Method for catalyzing and synthesizing 1, 2-pentanediol by using titanium silicalite

A technology of titanium silicon molecular sieve and pentanediol, applied in the field of chemical products 1, can solve problems such as uneconomical and unenvironmental protection

Inactive Publication Date: 2011-04-13
YUNNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these synthetic methods all need to consume at least twice the amount of formic acid as a solvent, and consume more than twice the amount of sodium hydroxide to neutralize the saponification products, resulting in a large amount of sodium formate as a by-product, which is not economical nor environmentally friendly.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: Add 400 grams of 30% hydrogen peroxide to 2000 grams of methanol solvent at room temperature, add 40 grams of TS-1 catalyst under stirring, then add 1200 grams of 1-pentene, heat it to 60 ° C in a sealed autoclave, and stir the reaction After 3 hours, the catalyst in the mixture was recovered by filtration, and the solution was rectified in a rectification tower to recover 960 grams of unreacted 1-pentene, and the methanol solvent was completely recovered. The bottom of the rectification tower is a mixture of 1,2-pentanediol and water, and gas chromatography analysis contains a small amount of 1,2-pentanediol and 1,2-pentanediol monomethyl ether, 1,2-pentanediol The selectivity was 96%. The residual amount of hydrogen peroxide in the bottom water of the rectification tower was analyzed by titration, and the conversion rate of hydrogen peroxide was calculated to be 99%. Add the mixed solution of 160 grams of water and 1 gram of sulfuric acid in the aqueous so...

Embodiment 2

[0015] Embodiment 2: Epoxidation catalyst is changed into TS / TiO 2 , Others were the same as in Example 1, finally got 310 grams of 1,2-pentanediol product with a purity of 99%, and a yield of 87% based on consumed 1-pentene.

Embodiment 3

[0016] Embodiment 3: the epoxidation catalyst is changed into Ti-MWW, and the solvent is changed into acetonitrile, and others are with embodiment 1, finally get 1,2-pentanediol product 314 grams of purity is 99%, with the 1-pentene of consumption The calculated yield was 88%.

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PUM

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Abstract

The invention provides a method for catalyzing and synthesizing 1, 2-pentanediol by using titanium silicalite, comprising the following processes of: (1) reacting 1-pentene with oxyful catalyzed and activated by the titanium silicalite in a solvent to obtain 1, 2-epoxy pentane in high selectivity and high yield; and (2) after vaporizing and eliminating the solvent, carrying out the ring cleavage reaction on the 1, 2-epoxy pentane and water in the presence of the action of an acidic or basic catalyst to obtain the 1, 2-pentanediol. The purity of the rectified product is greater than 99 percent.

Description

technical field [0001] The invention relates to a preparation method of chemical product 1,2-pentanediol. In particular, it relates to a preparation method for epoxidizing 1-pentene with titanium-silicon molecular sieve catalysts to catalyze hydrogen peroxide, and then ring-opening to obtain 1,2-pentanediol. Background technique [0002] 1,2-pentanediol is an important chemical product and an essential intermediate for the synthesis of the pesticide propiconazole. Propiconazole is an important fungicide. U.S. Patent No. 4,479,021 proposes to use formic acid and 70% concentration hydrogen peroxide in a continuous reactor to generate performic acid and then react continuously with 1-pentene, recycle excess 1-pentene, neutralize formic acid saponification products with sodium hydroxide at 70 ° C, and use ethyl acetate The synthesis method of extracting the product and then rectifying to obtain 1,2-pentanediol. The method reduces the pentene formic acid ratio of more than 1:1...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/10
Inventor 王洪林
Owner YUNNAN UNIV
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