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Method for separating neopentyl glycol from DL-pantoic acid lactone synthesis feed liquid

A technology of pantolactone and neopentyl glycol, which is applied in the field of separation of neopentyl glycol, can solve problems such as removal by chemical methods, and achieve high-purity results

Active Publication Date: 2022-05-13
安徽泰格生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the chemical properties of neopentyl glycol are relatively stable, and it is difficult to remove them by chemical methods. Therefore, it is necessary to study the method for separating neopentyl glycol suitable for industrial applications.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] This embodiment provides a method for separating neopentyl glycol from DL-pantolactone synthesis feed liquid, comprising the following steps:

[0036] (1) add formaldehyde aqueous solution 860g (formaldehyde content 35wt%), anhydrous sodium carbonate 30g in the reactor, drip isobutyraldehyde 720g (isobutyraldehyde content 99wt%) under the condition of heat preservation 40 ℃, dropwise after finishing , heat preservation reaction 4h, generate hydroxy pivalaldehyde;

[0037] (2) The reaction solution obtained in step (1) is cooled to 5° C., and 10 mol (224 L) of hydrocyanic acid gas is passed into it, and the reaction generates hydroxypivalonitrile;

[0038] (3) Adjust the pH of the reaction solution obtained in step (2) to 1 with concentrated sulfuric acid, heat up to 90° C. for reflux reaction for 2 hours, and generate DL-pantolactone;

[0039] (4) The reaction solution obtained in step (3) is cooled to normal temperature, and the pH is adjusted to neutrality with 30% s...

Embodiment 2

[0042] This embodiment provides a method for separating neopentyl glycol from DL-pantolactone synthesis feed liquid, comprising the following steps:

[0043] (1) Add 860g of formaldehyde aqueous solution (35wt% of formaldehyde content) in the reactor, anhydrous sodium carbonate 30g, dropwise isobutyraldehyde 720g (99wt% of isobutyraldehyde content) under the condition of heat preservation 45 ℃, dropwise after finishing , heat preservation reaction 5h, generate hydroxy pivalaldehyde;

[0044] (2) The reaction solution obtained in step (1) is cooled to 10° C., and 10 mol (224 L) of hydrocyanic acid gas is passed into it, and the reaction generates hydroxypivalonitrile;

[0045] (3) Adjust the pH of the reaction solution obtained in step (2) to 2 with concentrated sulfuric acid, heat up to 85° C. for reflux reaction for 4 hours, and generate DL-pantolactone;

[0046] (4) The reaction solution obtained in step (3) is cooled to normal temperature, and the pH is adjusted to neutral...

Embodiment 3

[0049] This embodiment provides a method for separating neopentyl glycol from DL-pantolactone synthesis feed liquid, comprising the following steps:

[0050] (1) Add 860g of formaldehyde aqueous solution (35wt% of formaldehyde content) in the reactor, anhydrous sodium carbonate 30g, drip isobutyraldehyde 720g (99wt% of isobutyraldehyde content) under the condition of heat preservation 43 ℃, dropwise after finishing , heat preservation reaction 4.5h, generate hydroxy pivalaldehyde;

[0051] (2) The reaction solution obtained in step (1) is cooled to 8° C., and 10 mol (224 L) of hydrocyanic acid gas is passed into it, and the reaction generates hydroxypivalonitrile;

[0052] (3) Adjust the pH of the reaction solution obtained in step (2) to 1.5 with concentrated sulfuric acid, heat up to 88° C. for reflux reaction for 3 hours, and generate DL-pantolactone;

[0053] (4) The reaction solution obtained in step (3) is cooled to normal temperature, and the pH is adjusted to neutrali...

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PUM

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Abstract

The invention provides a method for separating neopentyl glycol from a DL-pantoic acid lactone synthesis feed liquid. The method comprises the steps that the DL-pantoic acid lactone synthetic feed liquid is dewatered and then added into a rectifying tower to be rectified, the rectifying tower sequentially comprises a tower bottom, a tower lower part, a tower middle part and a tower top from bottom to top, the temperature of the tower bottom is controlled to range from 170 DEG C to 175 DEG C, the temperature of the tower lower part is controlled to range from 160 DEG C to 165 DEG C, the temperature of the tower middle part is controlled to range from 145 DEG C to 150 DEG C, and the temperature of the tower top is controlled to range from 115 DEG C to 120 DEG C; the vacuum pressure in the rectifying tower is-0.093 to-0.099 MPa, and collecting neopentyl glycol from the top of the tower. The method provided by the invention has a relatively high removal rate on the neopentyl glycol in the DL-pantoic acid lactone synthesis feed liquid, and the separated neopentyl glycol has relatively high purity.

Description

technical field [0001] The invention belongs to the technical field of chemical production, and in particular relates to a method for separating neopentyl glycol from DL-pantolactone synthesis feed liquid. Background technique [0002] As an important chemical intermediate, DL-pantolactone is an important raw material for the synthesis of calcium pantothenate and panthenol, and it plays an important role in feed, cosmetics and medicine. [0003] According to relevant literature reports, adopting the existing technology to produce DL-pantolactone, one of the important by-products, neopentyl glycol, cannot be avoided, and the output of neopentyl glycol as a by-product is relatively large, accounting for 3% of the total system. -5%. [0004] Neopentyl glycol (NPG) is a white crystalline solid, odorless, hygroscopic, mainly used in the production of unsaturated resins, oil-free alkyd resins, polyurethane foams and elastomer plasticizers, surfactants, Insulating materials, prin...

Claims

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Application Information

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IPC IPC(8): C07C29/80C07C31/20C07D307/33C07C45/75C07C47/19C07C253/16C07C255/12
CPCC07C29/80C07D307/33C07C45/75C07C253/16C07C47/19C07C255/12C07C31/20Y02P20/10
Inventor 李涛蔡奇峰赵毅徐帝汪洪湖刘伟
Owner 安徽泰格生物科技有限公司
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