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Metal silicide catalyst of selective hydrogenation 1,4-butynediol and application of metal silicide catalyst

A metal silicide and selective hydrogenation technology, which is applied in the field of fine chemicals, can solve the problems of low yield of 1,4-butenediol, easy loss of catalyst active components, and no consideration of catalyst stability, and achieves the goal of inhibiting accumulation. Carbon, good prospects for industrial applications, the effect of enhancing fluctuating adaptability

Active Publication Date: 2013-12-04
DALIAN UNIV OF TECH
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Chinese patent, publication number: CN1172792A, introduces the method that butynediol prepares butanediol through two-step method, and its first step used catalyst is suspended palladium-carrier catalyst, and the second step adopts nickel-carrier catalyst, adopts two stages to add Hydrogen process, the steps are cumbersome, the cost is high, the reaction pressure is high and the yield of the target product 1,4-butenediol is not high
[0009] Chinese patent, publication number: CN101306368A, introduces the preparation method of butynediol two-step hydrogenation to butanediol two-stage hydrogenation catalyst, uses surfactant, adopts impregnation method to prepare nickel-based supported catalyst, but does not consider the catalyst Stability in this reaction, and the active ingredient of the catalyst is easy to lose in the catalytic reaction

Method used

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  • Metal silicide catalyst of selective hydrogenation 1,4-butynediol and application of metal silicide catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Embodiment 1: the preparation of Raney type nickel silicide catalyst

[0022] Activate 0.3g of Raney-type nickel at 200°C for 2h under a hydrogen atmosphere, and then pass through 10% SiH 4 / H 2 The temperature of the mixed gas was raised to the silicide reaction, reacted at 250°C, 350°C, and 450°C for 15 minutes, and cooled to room temperature under an inert atmosphere to obtain Raney-type nickel silicide catalysts in different phases. Its specific phase changes are as attached figure 1 Shown in the XRD spectrum.

Embodiment 2

[0023] Embodiment 2: the preparation of cobalt silicide catalyst

[0024] Reduce 0.5g of cobalt oxide at 400°C for 2h under hydrogen atmosphere, then pass H 2 Carries 10% CH 3 SiCl 3 The saturated steam was programmed to heat up to 600°C for silicide reaction for 60 minutes, and cooled to room temperature under an inert atmosphere to obtain a cobalt silicide catalyst.

Embodiment 3

[0025] Embodiment 3: the preparation of PdSi / SBA-15 catalyst

[0026] Activate 0.3g of 1%Pd / SBA-15 at 200°C for 2h under a hydrogen atmosphere, and then pass in H 2 Carries 10% HSiCl 3 The saturated steam was programmed to heat up to 300°C for silicide reaction for 60 minutes, and cooled to room temperature under an inert atmosphere to obtain a PdSi / SBA-15 catalyst.

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Abstract

The invention relates to a metal silicide catalyst of selective hydrogenation 1,4-butynediol and application of the metal silicide catalyst. Temperature programmed silicification is performed on a corresponding metal catalyst under the atmosphere of organosilane to form the metal silicide catalyst. The invention provides a new technology: on the condition of low temperature and medium pressure, catalytic hydrogenation is performed on high-concentration 1,4-butynediol in one step in a fixed bed reactor through the metal silicide catalyst so as to prepare 1,4-butylene glycol. Compared with the traditional Lindlar catalyst, the prepared metal silicide catalyst has efficient hydrogenation activity, high stability and excellent industrial application prospect, is well adapted to the fluctuation of water in the reaction system so as to better restrain carbon deposition, and the addition of silicon enables higher selectivity of intermediate products, so that adoption of a poisonous addition agent is avoided.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and relates to a metal silicide catalyst for selectively hydrogenating 1,4-butynediol to prepare 1,4-butenediol and a preparation method for temperature-programmed silicification. More specifically, the present invention relates to a method of preparing 1,4-butanediol from high-concentration 1,4-butynediol by one-step catalytic hydrogenation of 1,4-butynediol in a fixed-bed reactor over a metal silicide catalyst under medium pressure conditions New technology for enediols. Compared with the traditional Lindlar catalyst, the prepared metal silicide catalyst has high-efficiency hydrogenation activity, the incorporation of silicon leads to an increase in the selectivity of intermediate products, avoids the use of poisoning additives, and has strong adaptability to water fluctuations in the reaction system , can well inhibit carbon deposition, exhibit high stability, and have good industrial appl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J25/02B01J23/75B01J29/03B01J23/42C07C33/035C07C29/17
Inventor 梁长海陈霄李闯张明明
Owner DALIAN UNIV OF TECH
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