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Preparation method of octylbenzene polyol

A technology of octoxynated polyol and p-tert-octylphenol, which is applied in the field of preparation of octoxynated polyol, can solve the problems of adverse effects on the production of octoxynated polyol, low concentration of action, low cytotoxicity, and the like, and achieves reduced generation, Yield-enhancing, easy-to-reproduce effects

Pending Publication Date: 2020-12-22
药大制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The mechanism of Octoxynol-9’s spermicidal action is to dissolve and destroy the sperm plasma membrane and acrosomal membrane, denature the membrane-bound protein and make the sperm lose vitality so as to achieve the contraceptive effect. It has a rapid effect, low concentration and good effect. And cytotoxicity is little, non-fertility toxicity, is a kind of excellent contraceptive substance, and sodium hydroxide is generally used as catalyst in the preparation of octoxynol, and its ethoxy adduct that its reaction generates is wider in distribution, and productive rate is higher Low
In addition, p-tert-octylphenol, the raw material for the synthesis of octoxynol, will have a certain amount of ortho products in the conventional preparation process, which will adversely affect the subsequent production of octoxynol

Method used

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  • Preparation method of octylbenzene polyol
  • Preparation method of octylbenzene polyol
  • Preparation method of octylbenzene polyol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) 1 mol of phenol and 1.2 mol of dimeric isobutylene were respectively exchanged through ion exchange columns equipped with 001x7 cation exchange resins, and passed into a reactor equipped with 001x7 cation exchange resins, and reacted at 90 ° C under normal pressure;

[0027] (2) Then the reactant is passed into a thin film evaporator, evaporated and purified under 140°C vacuum condition, and then passed into a rectification tower, the temperature at the bottom of the tower is 175°C, the temperature at the top of the tower is 125°C, and the high vacuum environment is obtained. p-Toctylphenol;

[0028] (3) Place the obtained p-tetylphenol in the reaction kettle replaced by nitrogen and add 0.014mol of strontium hydroxide, when the temperature is raised to 145°C, ethylene oxide is introduced, and the temperature is continued to be raised to 160°C, and the reaction is carried out until The cloud point is 65°C as the reaction end point, and the crude product is obtained;...

Embodiment 2

[0031] (1) 1 mol of phenol and 1.1 mol of dimeric isobutylene were respectively exchanged through ion exchange columns equipped with 001x7 cation exchange resin, and then passed into a reactor equipped with 001x7 cation exchange resin, and reacted at 90 ° C under normal pressure;

[0032] (2) Then the reactant is passed into a thin film evaporator, evaporated and purified under 140°C vacuum condition, and then passed into a rectification tower, the temperature at the bottom of the tower is 175°C, the temperature at the top of the tower is 125°C, and the high vacuum environment is obtained. p-Toctylphenol;

[0033] (3) Place the obtained p-tetylphenol in the reaction kettle replaced by nitrogen and add 0.014mol of strontium hydroxide, when the temperature is raised to 145°C, ethylene oxide is introduced, and the temperature is continued to be raised to 160°C, and the reaction is carried out until The cloud point is 65°C as the reaction end point, and the crude product is obtain...

Embodiment 3

[0036] (1) 1 mol of phenol and 1.3 mol of dimeric isobutylene were respectively exchanged through ion exchange columns equipped with 001x7 cation exchange resins, then passed into a reactor equipped with 001x7 cation exchange resins, and reacted at 90 ° C under normal pressure;

[0037] (2) Then the reactant is passed into a thin film evaporator, evaporated and purified under 140°C vacuum condition, and then passed into a rectification tower, the temperature at the bottom of the tower is 175°C, the temperature at the top of the tower is 125°C, and the high vacuum environment is obtained. p-Toctylphenol;

[0038] (3) Place the obtained p-tetylphenol in the reaction kettle replaced by nitrogen and add 0.014mol of strontium hydroxide, when the temperature is raised to 145°C, ethylene oxide is introduced, and the temperature is continued to be raised to 160°C, and the reaction is carried out until The cloud point is 65°C as the reaction end point, and the crude product is obtained...

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Abstract

The invention belongs to the field of chemical synthesis, and particularly relates to a preparation method of octylbenzene polyol and a preparation method of p-tert-octylphenol serving as a productionraw material of octylbenzene polyol. The preparation method disclosed by the invention is simple, the yield of the raw material preparation of the octylbenzene polyalcohol and the preparation processof the octylbenzene polyalcohol are improved, the production cost is saved from the beginning of the production of upstream raw materials, and the overall production efficiency is higher.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and in particular relates to a preparation method of octoxynol. Background technique [0002] The mechanism of Octoxynol-9’s spermicidal action is to dissolve and destroy the sperm plasma membrane and acrosomal membrane, denature the membrane-bound protein and make the sperm lose vitality so as to achieve the contraceptive effect. It has a rapid effect, low concentration and good effect. And cytotoxicity is little, non-fertility toxicity, is a kind of excellent contraceptive substance, and sodium hydroxide is generally used as catalyst in the preparation of octoxynol, and its ethoxy adduct that its reaction generates is wider in distribution, and productive rate is higher Low. In addition, p-tert-octylphenol, the raw material for synthesizing octoxynol, will have a certain amount of ortho products in the conventional preparation process, which will adversely affect the subsequent produc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/23C07C41/03C07C39/06C07C37/14
CPCC07C41/03C07C37/14C07C43/23C07C39/06
Inventor 郝静梅
Owner 药大制药有限公司