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Preparation method for fixed bed Raney nickel catalyst

A Raney nickel and catalyst technology is applied in the field of Raney catalyst preparation, which can solve the problems of reducing catalyst activity, complex preparation method, and easily broken catalyst, and achieves the effects of uniform activity, simple preparation process and high mechanical strength.

Active Publication Date: 2009-11-11
HANERGY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst prepared by this method has the defects of complex preparation method and low mechanical strength. When the reaction solution flows through the fixed-bed Raney nickel catalyst at a relatively high flow rate, the catalyst is easily broken and falls off, which reduces the activity of the catalyst.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Soak the nickel foam in acetone for 10 minutes, take it out and wash it with water; then immerse it in the aluminum nitrate solution, then add the formaldehyde solution, let it stand for 1 hour, take it out, wash it with water, spin it dry, dry it in vacuum, and put it under nitrogen Calcined at 600° C. for 5 minutes in an atmosphere; cooled to room temperature after calcination, and leached the obtained sample in 10 wt % sodium hydroxide solution for 1 hour to obtain a fixed-bed Raney nickel catalyst.

[0025] Wherein the volume ratio of aluminum nitrate solution and nickel foam is 1: 1, and the mass ratio of the nickel element in foam nickel and the aluminum element in aluminum nitrate is 3: 1; The concentration of formaldehyde solution is 0.02mol / L; The molar ratio of formaldehyde content to aluminum element content in the aluminum nitrate solution is 1:1.

Embodiment 2

[0027] Soak the nickel foam in acetylacetone for 360 minutes, take it out and wash it with water; then immerse it in the aluminum chloride solution, then add the hydrazine solution, take it out after standing for 3 hours, wash it with water, spin it dry, and dry it in vacuum. In a helium atmosphere, it was calcined at 700°C for 180 minutes; after calcined, it was cooled to room temperature, and the obtained sample was leached in 20 wt% sodium hydroxide solution for 24 hours to obtain a fixed-bed Raney nickel catalyst.

[0028] Wherein the volume ratio of aluminum chloride solution and nickel foam is 10:1, and the mass ratio of nickel element in foam nickel and aluminum element in aluminum chloride is 1:1; The concentration of hydrazine solution is 0.05mol / L; The hydrazine solution The molar ratio of the hydrazine content in the aluminum chloride solution to the aluminum element content in the aluminum chloride solution is 5:1.

Embodiment 3

[0030] Soak the nickel foam in thienoyl trifluoroacetone for 30 minutes, take it out and wash it with water; then immerse it in the aluminum sulfate solution, then add the sodium borohydride solution, let it stand for 5 hours, take it out, wash it with water, and dry it , after vacuum drying, in a neon gas atmosphere, at a temperature of 1000 ° C for 600 min; after roasting, cool to room temperature, and leaching the obtained sample in 30 wt% sodium hydroxide solution for 12 h to obtain a fixed-bed Raney nickel catalyst.

[0031] Wherein the volume ratio of aluminum sulfate solution and nickel foam is 30: 1, the mass ratio of nickel element in foam nickel and aluminum element in aluminum sulfate is 5: 1; The concentration of sodium borohydride solution is 0.2mol / L; Hydroboration The molar ratio of the sodium borohydride content in the sodium solution to the aluminum element content in the aluminum sulfate solution is 3:1.

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Abstract

The invention discloses a preparation method for a fixed bed Raney nickel catalyst, which comprises the following steps: (1) pretreatment: soaking ketone solvents by using foaming nickel, then taking out and washing the foam nickel by using water; (2) immersing and plating aluminum; immersing the foam nickel obtained from the step (1) into aluminum salt solution, then adding reducing solution into the mixed solution and standing the mixed solution for 1 to 12 hours; (3) baking: washing and drying a sample obtained from the step (2), and baking the sample at a temperature of between 600 and 1,000 DEG C in inert atmosphere for 5 to 600 minutes; and (4) leaching: leaching the sample obtained from the step (3) in sodium hydroxide or potassium hydroxide solution for 1 to 48 hours, and obtaining the fixed bed Raney nickel catalyst. The preparation method has the advantages that the preparation process is simple; and the catalyst prepared by the method has higher catalytic activity, stronger mechanical strength and longer service life. The invention belongs to the technical filed of catalyst preparation.

Description

technical field [0001] The invention relates to a preparation method of a Raney catalyst, in particular to a preparation method of a fixed-bed Raney nickel catalyst. Background technique [0002] Bin Hong Liu et al. reported the method of using Raney nickel, Raney cobalt and Raney nickel cobalt to catalyze the hydrolysis of sodium borohydride to generate hydrogen (Journal of Alloys and Compounds, 415, 2006, 288-293). The reaction equation is as follows: [0003] NaBH 4 +2H 2 O→4H 2 +NaBO 2 [0004] In this report, powdered Raney nickel and powdered Raney cobalt were used to catalyze the decomposition of sodium borohydride to produce hydrogen. The powdered Raney catalyst is easy to lose in practical application, which increases the difficulty of separating the generated hydrogen from the catalyst, thus limiting its application. In the patent application whose publication number is CN 1774390A, Raney nickel is used to catalyze the decomposition of sodium borohydride to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J25/02
Inventor 肖钢王玉晓
Owner HANERGY TECH
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