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Method for preparing 1,3-dioxolane

A dioxolane and ethylene glycol technology, applied in the direction of organic chemistry, can solve the problems of high requirements for reaction vessels, many by-products, and high corrosiveness, and achieve the effects of environmental friendliness, less impurities and less corrosiveness

Active Publication Date: 2015-01-07
定州旭邦新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional 1,3-dioxolane preparation process uses sulfuric acid as a catalyst, which is highly corrosive and requires high requirements on the reaction vessel; using strong acidic ion exchange resin as a catalyst requires a large amount and many by-products

Method used

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  • Method for preparing 1,3-dioxolane
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  • Method for preparing 1,3-dioxolane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Embodiment 1 (with 1-butyl-3-methylimidazolium bisulfate as catalyst)

[0055] First in the reactor, adding concentration is 99% ethylene glycol (purchased from Tianjin Hongyan Chemical Reagent Factory) 150mL, then adds 19.2g of 1-butyl-3-methylimidazolium bisulfate as a catalyst, through oil The bath heats the above mixture to around 70°C. Then, 180 mL of concentrated formaldehyde (purchased from Shijiazhuang Huadi Chemical Industry and Trade Co., Ltd.) with a concentration of 54.21% and a temperature of 70° C. was added into the reaction kettle (the mass concentration of the catalyst in the raw material mixture was 5.26 wt %). After uniformly mixing the above raw materials and catalyst, adjust the temperature of the oil bath to 120°C, and after 3 hours of total reflux reaction, set the extracted reflux ratio to 3 and continuously extract the 1,3- The concentration of dioxolane is above 80% on average, and the highest concentration is 93.83%. The product yield is 70....

Embodiment 2

[0056] Embodiment 2 (with 1-(4-sulfonic acid group) butyl-3-methylimidazole p-toluenesulfonate as catalyst)

[0057] First, in the reaction kettle, 150 mL of ethylene glycol (purchased from Tianjin Hongyan Chemical Reagent Factory) with a concentration of 95% was added, and then 15.1 g of 1-(4-sulfonic acid) butyl-3-methylimidazole was added. Tosylate is used as a catalyst, and the above mixture is heated to about 70°C through an oil bath. Then, 170 mL of concentrated formaldehyde (purchased from Shijiazhuang Huadi Chemical Industry and Trade Co., Ltd.) with a concentration of 57.08% and a temperature of 70° C. was added into the reaction kettle (the mass concentration of the catalyst in the raw material mixture was 4.34 wt %). After uniformly mixing the above raw materials and catalyst, adjust the temperature of the oil bath to 120°C, and after 2 hours of total reflux reaction, set the reflux ratio in extraction to 2.5, and extract continuously. The average concentration of ...

Embodiment 3

[0058] Embodiment 3 (with 1-(4-sulfonic acid group) butyl-3-methylimidazole triflate as catalyst)

[0059] First, 150 mL of ethylene glycol (purchased from Tianjin Hongyan Chemical Reagent Factory) with a concentration of 99% was added to the reaction kettle, and then 14.7 g of 1-(4-sulfonic acid group) butyl-3-methylimidazole tris Fluoromethanesulfonate was used as a catalyst, and the above mixture was heated to about 70°C through an oil bath. Then, 165mL of concentrated formaldehyde (purchased from Shijiazhuang Huadi Chemical Industry and Trade Co., Ltd.) with a concentration of 60.24% and a temperature of 70°C was added to the reaction kettle (the mass concentration of the catalyst in the raw material mixture was 4.02wt%). After uniformly mixing the above raw materials and catalyst, adjust the oil bath temperature to 120°C, and after 2 hours of total reflux reaction, set the extracted reflux ratio to 2, and continuously extract the 1,3- The average concentration of dioxola...

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Abstract

The invention belongs to the field of chemical synthesis, and particularly relates to a method for preparing 1,3-dioxolane. In the method, ionic liquid is used as a catalyst; and the 1,3-dioxolane is prepared through total reflux reaction of ethanol and concentrated formaldehyde. Compared with the prior art, the method for preparing the 1,3-dioxolane, provided by the invention, has the advantages that: the ionic liquid catalyst adopted by the method provided by the invention is acidic ionic liquid which has stable performance, less using amount, small corrosion and environment friendliness; a product prepared by the method has less impurity and high yield; in the method, the formaldehyde is concentrated, is subjected to temperature preservation at a temperature of 60-90 DEG C and then is directly thrown into a reaction kettle for preparing the 1,3-dioxolane; and thus, the sensible heat loss caused by forming paraformaldehyde from the concentrated formaldehyde at room temperature is avoided, and energy consumption caused by reaction heating can also be favorably reduced.

Description

technical field [0001] The invention belongs to the field of chemical synthesis. In particular, the present invention relates to a process for the preparation of 1,3-dioxolane. Background technique [0002] 1,3-dioxolane is commonly known as DOX. DOX is an excellent organic solvent with a wide range of uses. It is mainly used as a solvent for oil and fat, an extractant, an electrolytic solvent for lithium batteries, a chlorine-based solvent stabilizer, and a drug intermediate. DOX is the second monomer of polyoxymethylene, which is copolymerized with paraformaldehyde at a ratio of 95:5 to produce polyoxymethylene. DOX can also be used as silk finishing agent and sealing glue raw material. [0003] The traditional 1,3-dioxolane preparation process is to prepare the product by reacting paraformaldehyde and ethylene glycol. Paraformaldehyde and ethylene glycol are put into the reactor at a molar ratio of 1:1.25, and a strong acidic ion exchange resin is used as a catalyst, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/12
Inventor 杨雪岗唐旭博张英伟张新志王耀红彭永兴
Owner 定州旭邦新材料科技有限公司
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