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Preparation method of 1,3-dioxolane

A technology of dioxolane and ethylene glycol, applied in the direction of organic chemistry, etc., can solve the problems of large amount of catalyst, high reaction temperature and long reaction time, and achieve the effects of high product purity, low reaction temperature and short reaction time.

Inactive Publication Date: 2017-05-17
NEUFTECH BIOTECH HEFEI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing synthetic methods of 1,3-dioxolane are generally obtained by condensation of ethylene glycol and formaldehyde with strong protic acids such as sulfuric acid and hydrochloric acid or some inorganic salts and metal oxides as catalysts. Disadvantages such as long reaction time, high reaction temperature, low product purity, corrosion to equipment, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] This embodiment prepares 1,3-dioxolane as follows:

[0018] Add 100g of ethylene glycol and 0.37g of N86 ionic liquid catalyst into the reactor, then add 46g of paraformaldehyde, raise the temperature to 60°C, react for 1h, then slowly raise the temperature to 85°C, and keep this temperature for 2h. The obtained product was dried with solid alkali, rectified, and finally 0.2 g of 2,6-di-tert-butyl-p-cresol was added and mixed uniformly to obtain the product 1,3-dioxolane. The obtained product is a colorless transparent liquid with a yield of 89.8%.

Embodiment 2

[0020] This embodiment prepares 1,3-dioxolane as follows:

[0021] Add 100g of ethylene glycol and 0.37g of N86 ionic liquid catalyst into the reactor, then add 46g of paraformaldehyde, raise the temperature to 60°C, react for 1h, then slowly raise the temperature to 90°C, and keep this temperature for 3h. The obtained product was dried with solid alkali, rectified, and finally 0.2 g of 2,6-di-tert-butyl-p-cresol was added and mixed uniformly to obtain the product 1,3-dioxolane. The obtained product is a colorless transparent liquid with a yield of 90.5%.

Embodiment 3

[0023] This embodiment prepares 1,3-dioxolane as follows:

[0024] Add 100g of ethylene glycol and 0.37g of N86 ionic liquid catalyst into the reactor, then add 46g of paraformaldehyde, raise the temperature to 60°C, react for 1h, then slowly raise the temperature to 95°C, and keep this temperature for 4h. The obtained product was dried with solid alkali, rectified, and finally 0.2 g of 2,6-di-tert-butyl-p-cresol was added and mixed uniformly to obtain the product 1,3-dioxolane. The obtained product is a colorless transparent liquid with a yield of 92.1%.

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Abstract

The invention discloses a preparation method of 1,3-dioxolane. The preparation method comprises the steps of carrying out a reaction by taking ethylene glycol and polyformaldehyde as raw materials and adding right amount of N86 type ionic liquid catalyst; drying the obtained product with solid caustic soda, rectifying, adding right amount of antioxidant and evenly mixing to obtain the target product 1,3-dioxolane. The preparation method has the advantages of being less in consumption of the catalyst, short in reaction time, low in reaction temperature, high in product purity, and the like.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of 1,3-dioxolane with bactericidal effect. Background technique [0002] Formaldehyde is a colorless gas with a pungent smell. Because it can react with amino acids in proteins in living organisms, thereby deactivating the proteins, it is often used for sterilization and preservation. However, formaldehyde is a gas at normal temperature, and it is very inconvenient to transport and use. The 1,3-dioxolane produced by the condensation of ethylene glycol and paraformaldehyde is a hemiacetal that is soluble in water and most solvents, so it is particularly convenient and quick to use. [0003] The existing synthetic methods of 1,3-dioxolane are generally obtained by condensation of ethylene glycol and formaldehyde with strong protic acids such as sulfuric acid and hydrochloric acid or some inorganic salts and metal oxides as catalysts. Shortcomings ...

Claims

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Application Information

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IPC IPC(8): C07D317/12
CPCC07D317/12
Inventor 陈路程庆华陆静刘霁余杨柳
Owner NEUFTECH BIOTECH HEFEI
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