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Bi-component supported catalyst of ethanol condensed n-butanol and a method of preparing thereof

A technology of supported catalyst and n-butanol, which is applied in the direction of catalyst activation/preparation, preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of low selectivity of n-butanol and high reaction temperature, and achieve simple and catalytic The effect of high activity and low cost

Inactive Publication Date: 2009-09-16
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[Dimerisation of ethanol to butanol over solid-base catalysts. A.S.Ndou, N.J.Corille, Applied Catalysis A: General 2003, 251,337] in South Africa in 2003 [Dimerisation of ethanol to butanol over solid-base catalysts. Under, the heated nitrogen flow carries ethanol vapor condensation to make n-butanol, the problem of existence all is that reaction temperature is high, and n-butanol selectivity is low (50%)

Method used

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  • Bi-component supported catalyst of ethanol condensed n-butanol and a method of preparing thereof
  • Bi-component supported catalyst of ethanol condensed n-butanol and a method of preparing thereof

Examples

Experimental program
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Embodiment 1

[0014] Weigh 7.43 grams of nickel nitrate hexahydrate and dissolve it in 60 mL of water. After it is completely dissolved, add 36 grams of formed γ-Al with a particle size of 4-6 mm 2 o 3 After soaking for 3 days, the solution was evaporated to dryness, and then dried overnight at 130°C. Then weigh 4.87 grams of magnesium nitrate hexahydrate and dissolve it in 60 mL of water. 2 o 3 Immerse in it, evaporate the solution to dryness after immersing for 2 days, and then dry it at 130° C. to obtain a two-component supported catalyst. Put the catalyst into a tubular reactor with an inner diameter of 16 mm, fill the upper and lower parts of the reaction tube with ceramic beads, inject hydrogen gas at 80 mL / min, raise the temperature to 160 ° C for half an hour, then maintain the temperature at 260 ° C for 1 hour, and then raise the temperature to Restore at 430°C for 4 hours, continue to pass hydrogen to lower the temperature to 180°C, stop hydrogen flow, and directly pump 95% eth...

Embodiment 2

[0016] The first step is to load nickel nitrate (7.43g) on ​​the formed carrier γ-Al 2 o 3 (36g) The steps are the same as in Example 1; In the second step, take 3.20 grams of potassium fluoride dihydrate and dissolve it in 60mL of water. 2 o 3 Immerse in the potassium fluoride solution again, and the subsequent treatment is the same as the step of adding the second component in Example 1. The reaction conditions for hydrogen pretreatment before catalyst reaction and ethanol condensation are the same as in Example 1. In the presence of the catalyst, at a reaction temperature of 220° C., the conversion rate of ethanol is 15%, and the selectivity of n-butanol is 74%, as shown in the table 1.

Embodiment 3

[0018] The first step is to weigh 4.72 grams of nickel acetate tetrahydrate and dissolve it in 60 mL of water. After it is completely dissolved, add 36 grams of formed (particle size: 4-6mm) γ-Al 2 o 3 After soaking for 2 days, the solution was evaporated to dryness, and then dried at 130°C. In the second step, weigh 8.28 grams of nickel acetate tetrahydrate and dissolve it in 60 mL of water. After it is completely dissolved, dry the product obtained in the first step and then immerse it in the solution. After 2 days of immersion, the solution is evaporated to dryness, and then the drying. In the third step, 5.07 grams of magnesium nitrate hexahydrate was weighed and dissolved in 60 mL of water, and then the dried product obtained in the second step was immersed in the solution. After 2 days of immersion, the solution was evaporated to dryness. The hydrogen flow treatment of catalyzer and ethanol condensation reaction conditions are as embodiment 1. Under this catalyzer effe...

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Abstract

The invention discloses a bi-component supported catalyst of ethanol condensed n-butanol and a method of preparing thereof. The main active ingredients of the catalyst are as follows by weight percentage content: 2%-10% nickel, 0.5%-9% cocatalyst MgO or KF. The preparing method comprises the steps of: directly dipping 30-50 grams of granulose gamma-Al2O3 into nickel acetate or nickel nitrate aqueous solution with consistency being 0.5-1.0 mol / L, dipping for 2 to 4 days, occasionally stirring, evaporating, drying under 130 degrees centigrade, then dipping into magnesium nitrate or potassium fluoride aqueous solution with consistency being 0.1-1.0 mol / L for 2 to 3 days, evaporating, drying under 130 degrees centigrade to prepare the bi-component supported catalyst of ethanol condensed n-butanol. The method of preparing bi-component supported catalyst in the invention is simple and has low cost; the catalytic activity is higher than that of the single component nickel supported catalyst; the selectivity of the n-butanol in the products can achieve above 70% and has wildly industrialized application prospect.

Description

technical field [0001] The invention relates to a two-component supported catalyst for condensing ethanol into n-butanol and a preparation method thereof. Background technique [0002] N-butanol is an important chemical raw material. It is widely used in the production of dibutyl phthalate as a plastic plasticizer. It is also used in the production of medicines, spices and butylamines. n-butanol is also an important solvent. It is used in the production of fiber resin, alkyd resin and paint, and also as an excellent solvent for ethanol gasoline, which will have a large demand for energy. At present, there are two main methods for synthesizing n-butanol: one uses ethylene as a raw material to produce acetaldehyde, and then undergoes aldol condensation, followed by hydrogenation to obtain n-butanol. The process is long and uneconomical. The other is based on propylene and synthesis gas (CO+H 2 ) as the raw material, i.e. the hydroformylation of propylene (called oxo reaction...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J27/12B01J37/02C07C29/34C07C31/12
Inventor 姜玄珍杜志强
Owner ZHEJIANG UNIV
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