Synthesis method for nickel-base composite catalyst used for synthesizing n-amylamine from pentanenitrile

A technology of composite catalyst and synthesis method, which is applied in the field of synthesis of nickel-based composite catalyst, can solve the problems of increased cost, low yield, high cost of raw materials, etc., and achieve the effect of preventing agglomeration

Inactive Publication Date: 2017-04-26
浙江优创材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. A considerable amount of by-products are generated when the target product is generated in each method, which requires subsequent purification and separation, the yield is not high a

Method used

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  • Synthesis method for nickel-base composite catalyst used for synthesizing n-amylamine from pentanenitrile
  • Synthesis method for nickel-base composite catalyst used for synthesizing n-amylamine from pentanenitrile
  • Synthesis method for nickel-base composite catalyst used for synthesizing n-amylamine from pentanenitrile

Examples

Experimental program
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Effect test

Embodiment 1 and 2

[0022] Embodiment 1 and 2: the preparation of nickel-based composite catalyst

[0023] The catalyst carrier used in the following examples 1-6 is purchased from the market, and only the titanium-modified activated alumina carrier and the silica carrier are used as examples in the examples 1-6:

Embodiment 1

[0025] (1) Preparation of soluble nickel salt solution: Weigh 300g of nickel nitrate and put it into a 1L beaker, add 150ML deionized water and 150ML absolute ethanol, stir to dissolve; add additives EDTA 5g, diethylamine 15g, 20g of triethylamine, 5g of surfactant PEG800, 5g of PEG100005g were stirred and dissolved for later use;

[0026] (2) Preparation of the catalyst precursor: put 600 g of the purchased titanium-modified alumina carrier into the above room temperature solution and soak for 2 days and 2 nights, then take it out and ventilate and dry it in an oven at 80±1°C to obtain 700 g of the precursor for use;

[0027] (3) Catalyst precursor reduction: put 100g of the precursor into a 2L reaction kettle, put in 0.05mol / l sodium borohydride solution to cover the precursor, add a small amount of sodium hydroxide to adjust the pH to 14, start stirring and raise the temperature to 70±1℃ Down reaction, reaction is complete after 2 hours;

[0028] (4) Filter the reduced cat...

Embodiment 2

[0030] (1) Preparation of soluble nickel salt solution: Weigh 300g of nickel nitrate and put it into a 1L beaker, add 150ML deionized water and 150ML absolute ethanol, stir to dissolve; add additives EDTA 5g, diethylamine 15g, 20g of triethylamine, 5g of surfactant PEG800, 5g of PEG100005g were stirred and dissolved for later use;

[0031] (2) Preparation of catalyst precursor: Put 600g of the purchased large-pore silica carrier (particle size 1-3mm) into the above room temperature solution for 2 days and 2 nights, take it out and ventilate and dry it in an oven at 80±1°C Get 700g of precursor for later use;

[0032] (3) Catalyst precursor reduction: put 100g of the precursor into a 2L reaction kettle, put in 0.05mol / l sodium borohydride solution to cover the precursor, add a small amount of sodium hydroxide to adjust the pH to 14, and start stirring to raise the temperature to 70±1°C Down reaction, reaction is complete after 2 hours;

[0033] (4) Filter the reduced catalyst...

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Abstract

The invention relates to a synthesis method for a nickel-base composite catalyst used for synthesizing n-amylamine from pentanenitrile. The synthesis method includes the steps of: 1) dissolving soluble nickel salt in a solvent to prepare a solution; 2) impregnating a moulded carrier having a pore structure in the solution in the step 1) to produce a catalyst precursor; 3) reducing the catalyst precursor; 4) drying the reduced catalyst precursor to produce the nickel-base composite catalyst. In the method, the pH of a reductant solution is controlled to be a proper range of 8-14, so that Ni<2+> can be reduced completely and a moderated reduction rate can be maintained, thereby producing metal nickel particles in nano scale. The synthesis method can prevent agglomeration due to growth of the metal nickel particles, thereby producing high-activity supported nickel-base composite catalyst.

Description

technical field [0001] The invention relates to a method for synthesizing a nickel-based composite catalyst used for synthesizing n-pentylamine from valeronitrile, belonging to the technical field of fine chemicals. Background technique [0002] N-amylamine is an important chemical intermediate, which is widely used in the synthesis of medicines, dyes, solvents, anti-corrosion agents, emulsifiers, antioxidants, flotation agents and rubber vulcanization accelerators. [0003] There are many ways to synthesize n-pentylamine, the typical ones are: valeraldehyde method, hexamide method, valeronitrile method and n-pentanol method. Among them, the selectivity of the valeraldehyde method is about 48%, the selectivity of the azide method is about 88%, the selectivity of the hexamide method is about 81%, the selectivity of the valeronitrile method is about 71%, and the selectivity of the di-n-pentyl boron chloride method is about 93%. %Wait. Another: Our company's existing valeroni...

Claims

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Application Information

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IPC IPC(8): B01J23/755C07C209/48C07C211/07
CPCB01J23/755C07C209/48C07C211/07
Inventor 茅月成朱晓东施根祥吴元飞
Owner 浙江优创材料科技股份有限公司
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