Copper bismuth catalyst and preparation method thereof

A copper-bismuth catalyst and catalyst technology, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problem that copper species cannot be converted into active center alkyne copper complexes, poor dispersion of active components, and catalysts Serious wear and other problems, to achieve the effect of improving effective utilization, promoting dispersion and prolonging service life

Active Publication Date: 2012-09-12
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the lack of support, the dispersion of the active components of these two catalysts is poor, and the effective utilization rate is low; more importantly, the wear of the catalyst is serious, and the active components are easy to lose, resulting in a short catalyst life.
[0008] Patent US3920759 reports a supported catalyst with magnesium silicate as a carrier. The carrier increases the dispersion of active components and the wear resistance of the catalyst, but the strong interaction between magnesium silicate and copper species makes it difficult for CuO to be Effective activation, some copper species cannot be converted into active center alkyne copper complexes; on the other hand, this method must first prepare magnesium silicate carrier, and then use impregnation method to load active components, which increases the operation process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1: take by weighing 7.59g Cu(NO 3 ) 2 ·3H 2 O, 0.42g Bi(NO 3 ) 3 ·5H 2 O, 3.18g Mg(NO 3 ) 2 ·6H 2 0 and 3.00g of glucose are prepared into 100mL mixed aqueous solution; 24.81mL tetraethyl orthosilicate is prepared into 100mL ethanol solution and the solution is slowly added dropwise to the above-mentioned mixed solution at 40°C with stirring, and then mixed with 0.02g / Adjust the pH value of the solution to 8.0 with mL NaOH solution, age for 2 hours, and separate the mixed precipitate. Use a solution with a glucose content of 0.03g / mL to wash the precipitate by centrifugation for 3 times, dry at 80°C, and roast at 300°C in a nitrogen atmosphere. 6h, get 25wt%CuO, 2wt%Bi 2 o 3 , 3wt%C, 5wt%MgO and 65wt%SiO 2 Catalyst No. 1. The particle size range of the catalyst is 50~80μm, and the specific surface area is 242m 2 / g, CuO grain size is 5nm.

Embodiment 2

[0028] Embodiment 2: take by weighing 7.59g Cu(NO 3 ) 2 ·3H 2 O, 0.42g Bi(NO 3 ) 3 ·5H 2 O, 3.18g Mg(NO 3 ) 2 ·6H 2 0 and 3.00g of glucose are prepared into 100mL mixed aqueous solution; 24.81mL tetraethyl orthosilicate is prepared into 100mL ethanol solution and the solution is slowly added dropwise to the above-mentioned mixed solution at 90°C with stirring, and then mixed with 0.03g / mL NaOH, 0.03g / mLNa 2 CO 3 and 0.03g / mL (NH 4 ) 2 CO3 The pH value of the mixed lye solution was adjusted to 10.0, aged for 3 hours, and the mixed precipitate was separated, and the precipitate was centrifuged and washed 3 times with a solution with a glucose content of 0.03g / mL, dried at 80°C, and nitrogen atmosphere at 600°C Roasted for 2h to get 25wt%CuO, 2wt%Bi 2 o 3 , 3wt%C, 5wt%MgO and 65wt%SiO 2 Catalyst No. 2. The particle size range of the catalyst is 56~92μm, and the specific surface area is 222m 2 / g, CuO grain size is 8nm.

Embodiment 3

[0029] Embodiment 3: take by weighing 5.75g CuCl 2 2H 2 O, 0.41g BiCl 3 , 5.04g MgCl 2 ·6H 2 0 and 5.00g sucrose to make 100mL mixed aqueous solution, measure 18.56mL orthosilicate methyl ester to make 100mL ethanol solution and slowly add the solution dropwise to the above mixed aqueous solution at 50°C with stirring, then use 0.05g / mL ammonium carbonate solution to adjust the pH value of the solution to 9.0, age for 4h, separate the mixed precipitate, use a solution with a sucrose content of 0.05g / mL to centrifugally wash the precipitate 4 times, dry at 100°C, and place in a helium atmosphere at 350°C Roasting for 5h to get 30wt%CuO, 3wt%Bi 2 o 3 , 4wt%C, 10wt%MgO and 53wt%SiO 2 Catalyst No. 3. The particle size range of the catalyst is 56~93μm, and the specific surface area is 213m 2 / g, CuO grain size is 6nm.

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Abstract

The invention relates to a copper bismuth catalyst for combining chemically into 1, 4-butynediol with formaldehyde and ethyne and a preparation method thereof. The preparation method comprises the following steps of: preparing mixed solution which contains copper salt, bismuth salt, magnesium salt and dispersant; dropping alcoholic solution with an organic silicon source into the mixed solution; adjusting a pH value of the mixed solution with alkaline solution to obtain mixed precipitate; and further aging, washing, drying and baking in inert atmosphere to obtain the copper bismuth catalyst with C-MgO-SiO2 a carrier, in the catalyst, the content of CuO accounts for 25-50 weight percent, and the content of Bi2O3 accounts for 2-6 weight percent. The catalyst is applied in a reaction of combining chemically into 1, 4-butynediol with formaldehyde and ethyne, and has high catalytic activity and high selectivity.

Description

technical field [0001] The invention relates to a copper-bismuth catalyst, in particular to a copper-bismuth catalyst for acetylene synthesis of formaldehyde to 1,4-butynediol and a preparation method thereof. Background technique [0002] The synthesis of 1,4-butynediol by formaldehyde ethynylation is a classic route to generate 1,4-butynediol, and the reaction process is shown in the following formula: [0003] HCHO+C 2 h 2 →HOCH 2 C≡CH [0004] HOCH 2 C≡CH+HCHO→HOCH 2 C≡CCH 2 Oh [0005] The catalyst used in this process is a copper-bismuth catalyst, in which copper species is the active component and bismuth is the auxiliary agent. During the reaction of the catalyst, the active component CuO is first reduced by HCHO, and the reduced Cu + further with C 2 h 2 The action forms the active center of the alkyne copper complex, and Bi is used to inhibit the reduction process of Cu 0 formation, thereby preventing the polymerization of acetylene to form polyyne. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/843C07C33/046C07C29/42
Inventor 赵永祥郑艳李海涛王韶安
Owner SHANXI UNIV
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