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Method for preparing nonoxynol without ethylene oxide

A technology of ethylene oxide and nonoxynol, which is applied in the field of medicine and chemical industry, can solve the problems of ethylene oxide residue in nonoxynol, reduce the content of ethylene oxide, be simple to operate, and facilitate industrial scale-up production Effect

Inactive Publication Date: 2019-04-16
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

Mainly solve the technical problem of ethylene oxide residue in nonoxynol ether obtained by the existing process

Method used

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  • Method for preparing nonoxynol without ethylene oxide
  • Method for preparing nonoxynol without ethylene oxide
  • Method for preparing nonoxynol without ethylene oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add nonylphenol (100g, 0.45mol) and sodium hydroxide (0.25g, 6.25mmol) into the reaction kettle, and replace the air with nitrogen; raise the temperature to 140-160°C. Control the temperature at 140-160°C (keep the temperature at 140-160°C, keep this temperature when feeding ethylene oxide later and during the reaction, the same below), feed ethylene oxide (200g, 4.54mol), Ethylene oxide passing time is about 4 hours. After the introduction, take a sample to detect the cloud point (should be 52-56°C). After the cloud point is qualified, add sodium hydroxide (0.5g, 12.5mmol) and continue the reaction for 0.5h. Stop the reaction, lower the temperature to 65-75°C, and wash with saturated aqueous sodium chloride solution 2-3 times. Vacuum drying at 100°C for 2 hours gave 290 g of a colorless oil. Residual amount of ethylene oxide: not detected.

Embodiment 2

[0041] Add nonylphenol (100g, 0.45mol) and sodium hydroxide (0.25g, 6.25mmol) into the reaction kettle, and replace the air with nitrogen; raise the temperature to 140-160°C. The temperature was controlled at 140-160°C, and ethylene oxide (200 g, 4.54 mol) was passed in for about 4 hours. After the introduction, take a sample to detect the cloud point (should be 52-56°C). After the cloud point is qualified, add sodium hydroxide (0.75g, 18.75mmol) and continue the reaction for 0.5h. Stop the reaction, lower the temperature to 65-75°C, and wash with saturated aqueous sodium chloride solution 2-3 times. Vacuum drying at 100°C for 2 hours gave 288 g of light yellow oil. Residual amount of ethylene oxide: not detected.

Embodiment 3

[0043] Add nonylphenol (100g, 0.45mol) and sodium hydroxide (0.25g, 6.25mmol) into the reaction kettle, and replace the air with nitrogen; raise the temperature to 160-180°C. The temperature is controlled at 160-180°C, and ethylene oxide (200 g, 4.54 mol) is introduced, and the time for introducing ethylene oxide is about 4 hours. After the introduction, take a sample to detect the cloud point (should be 52-56°C). After the cloud point is qualified, add sodium hydroxide (0.75g, 18.75mmol) and continue the reaction for 0.5h. Stop the reaction, lower the temperature to 65-75°C, and wash with saturated aqueous sodium chloride solution 2-3 times. Vacuum drying at 100°C for 2 hours gave 280 g of light yellow oil. Residual amount of ethylene oxide: not detected.

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Abstract

The invention provides a method for preparing nonoxynol without ethylene oxide. The method comprises the following steps that a, nonyl phenol and alkali which are taken as raw materials are added intoa reaction still, and air is replaced with nitrogen; b, the temperature rises, and ethylene oxide is introduced; c, after introducing is finished, a sample is taken for detecting cloud points, afterthe cloud points are qualified, alkali is supplemented, and the reaction continues for some time; d, the reaction stops, and the temperature is reduced; e, a sodium chloride aqueous solution is adopted for washing; f, vacuum drying is conducted; the nonoxynol is shown in the formula I. According to the method, after finishing of the reaction, sodium hydroxide is supplemented, ethylene oxide remaining in reaction liquid can be completely consumed, finally, the obtained nonoxynol crude drug does not contain the ethylene oxide, and the quality of the nonoxynol crude drug is improved. In the reaction process, the content of the ethylene oxide is reduced, the frequency of washing in the after-treatment process can be reduced, discharged waste water is reduced, and the method is green and environmentally friendly. The method is short in reaction steps and simple in operation, industrial scale-up production is convenient, and the nonoxynol without ethylene oxide can be obtained.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a method for preparing nonoxynol without ethylene oxide. Background technique [0002] Nonoxynol (Nonoxinol), also known as nonoxynol-9 or nonylphenol polyether-1, belongs to the alkylbenzene polyoxyethylene nonionic surfactant, and is a safe, safe and widely used in various countries. Reliable topical spermicidal contraceptive. It was first listed in the UK in 1983, and has been included in the Chinese Pharmacopoeia, British Pharmacopoeia, European Pharmacopoeia, and WHO Pharmacopoeia. Its structural formula is shown in the following formula I, wherein the average value of the degree of polymerization is 9. [0003] [0004] As an effective vaginal spermicide, the spermicidal mechanism of nonoxynol is mainly to destroy the biomembrane system of sperm, leading to the rupture of sperm membrane, and the fragmentation and death of sperm. It has the adv...

Claims

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Application Information

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IPC IPC(8): C07C41/03C07C43/23
CPCC07C41/03C07C43/23
Inventor 王举波王卉李志裕
Owner 药大制药有限公司
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