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Load-type non-crystal-state alloy hydogenation catalyst and preparing method

A technology of amorphous alloys and hydrogenation catalysts, applied in the direction of metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of poor mechanical strength of catalysts, blockage of reactors, Broken and other problems, to achieve the effect of high selectivity and acquisition rate

Inactive Publication Date: 2006-10-25
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Phenol hydrogenation is further divided into gas-phase and liquid-phase hydrogenation. The catalysts used mainly focus on the research of supporting Pd-type gas-phase catalysis. The traditional carrier (Al 2 o 3 , MgO) by adding alkali metals and alkaline earth metals for modification, but there are mainly the following defects: (1) Al 2 o 3 It is easy to deposit carbon during the reaction process and cause catalyst deactivation; (2) MgO-based catalyst has poor mechanical strength, and it is easy to break and block the reactor during use.

Method used

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  • Load-type non-crystal-state alloy hydogenation catalyst and preparing method
  • Load-type non-crystal-state alloy hydogenation catalyst and preparing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Step 1: A certain amount of Mg(NO 3 ) 2 , Al(NO 3 ) 3 (both are solid) dissolved in deionized water, dubbed C Mg(NO3)2 =1.43M,C Al(NO3)3 = 0.36M of clear solution A. A certain amount of NaOH, Na 2 CO 3 (both are solid) dissolved in deionized water, dubbed C NaOH =3.5M, C Na2CO3 = 0.94M of clear solution B.

[0026] Step 2: Take 700mL of solution A and slowly add it dropwise to 1000mL of solution B at 60°C, the control time is 1-2 hours, then continue to age at 60°C for 18 hours, filter while hot and wash until neutral, at 80°C Dry at -120°C to obtain a hydrotalcite carrier, which is ground for use.

[0027] Step 3: Weigh a certain amount of KBH 4 (solid) and NaOH, which are dissolved in deionized water together to form a 2.0M transparent solution, which is used as a reducing agent for subsequent use. Weigh a certain amount of PdCl 2 (solid) and Ce(NO 3 ) 3 (solid), dissolve them together in deionized water to form C Pd2+ = 0.28M, C Ce3+ =0.021M solution...

Embodiment 2

[0032] Step 1: Same as Step 1 in Example 1.

[0033] Step 2: Same as step 2 in Example 1.

[0034] Step 3: Same as Step 3 in Example 1.

[0035] Step 4: Weigh 1.0 g of hydrotalcite carrier, impregnate 1.0 mL of solution C overnight with an equal volume, and the rest of the steps are the same as Step 4 of Example 1.

[0036] Step 5: Same as Step 5 in Example 1 to obtain an amorphous alloy (Pd-Ce-B / HT-2) catalyst.

[0037] Step 6: Same as Step 6 in Example 1.

Embodiment 3

[0039] Step 1: Same as Step 1 in Example 1.

[0040] Step 2: Same as step 2 in Example 1.

[0041] Step 3: Same as Step 3 in Example 1.

[0042] Step 4: Weigh 1.0 g of hydrotalcite carrier, impregnate 1.5 mL of solution C overnight with an equal volume, and the remaining steps are the same as Step 4 of Example 1.

[0043] Step 5: Same as Step 5 in Example 1 to obtain an amorphous alloy (Pd-Ce-B / HT-3) catalyst.

[0044] Step 6: Same as Step 6 in Example 1.

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Abstract

The present invention discloses a loaded type amorphous alloy catalyst for preparing cyclohexanone by means of phenol catalytic hydrogenation and its preparation method. Said invention utilizes isochoric impregnation KBH4 reduction method to prepare amorphous alloy catalyst, said preparation method includes the following steps: preparing hydrotalcite carrier; making metal salt precursor solution and hydrotalcite carrier undergo the process of isochoric impregnation treatment; drying; roasting; drop-adding reductant KBH4 solution to make reduction; successively using deionized water and absolute ethyl alcohol to wash black solid precipitate obtained by above-mentioned solution reaction to neutrality so as to obtain the invented amorphous alloy catalyst.

Description

technical field [0001] The invention relates to a catalyst and a preparation method thereof, in particular to a supported amorphous alloy hydrogenation catalyst and a preparation method thereof, which are mainly used for the catalytic hydrogenation of phenol to prepare cyclohexanone. Background technique [0002] Cyclohexanone is an important organic chemical product with high solubility and low volatility. It can be used as a special solvent. It is an ideal solvent for polymers such as nitrocellulose and cellulose. It is also an important organic chemical raw material. It is the main intermediate in the preparation of caprolactam and adipic acid. In 1893, A.Bayer first synthesized cyclohexanone by dry distillation of pimelic acid and lime (calcium pimelate). The industrial production processes of cyclohexanone in the world mainly include phenol hydrogenation method, cyclohexane liquid phase oxidation method, and cyclohexene hydration method. In 1943, the German I.G.Farben...

Claims

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Application Information

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IPC IPC(8): B01J23/835B01J21/12B01J21/14B01J23/10B01J23/40B01J23/74C07C49/11
Inventor 李辉李和兴张静
Owner SHANGHAI NORMAL UNIVERSITY
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