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Preparation method for methylene diacetate

A technology of methylene diacetate and acetate, which is applied in the field of preparation of methylene diacetate, can solve the problems of high price, achieve the effects of low toxicity, simple process, and meet the requirements of industrial scale-up production

Inactive Publication Date: 2015-06-24
CHANGSHU CHANGJI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are very few reports about methylene diacetate and its preparation method, and at present, only a small amount of synthesis can be carried out in the laboratory, and industrial scale-up production cannot be formed, so the price is very expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 1 mol (85 g) of dichloromethane, 1 mol (98.1 g) of potassium acetate, 85 g of 1,4-dioxane, and 13.4 g of tetrabutylammonium bromide into the reaction flask, and heat up to 50 degrees to react, and the reaction time is 15 hours , to obtain the reaction solution, the reaction solution was centrifugally filtered to obtain the filtrate, the filter residue was washed with 10 g of 1,4-dioxane, the filtrate obtained by centrifugal filtration and the washing solution (also called washing solution) obtained by washing the filter residue were combined, and the Pressure rectification to obtain methylene diacetate with a purity of 99.2% and a yield of 67.2%.

Embodiment 2

[0018] Add 1mol (174g) of dibromomethane, 5mol (1072g) of magnesium acetate, 740g of diethylformamide, 1000g of dimethylformamide, 10g of triphenylethylphosphonium bromide, and 2.7g of 18-crown-6 into the reaction flask , polyoxyethylene polyoxypropylene dialkyl ether PPG-4-ceteth-10 47g, heat up to 110 degrees for reaction, the reaction time is 4h, obtain the reaction solution, the reaction solution is centrifugally filtered to obtain the filtrate, and use acetonitrile 100g of filter residue was washed, the filtrate obtained by centrifugal filtration and the lotion (also called washing liquid) obtained by washing the filter residue were combined, and rectified under reduced pressure to obtain methylene diacetate with a purity of 99.4% and a yield of 69.1%.

Embodiment 3

[0020] Add 1 mol (267.9 g) of diiodomethane, 10 mol (820 g) of sodium acetate, 400 g of dimethyl sulfoxide, 400 g of ethylene glycol diethyl ether, 400 g of hexamethylphosphoric triamide, 140 g of propionitrile, and 15- Crown-5 1.2g, heat up to 160 degrees to react, the reaction time is 10h, the reaction solution is obtained, the reaction solution is centrifugally filtered to obtain the filtrate, the filter residue is washed with 200g of ethylene glycol diethyl ether, the filtrate obtained by centrifugal filtration and the filter residue are washed The obtained washing liquids (also called washing liquids) were combined and rectified under reduced pressure to obtain methylene diacetate with a purity of 99.1% and a yield of 68.4%.

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Abstract

The invention discloses a preparation method for methylene diacetate. The preparation method for methylene diacetate comprises the following steps: adding dihalogenated methane and acetate in a polar solvent so as to react in the presence of a phase transfer catalyst, controlling the reaction temperature and the reaction time to obtain a reaction solution, then filtering the reaction solution, washing the filter residue, then combining the filtrate with the filter residue, and carrying out reduced pressure distillation to obtain methylene diacetate. The raw materials of the used phase transfer catalyst, dihalogenated methane, acetate and a polar solvent are easily available and cheap; the process is concise and the reaction is moderate; because the purity of the obtained methylene diacetate is not less than 99%, and the yield is not less than 67% and the toxicity is low, the preparation method is capable of meeting the requirements of industrial enlarged production; the obtained methylene diacetate is capable of being either used as a methylenation medical intermediate or used as a raw material for synthesising an additive, namely methylene dimethane sulfonate, of a novel lithium-ion battery electrolyte.

Description

technical field [0001] The present invention relates to a kind of preparation method of methylene diacetate. Background technique [0002] Methylene diacetate is a colorless transparent liquid with a CAS number of 628-51-3, a boiling point of 164.5°C, a flash point of 72.6°C and a density of 1.119g / cm 3 , is a kind of important methylation pharmaceutical intermediate, and also a raw material for the synthesis of methylene methylene disulfonate (MMDS). With the emphasis on green and environmentally friendly new energy, lithium-ion power batteries have become a new type of green and environmentally friendly energy that replaces traditional batteries. MMDS is a new type of additive for lithium-ion electrolytes, which can greatly improve the safety performance of lithium-ion batteries. growing demand. However, the synthesis of MMDS is relatively difficult. Japanese Patent JP2005336155A discloses a method for generating methylene methanedisulfonate by reacting methylene diacet...

Claims

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Application Information

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IPC IPC(8): C07C67/11C07C69/16
CPCC07C67/11C07C69/16
Inventor 林晓文艾玉玲傅人俊唐智华
Owner CHANGSHU CHANGJI CHEM
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