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The preparation method of ethylene glycol hemiformal

A technology of hemiformal and ethylene glycol, which is applied in the field of preparation of ethylene glycol hemiformal, can solve the problems of low primary conversion rate and high content of impurity ethylene glycol diformal, and achieve fast reaction speed and high product purity , the effect of high conversion rate

Active Publication Date: 2016-12-07
NANTONG JIANGTIAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

However, the existing methods often have the disadvantages of low primary conversion rate and high content of impurity ethylene glycol diformal in the product.

Method used

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  • The preparation method of ethylene glycol hemiformal

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Add 62g of ethylene glycol and 1.05g of trimethylchlorosilane into a stainless steel autoclave, then feed 29g of formaldehyde, raise the temperature to 40°C for 1 hour, then slowly raise the temperature to 160°C within 5 hours, and keep it warm for 2 hours. After cooling, it was transferred to a vacuum distillation device, and the product ethylene glycol hemiformal was distilled under reduced pressure at 2-3 Torr, 66.5 g, and the yield was 91%.

Embodiment 2

[0019] Add 62g of ethylene glycol and 3.5g of trimethylchlorosilane into a stainless steel autoclave, then add 30g of paraformaldehyde, raise the temperature to 80°C for 1 hour, then slowly raise the temperature to 180°C within 5 hours, and keep it warm for 4 hours , cooled, and then transferred to a vacuum distillation device, and the product ethylene glycol hemiformal was evaporated under reduced pressure at 2 to 3 Torr, 65g, and the yield was 89%.

Embodiment 3

[0021] Add 62g of ethylene glycol and 3.5g of trimethylchlorosilane into a stainless steel autoclave, then add 30g of paraformaldehyde and 0.1mL of triethylamine, raise the temperature to 80°C for 1 hour, then slowly raise the temperature to 180°C within 5 hours , after heat preservation reaction for 2 hours, cooled, then transferred to a vacuum distillation device, and the product ethylene glycol hemiformal was distilled under reduced pressure at 2-3 Torr, 6.8g, yield 93.1%.

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Abstract

The invention discloses a preparation method of ethylene glycol hemiformal with bactericidal activity, which is obtained by condensing ethylene glycol with formaldehyde or paraformaldehyde under the catalysis of trimethylchlorosilane. The invention has the advantages of high single conversion rate, fast reaction speed, high product purity and the like.

Description

technical field [0001] The invention belongs to the field of bactericides, and in particular relates to a preparation method of ethylene glycol hemiformal with bactericidal activity. Background technique [0002] Formaldehyde, colorless, pungent smell, soluble in water. Since the amino acid residues on proteins of organisms (especially bacteria) can react with formaldehyde, formaldehyde is often used for sterilization. The 35% to 40% formaldehyde solution is commonly known as formalin, which is often used to soak biological specimens because of its bactericidal effect. [0003] However, since formaldehyde is a gas at room temperature and has a strong odor, it is not suitable for use as a long-term fungicide. Ethylene glycol hemiformal is a hemiacetal formed from formaldehyde, which can release formaldehyde through slow hydrolysis, thus playing a long-term bactericidal effect. Moreover, since ethylene glycol hemiformal has good solubility in water and most organic solvents...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/56C07C43/30
CPCC07C41/56C07C43/30
Inventor 黄耀辉
Owner NANTONG JIANGTIAN CHEM CO LTD
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