Method for preparing 1,2-pentadiol

A technology of pentanediol and pentene, applied in 1 field, can solve the problems of difficult industrial preparation of catalysts, high engineering equipment requirements, difficult industrialized production, etc., and achieve the effects of being conducive to safe production, reducing costs, and stable properties

Inactive Publication Date: 2011-02-09
SINOCHEM NINGBO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

U.S. Patent No. 4,479,021 discloses a continuous production process for 1,2-pentanediol that uses pentene and formic acid as raw materials and hydrogen peroxide as an oxidant. However, the process is complicated to operate, difficult to control, and requires high engineering equipment; U.S. Patent No. 4,605,795 discloses A method for producing 1,2-pentanediol with pentene and peroxypropionic acid in a benzene solvent, the benzene used in the process is highly toxic and harmful to the human body; Chinese patent CN1226259C discloses A method for producing 1,2-pentanediol using pentene, formic acid and hydrogen peroxide as main raw materials, but a large excess of formic acid needs to be used in this method, the operation is complicated, the cost is high, and a large amount of by-product sodium formate is produced. It is difficult to handle, and the 50% hydrogen peroxide used at the same time is not easy to store, and there are potential safety hazards; Chinese patent CN1923777A discloses a method for catalytically synthesizing 1,2-pentanediol using phosphotungstic heteropolyacid, but the catalyst used in this method is not easy to be industrially prepared , and the reaction requires the use of high-pressure equipment, which is difficult for industrial production

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0021] Add 65kg of 85% formic acid, 70kg of 1-pentene, 1kg of 98% sulfuric acid and 125kg of 30% hydrogen peroxide into the reaction kettle at one time at 0°C, then raise the temperature to 30°C, keep it warm for 3 hours, cool naturally, and add ammonia water dropwise Neutralize, stop when the pH value reaches 8-9, control the temperature not to exceed 30°C, keep warm for 1 hour and then cool to room temperature. Using n-butanol to extract three times, the organic phases were combined and then concentrated under reduced pressure to obtain crude 1,2-pentanediol. Vacuum rectification at 0.1Mpa, collecting fractions at 96°C, yielded 84kg of 1,2-pentanediol with a yield of 81% and a product purity greater than 99%. The inorganic phase is concentrated and then recrystallized to obtain high-purity ammonium formate.

Embodiment 2

[0023] 65kg of 85% formic acid, 70kg of 1-pentene, 3kg of 36% concentrated hydrochloric acid and 125kg of 30% hydrogen peroxide were added to the reactor at one time at 0°C, and other operations were the same as in Example 1. 76kg of 1,2-pentanediol was obtained, the yield was 73%, and the product purity was greater than 99%. The inorganic phase is concentrated and then recrystallized to obtain high-purity ammonium formate.

Embodiment 3

[0025] 65kg of 85% formic acid, 70kg of 1-pentene, 1.8kg of 60% perchloric acid and 125kg of 30% hydrogen peroxide were added to the reactor at one time at 0°C, and other operations were the same as in Example 1. 64kg of 1,2-pentanediol was obtained, the yield was 62%, and the product purity was greater than 99%. The inorganic phase is concentrated and then recrystallized to obtain high-purity ammonium formate.

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Abstract

The invention provides a method for preparing 1,2-pentadiol from 1-amylene serving as a raw material by taking hydrogen peroxide serving as an oxidant, a strong acid serving as a catalyst, and formic acid serving as a solvent. The technology for preparing 1,2-pentadiol is easy and convenient to operate, has low cost, avoids the generation of a by-product sodium formate and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing 1,2-pentanediol, in particular to a method for preparing 1,2-pentanediol by reacting 1-pentene with hydrogen peroxide. Background technique [0002] 1,2-pentanediol is an intermediate in the production of various chemical products, and is also the main raw material for the fungicide propiconazole. Propiconazole is a high-efficiency triazole fungicide. U.S. Patent No. 4,479,021 discloses a continuous production process for 1,2-pentanediol that uses pentene and formic acid as raw materials and hydrogen peroxide as an oxidant. However, the process is complicated to operate, difficult to control, and requires high engineering equipment; U.S. Patent No. 4,605,795 discloses A method for producing 1,2-pentanediol with pentene and peroxypropionic acid in a benzene solvent, the benzene used in the process is highly toxic and harmful to the human body; Chinese patent CN1226259C discloses A method for producing 1,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/03
Inventor 钟铮金甘秋刘欣一
Owner SINOCHEM NINGBO CHEM
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