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Method for preparing 1, 2-pentanediol from n-butanol as raw material

A process method and n-butanol technology, applied in the field of preparing 1,2-pentanediol, can solve the problems of flammable and explosive raw materials, corrosion of formaldehyde environment, pollution, etc., and achieve simple post-processing, simple operation and short time. Effect

Inactive Publication Date: 2017-10-20
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the deficiencies in the prior art, to provide a kind of processing method using n-butanol as raw material to prepare 1,2-pentanediol, to solve the inflammable and explosive problem of n-pentene epoxy method in the prior art And the problem of expensive raw materials, and technical problems such as strong acid corrosion and formaldehyde environmental pollution using n-butanol as raw material

Method used

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  • Method for preparing 1, 2-pentanediol from n-butanol as raw material
  • Method for preparing 1, 2-pentanediol from n-butanol as raw material
  • Method for preparing 1, 2-pentanediol from n-butanol as raw material

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Effect test

Embodiment 1

[0019] The synthetic technique of the present invention is as follows:

[0020]

[0021] In the first step, n-butanol is oxidized to prepare n-butyraldehyde

[0022] Its specific synthesis method is: n-butanol is oxidized to prepare n-butyraldehyde: add 0.1mol n-butanol (7.4g), 1mmol TEMPO (0.16g), 34ml dichloromethane, 0.01mol KBr (1.19g) into a 250ml three-necked flask respectively Add it into a three-necked flask after adding 5ml of water, then place it in an ice-water bath at -8°C, and add 0.11mol of sodium hypochlorite aqueous solution (the pH of the sodium hypochlorite solution is 9.5) dropwise with a constant pressure dropping funnel. ℃-30℃, reaction time 5-60min, wash with water, stand to separate the liquid, and remove the solvent under reduced pressure to obtain n-butyraldehyde.

[0023] Using the same conditions as the above-mentioned oxidation method, the difference is that different oxidants are used, and the yield of the product is shown in Table 1.

[0024]...

Embodiment 2

[0027] The second step, the preparation of 1,2-epoxypentane

[0028] Add 0.25 mol of n-butyraldehyde, 0.38 mol of methyl sulfide ylide, potassium carbonate (0.75 mol), and then add 3 mL of dry isopropanol, 0.3 mL of ethanol, and react at room temperature for 12 hours, then add 3 mL of water into a nitrogen-protected reaction flask. Quench the reaction, let stand for liquid separation, dry over anhydrous sodium sulfate, and filter to obtain 1,2-epoxypentane.

[0029] Using the same conditions as the above-mentioned ylide reaction, the difference is that different ylide reagents are used, and the yield of the product is shown in Table 2.

[0030] Table 2

[0031]

Embodiment 3

[0033] The third step, the preparation of 1,2-pentanediol

[0034] Add 5g of potassium hydroxide into 50g of 85% methanol aqueous solution, stir evenly, and heat to reflux, add the separated 1,2-epoxypentane dropwise to the methanol aqueous solution containing a small amount of potassium hydroxide to open the ring, and keep the aqueous solution The pH value is 8, and the 1,2-pentanediol is obtained by static separation.

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Abstract

The invention discloses a method for preparing 1, 2-pentanediol from n-butanol as a raw material. The method comprises that 1) n-butanol as a raw material undergoes a catalytic oxidation reaction to produce n-butyraldehyde, 2) a ylide reagent is added into the n-butyraldehyde under alkaline conditions and the mixture undergoes a ylide reaction to produce 1, 2-cyclopentene oxide, and 3) the 1, 2-cyclopentene oxide is hydrolyzed into a desired product 1, 2-pentanediol. Compared with the prior art, the method utilizes cheap and easily available n-butanol having a sufficient source as a raw material, simplifies the process for synthesizing and separating to purify 1, 2-pentanediol, improves the reaction conversion rate and the purity of the product and greatly reduces reaction time and cost. Compared with the process using n-pentene as a raw material, the method greatly reduces a production cost, can be carried out under mild and reliable production conditions, is stable and safe and solves the problem that the existing device is easily corroded by a strong acid and formaldehyde pollutes the environment.

Description

technical field [0001] The invention relates to a synthesis process of a fine chemical intermediate, in particular to a process for preparing 1,2-pentanediol from n-butanol. Background technique [0002] 1,2-Pentanediol is a straight-chain diol, which is a colorless to light yellow transparent liquid at room temperature. It has obvious polarity and non-polarity, which makes it have different properties from other diols, which is important Chemical raw materials. 1,2-Pentanediol is not only used as the intermediate of fungicide propiconazole and cosmetic formula, but also an important raw material for the production of polyester fibers, surfactants, pharmaceuticals and other products, and has very broad application prospects. [0003] US Patent (US4479021) reports a method for preparing 1,2-pentanediol from olefins, formic acid and hydrogen peroxide, with a yield of 70%. However, there are many by-products of 1,2-pentanediol prepared by this method, the product separation i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/10C07C31/20
CPCC07C29/106C07C45/29C07C45/298C07D301/02C07D303/04C07C31/20C07C47/02
Inventor 秦伟石旵东王钧伟郑学根张元广黄劲松高迎春余世金崔晓峰吴秀银
Owner CHINA PETROLEUM & CHEM CORP
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