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Method for synthesizing 1,2-pentanediol from n-butyl alcohol

A technology of pentanediol and n-butanol, which is applied in the field of synthesis of fine chemical intermediates, to achieve the effects of safe production process, simplified separation procedure and increased yield

Inactive Publication Date: 2010-10-13
王永军 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Formula C is a synthetic reaction process:

Method used

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  • Method for synthesizing 1,2-pentanediol from n-butyl alcohol
  • Method for synthesizing 1,2-pentanediol from n-butyl alcohol
  • Method for synthesizing 1,2-pentanediol from n-butyl alcohol

Examples

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Embodiment 1

[0019] In a 1000ml three-necked flask, add 120g of diisopropyl sulfide (1mol) and 150g of n-butanol, after heating to 80-100 degrees, slowly add 120g of 85% sulfuric acid dropwise, and keep it at 100-120 degrees for 3~ After 4 hours, the layers were separated after resting to obtain 265 g of the sulfenyl salt solution in the lower layer. Mix sulfenyl salt solution with 160 g of 37% formaldehyde solution, add dropwise 40% liquid caustic soda NaOH until the pH is greater than 13, react at 30-40 degrees for 3-4 hours, and obtain a light yellow oil layer, which is 1,2-epoxypentyl A mixture of alkanes and diisopropyl sulfide.

[0020] Add 5g of barium hydroxide to 600g of 85%wt methanol aqueous solution, stir evenly, and heat to reflux, then slowly add the above oil layer mixture dropwise, after the dropwise addition, continue to reflux for 2h, then dropwise add 20%wt of sulfuric acid to neutralize to pH = 7.0, the barium sulfate precipitate was removed by filtration to obtain a s...

Embodiment 2

[0022] In a 1000ml three-neck flask with a condensing reflux tube, add 62g dimethyl sulfide (1mol) and 150g n-butanol, after heating to reflux, slowly add 120g of 85% sulfuric acid dropwise, keep the reflux reaction for 3-4h, after standing still The layers were separated to obtain 168 g of the lower layer sulfur salt solution. Mix sulfenyl salt solution with 100 g of 37% formaldehyde solution, add dropwise 40% liquid caustic soda NaOH until the pH is greater than 13, react at 30-40 degrees for 3-4 hours, and obtain a light yellow oil layer, which is 1,2-epoxypentyl A mixture of alkanes and dimethyl sulfide.

[0023] Add 5g of barium hydroxide to 600g of 85%wt methanol aqueous solution, stir evenly, and heat to reflux, then slowly add the above oil layer mixture dropwise, after the dropwise addition, continue to reflux for 2h, then dropwise add 20%wt of sulfuric acid to neutralize to pH = 7.0, the barium sulfate precipitate was removed by filtration to obtain a salt-free 1,2-...

Embodiment 3

[0025] In a 1000ml three-necked flask with a condensing reflux tube, add 150g of dibutyl sulfide (1mol) and 150g of n-butanol. After heating and keeping at 80-100 degrees, slowly add 120g of 85% sulfuric acid dropwise, and keep the reflux reaction for 3 After ~4h, the layers were separated after resting to obtain 352g of the lower layer of sulfuric acid salt solution. Mix sulfenyl salt solution with 100 g of 37% formaldehyde solution, add dropwise 40% liquid caustic soda NaOH until the pH is greater than 13, react at 30-40 degrees for 3-4 hours, and obtain a light yellow oil layer, which is 1,2-epoxypentyl A mixture of alkanes and dibutyl sulfide.

[0026] Add 5g of barium hydroxide to 600g of 85%wt methanol aqueous solution, stir evenly, and heat to reflux, then slowly add the above oil layer mixture dropwise, after the dropwise addition, continue to reflux for 2h, then dropwise add 20%wt of sulfuric acid to neutralize to pH = 7.0, the barium sulfate precipitate was removed ...

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Abstract

The invention discloses a low-cost synthesis process for synthesizing 1,2-pentanediol from n-butyl alcohol. The method comprises the following steps of: synthesizing butyl sulfosalt from n-butyl alcohol and thioether in the presence of the catalysis of strong acid by adopting the n-butyl alcohol as a starting raw material; then reacting the butyl sulfosalt with methanal to obtain 1,2-epoxy pentane; and carrying out ring opening in the presence of the catalysis of barium hydroxide to obtain the 1,2-pentanediol. Compared with a process using n-amylene as a raw material, the method greatly reduces the production cost, has moderate and reliable production condition and is quite stable and safe.

Description

Technical field: [0001] The invention relates to a method for synthesizing fine chemical intermediates, in particular to synthesizing 1,2-pentanediol with cheap n-butanol. technical background: [0002] 1,2-pentanediol is a fine chemical with a wide range of uses, and it is also a key raw material for the pesticide propiconazole. Chinese patent CN03128893 discloses that with n-pentene, formic acid and hydrogen peroxide as raw materials, at low temperature, formic acid and hydrogen peroxide react with a certain molar ratio to produce peroxyformic acid, and n-pentene is generated under the action of strong oxidant peroxyformic acid 1,2-Epoxypentane, then hydrolyzed under basic conditions to give 1,2-pentanediol. Due to the absence of a large amount of cheap n-pentene production and supply in China, the imported expensive n-pentene leads to high production costs; and the boiling point and flash point of n-pentene are too low, which is a highly flammable and explosive chemical,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/10
Inventor 王永军赖维贞
Owner 王永军
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