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Novel production process of liquid hindered phenol antioxidant 1135

A technology of hindered phenols and antioxidants, applied in the field of preparation of liquid antioxidants, can solve the problems of long reaction process time, small output of antioxidant 246, adverse environmental effects and the like

Pending Publication Date: 2021-07-06
南京晶典抗氧化技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example: U.S. Patents US3330859 and US5892097 both use organotin as a catalyst, 3,5-methyl ester and isooctyl alcohol for transesterification reaction, the reaction is easy to carry out, but the tin catalyst is not easy to remove, which has adverse effects on the environment
[0004] U.S. Patent US5481023 provides a catalyst with aluminum isopropoxide, 3,5-methyl ester and isooctyl alcohol carry out transesterification reaction to obtain 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionic acid The preparation method of isooctyl ester, although this method adopts non-tin catalyst, needs pickling, water washing in the aftertreatment process, produces a large amount of waste water, is unfavorable for protecting the environment
[0005] Chinese patent CN10

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0026] Example 1:

[0027] A new production process of liquid hindered phenolic antioxidant 1135, the operation steps are as follows:

[0028] Add 116.96 g (0.4 mol) of methyl 3,5-di-tert-butyl-4-hydroxyphenylpropionate, 78.14 g of isooctyl alcohol into a 500 mL four-neck flask equipped with mechanical stirring, a thermometer, a distillation condenser, and a nitrogen inlet. g (0.6mol), HND-6 0.585g, nitrogen purging, vacuum degree -0.04MPa, gradually raise the temperature to 100°C, react for 1h, methanol distills out during the reaction, after the reaction, the temperature rises to 120°C, Adjust the vacuum degree to -0.1MPa, distill for 0.5h, distill out unreacted isooctyl alcohol, cool down to 80°C after completion, filter and remove the catalyst to obtain 153.15g of transparent water sample, which is the product. The yield of isooctyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate obtained in this example was 98.05%, and the product purity was 99.40%.

Example Embodiment

[0029] Example 2:

[0030] A new production process of liquid hindered phenolic antioxidant 1135, the operation steps are as follows:

[0031] Add 116.96 g (0.4 mol) of methyl 3,5-di-tert-butyl-4-hydroxyphenylpropionate, 72.85 g of isooctyl alcohol into a 500 mL four-necked flask equipped with mechanical stirring, a thermometer, a distillation condenser, and nitrogen inlet. g (0.56mol), HND-8 0.585g, nitrogen purging, vacuum degree -0.03MPa, gradually raise the temperature to 110°C, react for 1h, methanol distills out during the reaction, after the reaction, the temperature rises to 130°C, Adjust the vacuum to -0.09MPa, distill for 0.5h to remove unreacted isooctyl alcohol, cool down to 80°C after the end, filter and remove the catalyst to obtain 152.18g of transparent water sample, which is the product. The yield of isooctyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate obtained in this example was 97.43%, and the product purity was 99.35%.

Example Embodiment

[0032] Example 3:

[0033] A new production process of liquid hindered phenolic antioxidant 1135, the operation steps are as follows:

[0034] Add 116.96 g (0.4 mol) of methyl 3,5-di-tert-butyl-4-hydroxyphenylpropionate, 78.14 g of isooctyl alcohol into a 500 mL four-neck flask equipped with mechanical stirring, a thermometer, a distillation condenser, and a nitrogen inlet. g (0.6mol), CP002 0.585g, nitrogen purging, vacuum degree -0.02MPa, gradually raise the temperature to 120°C, react for 1h, methanol distills out during the reaction, after the reaction, the temperature rises to 140°C, vacuum degree Adjust it to -0.08MPa, distill for 0.5h, distill out the unreacted isooctyl alcohol, cool down to 90°C after the end, filter and remove the catalyst to obtain 153.29g of transparent water sample, which is the product. The yield of isooctyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate obtained in this example was 98.14%, and the product purity was 99.27%.

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PUM

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Abstract

The invention discloses a novel production process of a liquid hindered phenol antioxidant 1135. The production process comprises the following steps: S1, putting a certain amount of methyl 3, 5-di-tert-butyl-4-hydroxyphenyl propionate, isooctanol and a catalyst into a reactor, purging with nitrogen, opening vacuum, and heating for catalytic reaction; S2, heating the reactor after the reaction is finished, increasing the vacuum degree, distilling to remove unreacted isooctanol, and applying the unreacted isooctanol to the step S1; and S3, cooling the reactor without isooctanol to 80-90 DEG C, and filtering to obtain a filtrate which is the target product. A solid acid is used as the catalyst, so the technological process is simple; and the solid acid can be recycled, so pollution is small, and the method is safe and environmentally friendly. According to the invention, the production time is compressed to 2 hours, so that the production time is greatly shortened, the energy consumption is saved, and the production cost is reduced. The highest temperature does not exceed 140 DEG C, so that the hidden danger risk caused by the traditional high process temperature is reduced, and the production safety is ensured.

Description

technical field [0001] The invention relates to a preparation method of a liquid antioxidant, in particular to a new production process of a liquid hindered phenolic antioxidant 1135. Background technique [0002] Liquid hindered phenolic antioxidant 1135 (3-(3,5-di-tert-butyl-4-hydroxyphenyl) isooctyl propionate) is an antioxidant with excellent performance widely used in various polymers, especially It has a unique function in the oxidation resistance of polyurethane and its polymeric polyols in the automotive industry and lubricant antioxidants. Therefore, liquid antioxidant 1135 is a new type of high-efficiency liquid antioxidant that cannot be replaced by powder antioxidants. Its development and development is important. [0003] At present, there are many preparation methods of isooctyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate. For example, U.S. Patents US3330859 and US5892097 both use organotin as a catalyst to carry out transesterification of 3,5-methyl este...

Claims

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Application Information

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IPC IPC(8): C07C67/03C07C67/54C07C69/732
CPCC07C67/03C07C67/54
Inventor 何金义陈福新杨香莲戴杰辛璇
Owner 南京晶典抗氧化技术研究院有限公司
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