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Preparation method of neopentyl glycol

A technology of neopentyl glycol and hydroxypivalaldehyde is applied in the preparation of organic compounds, chemical instruments and methods, preparation of hydroxy compounds, etc., and can solve the problems of cumbersome production process, reduced yield and purity of neopentyl glycol, and the like, To achieve the effect of shortening the process flow, improving the selectivity and improving the yield

Active Publication Date: 2013-12-18
BEIJING SJ ENVIRONMENTAL PROTECTION & NEW MATERIAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that in the prior art, the ester substances contained in the catalytic hydrogenation product of hydroxypivalaldehyde are treated by saponification, which leads to a reduction in the yield and purity of neopentyl glycol, and the production process is cumbersome, and then provides a A method for producing neopentyl glycol with a simple process capable of simultaneously performing the catalytic hydrogenation of hydroxypivalaldehyde and the hydrogenolysis of by-product esters

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Use 5wt% NaOH solution and 10wt% KOH solution to adjust the pH value of the hydroxypivalaldehyde solution to 10.0. In the hydroxypivalaldehyde solution, in terms of mass percentage, the hydroxypivalaldehyde is 79wt%, and the water is 20wt%, the remainder is impurities;

[0028] (2) Using a fixed-bed reactor as a catalytic hydrogenation reactor, add the hydroxypivalaldehyde solution treated in step (1) into the fixed-bed reactor equipped with a nickel catalyst. 2 In the presence, the liquid space velocity of the hydroxypivalaldehyde solution is controlled to be 0.1h -1 , H 2 The gas space velocity is 300h -1 , reacting at a temperature of 110°C and a pressure of 2.0Mpa to obtain crude neopentyl glycol;

[0029] (3) The crude product of neopentyl glycol obtained in step (2) was subjected to vacuum distillation and purification at an absolute pressure of 0.02 MPa and a temperature of 180° C. to obtain neopentyl glycol.

[0030] After testing, during the operation p...

Embodiment 2

[0032] (1) With 10wt% Na 2 CO 3solution and 5wt% K 2 CO 3 The solution adjusts the pH value of the hydroxypivalaldehyde solution to 9.5. In the hydroxypivalaldehyde solution, in terms of mass percentage, the hydroxypivalaldehyde is 45wt%, water is 52wt%, and the balance is impurities, wherein the impurities include methanol , isobutyraldehyde, neopentyl glycol isobutyrate, triethylamine and other substances;

[0033] (2) Using a fixed-bed reactor as a catalytic hydrogenation reactor, add the hydroxypivalaldehyde solution treated in step (1) into the fixed-bed reactor equipped with a copper catalyst. 2 In the presence, the liquid space velocity of the hydroxypivalaldehyde solution is controlled to be 0.3h -1 , H 2 The gas space velocity is 300h -1 , reacting at a temperature of 120°C and a pressure of 3.5Mpa to obtain crude neopentyl glycol;

[0034] (3) Purify the crude product of neopentyl glycol obtained in step (2) by vacuum distillation under the conditions of an ab...

Embodiment 3

[0037] (1) Use 5wt% KOH solution to adjust the pH value of the hydroxypivalaldehyde solution to 9.0. In the hydroxypivalaldehyde solution, in terms of mass percentage, hydroxypivalaldehyde is 55wt%, methanol is 20wt%, and ether is 20wt% %, the remainder is impurities, wherein said impurities include methanol, isobutyraldehyde, hydroxyvaleric acid-neopentyl glycol ester, isobutyric acid neopentyl glycol ester;

[0038] (2) Using a fixed-bed reactor as a catalytic hydrogenation reactor, add the hydroxypivalaldehyde solution treated in step (1) into the fixed-bed reactor equipped with a copper catalyst. 2 In the presence, the liquid space velocity of the hydroxypivalaldehyde solution is controlled to be 0.5h -1 、H 2 The gas space velocity is 300h -1 , reacting at a temperature of 130°C and a pressure of 4.0Mpa to obtain crude neopentyl glycol;

[0039] (3) The crude product of neopentyl glycol obtained in step (2) is subjected to vacuum distillation and purification under the ...

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Abstract

The invention provides a preparation method of neopentyl glycol, and belongs to the technical field of the preparation of alcohols. The preparation method includes the following steps: (1) regulating the pH value of a hydroxypivalaldehyde solution to 7.5-10; (2) obtaining a neopentyl glycol crude product by catalytic hydrogenation of hydroxypivalaldehyde treated by the step (1) under the effect of a hydrogenation catalyst at the temperature of 110-140 DEG C and with the pressure of 2.0-5.0 Mpa; and (3) purifying the neopentyl glycol crude product obtained in the step (2). The content of esters and other side products in the neopentyl glycol crude product prepared by the preparation method of the neopentylene glycol is extremely low, and the yield and purity of the neopentyl glycol are improved. In addition, a hydroxypivalaldehyde raw material system can be directly used for catalytic hydrogenation without any treatment, processes of aldol condensation and catalytic hydrogenation for preparation of the neopentyl glycol can be reduced, and the production efficiency can be improved.

Description

technical field [0001] The invention relates to a method for preparing neopentyl glycol, in particular to a method for preparing neopentyl glycol by hydrogenation of hydroxypivalaldehyde, and belongs to the technical field of alcohol preparation. Background technique [0002] Neopentyl glycol (NPG, chemical name: 2,2-dimethyl-1,3-propanediol) is a stable diol. As an important fine chemical product, neopentyl glycol is mainly used in the production of unsaturated resins, polyester powder coatings, oil-free alkyd resins, polyurethane foams, synthetic plasticizers, surfactants, insulating materials, Printing inks, polymerization inhibitors, synthetic aviation lubricating oil additives, etc. [0003] The preparation methods of neopentyl glycol mainly include condensation hydrogenation method and disproportionation method, wherein, the research on the preparation of neopentyl glycol by condensation hydrogenation method began in the 1970s. The steps for preparing neopentyl glyco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/141C07C29/149
Inventor 王振凡林科王庆明刘玉珍李春伟金凤迟徐蒋红赵新颖
Owner BEIJING SJ ENVIRONMENTAL PROTECTION & NEW MATERIAL CO LTD
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