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Preparation method of 1,3-propylene glycol

A technology of propylene glycol and hydroxypropionaldehyde, applied in 1 field, can solve problems such as difficult separation, high acetal impurity content, and high acetal content

Inactive Publication Date: 2018-08-03
王鹏飞
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  • Application Information

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Problems solved by technology

[0004] The preparation of 1,3-propanediol by the hydrogenation of intermediate 3-hydroxypropionaldehyde mostly has the following problems: the hydrogenation of 3-hydroxypropionaldehyde to synthesize 1,3-propanediol is an exothermic reaction, and in the hydrogenation process of 3-hydroxypropionaldehyde, 3-Hydroxypropionaldehyde and 1,3-propanediol are prone to generate acetal impurities such as 2-(2-hydroxyethyl)-1,3-epoxyhexacyclo, and the higher the reaction temperature, the higher the content of acetal impurities generated
The volatility difference between these acetal impurities and 1,3-propanediol is very small, and the separation is difficult, resulting in high acetal content in the product, resulting in unqualified viscosity and chromaticity of the polymerization product downstream of 1,3-propanediol

Method used

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Examples

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preparation example Construction

[0024] The preparation method of 1,3-propanediol of one embodiment, comprises the following steps S110~S130:

[0025] S110, providing an aqueous solution of 3-hydroxypropanal with a mass concentration of 8%-13%.

[0026] Specifically, the aqueous solution of 3-hydroxypropanal is prepared by the following method (S1101~S1102):

[0027] S1101. Mix acrolein aqueous solution with a mass concentration of 12%~17% and hydroquinone, and react at 40°C~70°C, 0.1MPa~1.0MPa, under the action of a weakly acidic chelating resin catalyst to obtain 3- Aqueous solution of hydroxypropionaldehyde.

[0028] Among them, the aqueous solution of acrolein is prepared by oxidation of propylene and then simply concentrated to 12%~17%.

[0029] It can be understood that if the mass concentration of acrolein in the aqueous solution of acrolein is less than 12%, although it is beneficial to improve the selectivity of the hydration reaction, it will cause the concentration of 1,3-propanediol in the hydro...

Embodiment 1

[0052] Mix acrolein aqueous solution with a mass concentration of 14% and hydroquinone (the mass concentration of hydroquinone after mixing is 300ppm), at 50°C, 0.12MPa, 380g weakly acidic chelating resin catalyst D851 (purchased in Zhejiang Under the action of Zhengguang Industrial Co., Ltd.), the reaction obtained an aqueous solution of 3-hydroxypropanal.

[0053] After testing, the conversion rate of acrolein was 85.1%, and the selectivity of 3-hydroxypropanal was 87.5%.

Embodiment 2

[0055] The aqueous solution of 3-hydroxypropionaldehyde with a mass concentration of 8% to 13% prepared in Example 1 is provided.

[0056] Mix hydrogen with a flow rate of 130L / h and 1.0L / h of 11.9wt% 3-hydroxypropanal in water (the molar ratio of hydrogen to 3-hydroxypropanal is 3.6:1), and carry out a hydrogenation reaction and Two-stage hydrogenation reaction to obtain a two-stage hydrogenation reaction product. Among them, the reaction conditions of the one-stage hydrogenation reaction are: 764g supported nickel-based catalyst (the carrier is a combination of alumina and silica, with a nickel content of 31wt%), 50°C~60°C, 10.0MPa. The reaction conditions of the two-stage hydrogenation reaction are: 236g supported nickel-based catalyst (the carrier is a combination of alumina and silica, and the nickel content is 31wt%), 115°C, 10.0MPa.

[0057] After cooling part of the second-stage hydrogenation reaction product to 50°C, it was circulated to the first-stage hydrogenation...

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Abstract

The invention provides a preparation method of 1,3-propylene glycol. The preparation method comprises the following steps: providing an aqueous solution of 3-hydroxypropionaldehyde with the mass concentration of 8 to 13 percent; mixing hydrogen and the aqueous solution of 3-hydroxypropionaldehyde, and successively performing the one-stage hydrogenation reaction and two-stage hydrogenation reactionto obtain a two-stage hydrogenated product; and circulating a part of the two-stage hydrogenated product to the one-stage hydrogenation reaction. According to the preparation method of 1,3-propyleneglycol, part of the two-stage hydrogenated product is circulated to the one-stage hydrogenation reaction to absorb the reaction heat, so that the hot-spot temperature of the first hydrogenation reaction can be reduced, the content of acetal impurities in the product can be effectively reduced, and the selectivity of the hydrogenation reaction can be improved.

Description

technical field [0001] The invention relates to the field of hydrogenation technology, in particular to a method for preparing 1,3-propanediol. Background technique [0002] 1,3-propanediol is an important chemical raw material, and its main use is as a monomer and terephthalic acid to synthesize new polyester material poly(1,3-trimethylene terephthalate) (PTT). Nylon fiber has more excellent performance. [0003] There are two main methods for preparing 1,3-propanediol: (1) 3-hydroxypropionaldehyde is synthesized from ethylene oxide, carbon monoxide and hydrogen, and 3-hydroxypropionaldehyde is hydrogenated to synthesize 1,3-propanediol; (2) Acrolein is hydrated to synthesize 3-hydroxypropanal, and 3-hydroxypropanal is hydrogenated to synthesize 1,3-propanediol. [0004] The preparation of 1,3-propanediol by the hydrogenation of intermediate 3-hydroxypropionaldehyde mostly has the following problems: the hydrogenation of 3-hydroxypropionaldehyde to synthesize 1,3-propaned...

Claims

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Application Information

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IPC IPC(8): C07C29/141C07C31/20
CPCC07C29/141C07C45/64C07C31/205C07C47/19
Inventor 王鹏飞
Owner 王鹏飞
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