light-colored polycaprolactone

A technology of polycaprolactone and caprolactone, which is applied in the field of polyester synthesis, can solve the problems of polycaprolactone yellowing and yellowing, and achieve the effect of solving the yellowing of products

Inactive Publication Date: 2022-04-15
DAICEL (CHINA) INVESTMENT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, in the high temperature polymerization of caprolactone, yellowing problem still exists
The inventors of the present invention have found that this is because the hindered phenol as an antioxidant reacts with the oxygen free radicals formed by residual oxygen molecules and is oxidized into darker quinone compounds, so it is easy to cause serious damage to the polycaprolactone as the product. yellowing problem

Method used

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  • Preparation method of light-colored polycaprolactone and product prepared from light-colored polycaprolactone
  • Preparation method of light-colored polycaprolactone and product prepared from light-colored polycaprolactone
  • Preparation method of light-colored polycaprolactone and product prepared from light-colored polycaprolactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 100 parts by mass of caprolactone monomer (produced by Daicel Co., Ltd.), 0.3 parts by mass of a ring-opening catalyst (p-toluenesulfonic acid monohydrate, produced by Adamas), 0.1 parts by mass of PEP-8T (Dioctadecyl pentaerythritol bisphosphite, from Aidike (China) Investment Co., Ltd.), under nitrogen protection conditions, after the temperature of the reaction solution reaches 200 degrees Celsius, stir for four hours. After the reaction, immediately take a sample and use a petroleum colorimeter to measure the APHA chromaticity of the sample. The APHA chromaticity of the sample can be measured to be 36. The number average molecular weight measured by GPC was 15496.

[0041]

Embodiment 2

[0043] In the reaction vessel, add 100 parts by mass of caprolactone monomer (produced by Daicel Corporation), 0.3 parts by mass of ring-opening catalyst (p-toluenesulfonic acid monohydrate, produced by Adamas), 0.1 parts by mass of 3010W (produced by Produced by Nanxiong Zhiyi Fine Chemical Co., Ltd., it is diisodecyl pentaerythritol diphosphite, similar to the phosphite of PEP-8T structure), adopts the same method as Example 1 to prepare polycaprolactone, and similarly The determination of the sample APHA color is carried out. The APHA chromaticity of the sample can be measured as 61. The number average molecular weight measured by GPC was 11042.

[0044]

[0045] The measured APHA chromaticity is 61, second only to PEP-8T. It can be seen that phosphite esters with similar structures can effectively inhibit the yellowing problem in the process of using caprolactone monomers to synthesize polycaprolactone.

Embodiment 3

[0047] Except that the antioxidant is changed to triisodecyl phosphite (from Tisi Ai (Shanghai) Chemical Industry Development Co., Ltd.), polycaprolactone is prepared in the same manner as in Example 1, and the solution APHA chromaticity is also tested in the same way. Determination. The APHA chromaticity of the sample can be measured to be 72. The number average molecular weight measured by GPC was 29719.

[0048]

[0049] Antioxidant triisodecyl phosphite (phosphite without hindered phenol structure)

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Abstract

The invention provides a preparation method of light-colored polycaprolactone, which is characterized by comprising the following steps: in an inert atmosphere, in the presence of a ring-opening catalyst and an antioxidant, a caprolactone monomer is subjected to ring-opening polymerization to prepare polycaprolactone, and the antioxidant is a phosphite antioxidant without a hindered phenol structure. According to the method disclosed by the invention, the problem of yellowing of the polycaprolactone product under the condition of high-temperature polymerization reaction can be solved.

Description

technical field [0001] The invention belongs to the synthetic field of polyester, and in particular relates to a preparation method of light-colored polycaprolactone and polycaprolactone prepared therefrom. Background technique [0002] In recent years, polycaprolactone has better mechanical properties, especially in terms of wear resistance and elastic recovery, and has better weather resistance and heat resistance than polyether polyols. Diacid polyester has better hydrolysis resistance and is widely used in polyurethane elastomers, adhesives, coatings and other fields. [0003] Polycaprolactone is used as an oligomer and a denaturant in the raw materials of polyurethane systems such as elastomers, elastic fibers, latex, and ink adhesives, which can improve toughness, low-temperature characteristics, and reactivity; in terms of resin modification, it can It is used to improve the flexibility, fluidity, low temperature impact resistance, formability, etc. of acrylic, polye...

Claims

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Application Information

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IPC IPC(8): C08G63/08C08G63/78C08K5/524
CPCC08G63/08C08G63/78C08K5/524
Inventor 张立昊陈万滨
Owner DAICEL (CHINA) INVESTMENT CO LTD