Method for synthesizing 1,4-butanediol by hydrogenating 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: 2019-11-22
LINGNAN NORMAL UNIV
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  • Summary
  • 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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  • Method for synthesizing 1,4-butanediol by hydrogenating 1,4-butynediol
  • Method for synthesizing 1,4-butanediol by hydrogenating 1,4-butynediol
  • Method for synthesizing 1,4-butanediol by hydrogenating 1,4-butynediol

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Embodiment 1～8

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

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

[0037] Weigh a certain amount of ruthenium trichloride, nickel nitrate, and soluble salts of additives and dissolve them in 50mL of water, then add 3g of carrier, and continue stirring for 6h; then add 1mol / L ammonia water to adjust the pH=9~10, and continue stirring for 4h , standing overnight; suction filtration, washing with deionized water, drying at 120°C, roasting at 700°C in argon for 2h, and reducing in a hydrogen atmosphere at a temperature of 300°C for 3h to obtain a hydrogenation reaction catalyst 1-8 (see Table 1).

Embodiment 9～16

[0038] The preparation of embodiment 9~16 two stage hydrogenation reaction catalyst 9~16

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

[0040] Dissolve a certain amount of ruthenium trichloride and soluble salts of additives in 30 mL of deionized water, then add 5 g of carrier, and continue stirring for 2 h; then add 1 mol / L sodium hydroxide solution to adjust the pH to 9-10, and continue stirring for 4 h , standing overnight; suction filtration, washing with deionized water, drying at room temperature, calcination at 200°C for 6h in argon, and reduction in a hydrogen atmosphere at 600°C for 8h to obtain two-stage hydrogenation catalysts 9-16( See Table 1).

Embodiment 17

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

[0042] One-stage hydrogenation step: add 100mL 40% 1,4-butynediol aqueous solution into a 250mL autoclave, add any one of the one-stage hydrogenation reaction catalysts 1 to 8, seal, replace with nitrogen gas for 4 times, and fill with hydrogen The pressure was raised to 2MPa, the temperature was raised to 130°C, and the stirring was continued until the pressure in the reactor remained unchanged, and the catalyst was separated by releasing the pressure to obtain a hydrogenation product.

[0043] Second-stage hydrogenation step: Add the first-stage hydrogenation product into a 250mL autoclave, add any one of the second-stage hydrogenation reaction catalysts 9 to 16, seal it, replace it with nitrogen gas 4 times, fill it with hydrogen gas to a pressure of 1MPa, and raise the temperature To 90°C, continue to stir until the pressure in the reactor does not change, release the pressure...

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Abstract

The invention discloses a method for synthesizing 1,4-butanediol through hydrogenation of 1,4-butynediol. The method comprises the following steps: 1,4-butynediol is subjected to a hydrogenation reaction in a first-stage hydrogenation reactor on a modified Ni-based catalyst, and pressure relief and separation is performed, so that a first-stage hydrogenation product is obtained, wherein the activecomponent of the modified Ni-based catalyst is Ni, and the auxiliary agent is at least one of Ru, K or Mg; then a second-stage hydrogenation reaction is carried out on the obtained first-stage hydrogenation product and a Ru-based catalyst in a second-stage hydrogenation reactor, and pressure relief and separation is performed to obtain the 1,4-butanediol, wherein the active component of the Ru-based catalyst is Ru. According to the method, the modified Ni-based catalyst and the Ru-based catalyst are combined, so that the conversion rate of the 1,4-butynediol reaches 100%, the selectivity of the 1,4-butanediol reaches 98%, and the method has the advantages of being good in catalytic activity, high in selectivity, mild in reaction condition, few in by-product variety and easy to separate.

Description

technical field [0001] The invention belongs to the field of fine chemical technology. More specifically, it relates to a method for synthesizing 1,4-butanediol by hydrogenating 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., and can also be used as a solvent and chain extender and crosslinking agents, etc. [0003] The Reppe synthesis method is a widely used method for the industrial production of 1,4-butanediol. The method uses acetylene and formaldehyde as raw materials, and first synthesizes 1,4-butynediol from acetylene and formaldehyde under the action of a copper catalyst, and then 1,4-butynediol is produced by catalytic hydrogenation to 1,4-butanediol . The hydrogenation process is usually carried out in two steps. The first-stage hydrogenation is usually carried out in a suspended bed reactor or a fix...

Claims

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Application Information

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Patent Type & Authority Applications(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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