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Method used for preparing 1,4-dioxane from 1,3-dioxolane

A kind of technology of dioxane and dioxane, applied in the field of preparation 1

Inactive Publication Date: 2014-07-02
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Recently, when we studied the carbonylation of 1,3-dioxane, we found that under gas-solid phase conditions, solid acid can efficiently catalyze 1,3-dioxane to produce 1,4-dioxane, as shown in the formula As shown in (1), this reaction has never been reported

Method used

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  • Method used for preparing 1,4-dioxane from 1,3-dioxolane
  • Method used for preparing 1,4-dioxane from 1,3-dioxolane
  • Method used for preparing 1,4-dioxane from 1,3-dioxolane

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Experimental program
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Effect test

Embodiment 1

[0019] The 40-60 mesh catalyst obtained by pressing H-β (Si / Al=25) molecular sieve powder into tablets, crushing and sieving. Put 0.6g of catalyst into a reactor with an inner diameter of 8mm, raise the temperature to 500°C in a nitrogen atmosphere, keep the temperature at this temperature for 1h, and then cool down naturally to the reaction temperature of 130°C. Use the carrier gas CO to carry 1,3-dioxane into the reaction tube, the partial pressure of 1,3-dioxane is 42KPa (calculated by Clausius-Clapeyron), and the volume space velocity of CO is 2120h -1 , the reaction was carried out under normal pressure. The reactants were analyzed by online chromatography, the conversion rate of 1,3-dioxane was 64.3%, and the selectivity of 1,4-dioxane was 91.2%.

Embodiment 2

[0021] Other conditions were the same as in Example 1, and the catalytic performance of different solid acid catalysts to generate 1,4-dioxane from 1,3-dioxapenta was evaluated, and the reaction effluent was analyzed by online chromatography. The results are shown in Table 1.

[0022] Table 1

[0023] solid acid

Embodiment 3

[0025] Respectively at 120°C, 140°C, and 160°C, other conditions were the same as in Example 1, and the influence of temperature on the disproportionation of 1,3-dioxane to generate 1,4-dioxane was investigated, and the reaction effluent was obtained by online chromatography analyze. The results are shown in Table 2.

[0026] Table 2

[0027] temperature(℃)

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Abstract

The invention provides a method used for preparing 1,4-dioxane from 1,3-dioxolane. According to the method, raw material gas containing 1,3-dioxolane and carrier gas is delivered into a reactor filled with a solid acid catalyst, and reaction is carried out at a reaction temperature of 120 to 160 DEG C, under a reaction pressure of 0.1 to 2.0MPa, and with gaseous hourly space velocity of 500 to 4500 / h so as to obtain 1,4-dioxane, wherein partial pressure ratio of the carrier gas to 1,3-dioxolane in the raw material gas ranges from 1.0 to 50. The method is capable of realizing production of 1,4-dioxane under gas-solid reaction conditions; reaction conditions are mild; and separation of products from the catalyst is simple.

Description

technical field [0001] The invention relates to a method for preparing 1,4-dioxane by catalyzing 1,3-dioxane under gas-solid phase conditions. Background technique [0002] 1,4-Dioxane is an aprotic solvent with excellent solubility, suitable volatility and strong penetration ability, and is miscible with water and many organic solvents. It is often used as a solvent in industrial production , is widely used. The traditional production method uses concentrated sulfuric acid or phosphoric acid as a catalyst and dehydration with ethylene glycol or diethylene glycol. This method not only has many side reactions, is difficult to separate, and has a low product yield, but also uses inorganic acids as catalysts, causing severe equipment corrosion and polluting the environment. Researchers have therefore been working for a long time to develop an environmentally friendly process for the production of 1,4-dioxane. [0003] German Offenlegungschrifen in [2,430,350 and 2,300,990] d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/12
CPCC07D319/12
Inventor 刘世平朱文良刘红超刘勇刘中民孟霜鹤倪友明李利娜周慧
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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