A kind of method for synthesizing 1,4-butanediol by hydrogenation of 1,4-butynediol

A technology of butynediol and butanediol, which is applied in chemical instruments and methods, preparation of organic compounds, hydrogenation preparation, etc., can solve the problems of increased fixed capital investment, increased separation cost, large energy consumption, etc., and achieves by-products Fewer types, lower separation costs, and easier separation

Active Publication Date: 2022-07-22
LINGNAN NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Based on the above analysis, the low-pressure hydrogenation process usually produces a large amount of polycondensation aldehyde, and at the same time leads to the isomerization of butylene glycol to generate a large amount of hydroxybutyraldehyde, which increases the cost of separation, while the high-pressure hydrogenation can reduce the production of by-products , but it needs to consume a lot of energy, and the requirements for equipment are also high, and the investment in fixed capital increases

Method used

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  • A kind of method for synthesizing 1,4-butanediol by hydrogenation of 1,4-butynediol
  • A kind of method for synthesizing 1,4-butanediol by hydrogenation of 1,4-butynediol
  • A kind of method for synthesizing 1,4-butanediol by hydrogenation of 1,4-butynediol

Examples

Experimental program
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Effect test

Embodiment 1～8

[0035] The preparation of embodiment 1~8 one-stage hydrogenation reaction catalyst 1~8

[0036] The compositions of the one-stage hydrogenation reaction catalysts 1 to 8 are shown in Table 1.

[0037] Weigh a certain amount of ruthenium trichloride, nickel nitrate, and the soluble salt of the auxiliary agent and dissolve them in 50 mL of water, then add 3 g of carrier, and continue to stir for 6 h; then add 1 mol / L ammonia water to adjust pH=9 to 10, and continue to stir for 4 h , left to stand overnight; suction filtration, washed with deionized water, dried at 120 °C, calcined at 700 °C in argon for 2 h, and reduced in a hydrogen atmosphere at a temperature of 300 °C for 3 h to obtain a hydrogenation reaction catalyst 1-8 (see Table 1). 1).

Embodiment 9～16

[0038] Examples 9-16 Preparation of two-stage hydrogenation catalysts 9-16

[0039] The compositions of the two-stage hydrogenation reaction catalysts 9 to 16 are shown in Table 1.

[0040] Dissolve a certain amount of ruthenium trichloride and the soluble salt of the auxiliary agent in 30 mL of deionized water, then add 5 g of carrier, and continue to stir for 2 hours; then add 1 mol / L sodium hydroxide solution to adjust pH=9 to 10, and continue to stir for 4 hours , let stand overnight; suction filtration, wash with deionized water, dry at room temperature, roast in argon at 200 ° C for 6 h, and reduce in a hydrogen atmosphere at a temperature of 600 ° C for 8 h to obtain a two-stage hydrogenation reaction catalyst 9-16 ( See Table 1).

Embodiment 17

[0041] Example 17 Method for synthesizing 1,4-butanediol by hydrogenation of 1,4-butynediol

[0042] One-stage hydrogenation step: add 100 mL of 40% 1,4-butynediol aqueous solution to a 250-mL autoclave, add any one of the first-stage hydrogenation reaction catalysts 1 to 8, seal, replace with nitrogen for 4 times, and fill with hydrogen The pressure is increased to 2MPa, the temperature is raised to 130°C, and the stirring is continued until the pressure in the reaction kettle does not change.

[0043] Second-stage hydrogenation step: add the first-stage hydrogenation product into a 250 mL autoclave, add any one of the second-stage hydrogenation reaction catalysts 9 to 16, seal, replace with nitrogen for 4 times, fill with hydrogen to a pressure of 1 MPa, and heat up. When the temperature reaches 90°C, stirring is continued until the pressure in the reaction kettle does not change, and the catalyst is separated by releasing the pressure to obtain the final hydrogenated produc...

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Abstract

The invention discloses a method for synthesizing 1,4-butanediol by hydrogenation of 1,4-butynediol. The method comprises the following steps: performing hydrogenation reaction on 1,4-butynediol in a first-stage hydrogenation reactor on a modified Ni-based catalyst, and separating under pressure to obtain a first-stage hydrogenation product; the modified Ni-based catalyst has an active group of It is divided into Ni, and the auxiliary agent is at least one of Ru, K or Mg; the obtained one-stage hydrogenation product and Ru-based catalyst are carried out in a two-stage hydrogenation reactor for a two-stage hydrogenation reaction, and pressure relief is separated to obtain 1, 4-Butanediol; the active component of Ru-based catalyst is Ru. In the present invention, the modified Ni-based catalyst and Ru-based catalyst are combined, so that the conversion rate of 1,4-butynediol reaches 100%, the selectivity of 1,4-butanediol reaches 98%, and the catalytic activity is good. , high selectivity, mild reaction conditions, less by-products, and easy separation.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals. More specifically, it relates to a method for synthesizing 1,4-butanediol by hydrogenation of 1,4-butynediol. Background technique [0002] 1,4-Butanediol is an important organic chemical raw material, which can be used to produce polybutylene succinate, polybutylene terephthalate, tetrahydrofuran, etc. It can also be used as solvent and chain extender and cross-linking agents, etc. [0003] Reppe synthesis is a widely used method for industrial production of 1,4-butanediol. The method takes acetylene and formaldehyde as raw materials, firstly synthesizes 1,4-butynediol from acetylene and formaldehyde under the action of copper catalyst, and then 1,4-butynediol is produced by catalytic hydrogenation to produce 1,4-butynediol . The hydrogenation process is usually carried out by a two-step method. The first-stage hydrogenation is usually carried out in a suspended bed reactor or a fixed...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/17C07C31/20B01J23/89B01J37/08B01J37/18
CPCC07C29/172B01J23/8946B01J23/58B01J37/082B01J37/18C07C31/207
Inventor 王磊陈莉张国强王胜
Owner LINGNAN NORMAL UNIV
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