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Method for preparing high dispersion supported hydrogenation catalyst

A catalyst and hydrogenation reaction technology, which is applied in the field of preparation of highly dispersed and loaded hydrogenation catalysts, can solve the problems of complex preparation process, high price, and low nanoparticle content, and achieve high catalytic activity, short preparation cycle and simple operation Effect

Inactive Publication Date: 2009-10-07
NANKAI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] CN1792440 adopts ultrasonic-assisted method to prepare NiB amorphous alloy catalyst, and CN1792439 adopts microwave-assisted electroless plating method to prepare supported NiB amorphous alloy catalyst. Electroless plating method needs noble metal as inducer, and generally adopts impregnation method to load noble metal on the carrier. The catalyst precursor is obtained by drying and roasting. The preparation process of this method is relatively complicated, and the introduction of an external field will increase the difficulty of preparing the catalyst.
The microemulsion method is also one of the commonly used methods to prepare small-sized nanoparticles. The content of nanoparticles obtained by the water-in-oil microemulsion method is small, and a large amount of organic solvents are used in the preparation process, which not only pollutes the environment, but also makes it difficult to separate the products.
CN101157034 prepares nanometer amorphous alloy catalyst by oil-in-water microemulsion method, although this method is better than water-in-oil type microemulsion method, will inevitably introduce organic solvent and tensio-active agent in the preparation process, give product Separation poses certain difficulties
Introducing polymer substances such as surfactants or ionic liquids is also an effective method for preparing nanoparticles, but the introduction of surfactants and ionic liquids will bring difficulties to the separation of products, and the price is relatively expensive. Therefore, it is necessary to develop a simple, Low-cost high-activity catalysts have great theoretical and practical significance

Method used

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  • Method for preparing high dispersion supported hydrogenation catalyst
  • Method for preparing high dispersion supported hydrogenation catalyst
  • Method for preparing high dispersion supported hydrogenation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] These examples illustrate the preparation of a NiB catalyst supported by a solid content of 20% aluminum sol.

[0023] Prepare a nickel acetate solution with a concentration of 0.1mol / L, mix it with a certain amount of aluminum sol with a solid content of 20%, and then prepare KBH with a concentration of 1.2mol / L 4 solution (B:Ni=3.0:1.0, atomic ratio), at 20°C, under the protection of Ar gas, the KBH 4 Drop it into the mixed solution of aluminum sol and nickel salt with a solid content of 20% at a speed of 1-6ml / min until no gas is generated during the reaction. Nickel accounts for 15% by weight of the catalyst, and the prepared catalyst is used directly, or the catalyst is washed until the washing liquid is neutral, and then stored in water or ethanol. The resulting catalyst is designated as A1.

[0024] The catalyst obtained in this example is used to prepare 4-aminophenol by hydrogenating 4-nitrophenol in the liquid phase, that is: in a 100ml autoclave, add a cata...

Embodiment 2

[0026] These examples illustrate the preparation of NiB catalysts with different loadings.

[0027]Prepare a nickel acetate solution with a concentration of 0.1mol / L, mix it with a certain amount of aluminum sol with a solid content of 20%, and then prepare KBH with a concentration of 1.2mol / L 4 solution (B:Ni=3.0:1.0, atomic ratio), at 20°C, under the protection of Ar gas, the KBH 4 Drop it into the mixed solution of aluminum sol and nickel salt with a solid content of 20% at a speed of 1-6ml / min until no gas is generated during the reaction. In the case of keeping the amount of nickel acetate constant, by changing the amount of aluminum sol, NiB catalysts with nickel loadings of 10wt%, 20wt%, 30wt% and 40wt% were prepared, and the prepared catalysts were used directly. Or wash the catalyst until the washing solution is neutral, and then store it in water or ethanol. Recorded as A2, A3, A4, A5 respectively, samples A2, A3, A4, A5 have figure 1 Characteristics.

Embodiment 3

[0029] These examples illustrate the procedure for supported NiB catalysts prepared at different temperatures.

[0030] Prepare a nickel acetate solution with a concentration of 0.1mol / L, mix it with a certain amount of aluminum sol with a solid content of 20%, and then prepare KBH with a concentration of 1.2mol / L 4 solution (B:Ni=3.0:1.0, atomic ratio), at 15°C, 25°C and 30°C, respectively, under the protection of Ar gas, the KBH 4 Drop it into the mixed solution of aluminum sol and nickel salt at a rate of 1-6ml / min until no gas is generated during the reaction. The prepared catalyst is directly used, or the catalyst is washed until the washing liquid is neutral, and then stored in water or ethanol, and the nickel accounts for 15% of the weight of the catalyst. Catalysts A6, A7 and A8 were obtained.

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Abstract

The present invention provides a method for preparing high dispersion supported hydrogenation catalyst. Alumina sol is used as a supporting material for preparing a NiB amorphous alloy catalyst with highly dispersed active component through a simple chemical reduction method. Excellent catalytic activity is represented in a reaction in which 4-nitrophenol hydrogenation is used as a probe. The activity is further higher than the NiB / r-Al2O3 catalyst which is prepared through a simple method. The catalyst has the advantages of high activity, simple preparing method, short preparing period, low cost, good reusability and excellent application prospect.

Description

technical field [0001] The invention relates to a preparation method of a supported amorphous alloy catalyst. The catalyst prepared by this method exhibited excellent catalytic activity in the hydrogenation reaction using 4-nitrophenol as a probe. Background technique [0002] Amorphous alloy catalysts have been proposed for the first time by Smith at the Seventh International Conference on Catalysis in 1980. So far, amorphous alloy catalysts are still the focus and hotspot of catalytic researchers. Amorphous alloys are a class of materials with long-range disorder and short-range order. Their unique structural characteristics endow them with excellent electrical, magnetic and catalytic properties, and they are also environmentally friendly. At present, the chemical reduction method is generally used to prepare amorphous alloy catalysts, and the metal borohydride compound KBH 4 or NaBH 4 As a reducing agent to reduce metal ions, due to metal ions and reducing agent KBH 4...

Claims

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Application Information

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IPC IPC(8): B01J21/02B01J23/755B01J37/16C07B37/02C07C213/02C07C215/76
Inventor 李伟刘皓张海保张增入
Owner NANKAI UNIV
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