Magnetic copper and bismuth catalyst and preparation method thereof

A copper-bismuth catalyst and catalyst technology are applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., which can solve the problems of difficult separation of catalysts, and achieve the effects of shortening production cycle, simple and easy operation, and uniform particle size.

Active Publication Date: 2014-10-01
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the problem that the catalyst is difficult to separate, the present invention provides a magnetic copper-bismuth catalyst and a preparation method thereof

Method used

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  • Magnetic copper and bismuth catalyst and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: the preparation method of magnetic copper-bismuth catalyst of the present invention comprises the following steps:

[0021] (1) Take 0.015m2ol Fe(NO 3 ) 3 9H 2 O, 0.12mol of sodium acetate, dissolved in 100mL of ethylene glycol, configuration Fe 3+ Concentration is 0.15mol / L, Na + Ethylene glycol solution with a concentration of 1.2 mol / L was placed in a hydrothermal kettle, reacted at 150°C for 24 hours, cooled to room temperature, and the generated Fe 3 o 4 Perform magnetic separation, wash several times with distilled water, and dry in a vacuum oven at 40°C; the obtained Fe 3 o 4 The grain size is 30nm;

[0022] (2) Weigh 6.07g Cu(NO 3 ) 2 ·3H 2 O, 0.21g Bi(NO 3 ) 3 ·5H 2 O, 15.90g Mg(NO 3 ) 2 ·6H 2 O, dissolved in water, prepared into a mixed solution with a total concentration of metal ions of 0.5mol / L;

[0023] (3) Take 11.50g tetraethyl orthosilicate and configure SiO 2 Concentration is the ethanol solution of 2.0mol / L, add the Fe ...

Embodiment 2

[0026] Embodiment 2: the preparation method of magnetic copper-bismuth catalyst of the present invention comprises the following steps:

[0027] (1) Take 0.015mol Fe(NO 3 ) 3 9H 2 O, 0.12mol of sodium acetate, dissolved in 100mL of ethylene glycol, configuration Fe 3+ Concentration is 0.15mol / L, Na+ Ethylene glycol solution with a concentration of 1.2 mol / L was placed in a hydrothermal kettle, reacted at 180°C for 24 hours, cooled to room temperature, and the generated Fe 3 o 4 Perform magnetic separation, wash several times with distilled water, and dry in a vacuum oven at 60°C; the obtained Fe 3 o 4 The grain size is 35nm;

[0028] (2) Weigh 6.07g Cu(NO 3 ) 2 ·3H 2 O, 0.21g Bi(NO 3 ) 3 ·5H 2 O, 15.90g Mg(NO 3 ) 2 ·6H 2 O is dissolved in water and prepared into a mixed solution with a total concentration of metal ions of 1.0 mol / L;

[0029] (3) Take 11.50g tetraethyl orthosilicate and configure SiO 2 Concentration is the ethanol solution of 1.8mol / L, add the ...

Embodiment 3

[0032] Embodiment 3: the preparation method of magnetic copper-bismuth catalyst of the present invention comprises the following steps:

[0033] (1) Take 0.03mol of FeCl 3 9H 2 O, 0.24mol of sodium acetate, dissolved in 150mL of ethylene glycol, configuration Fe 3+ Concentration is 0.2mol / L, Na + Ethylene glycol solution with a concentration of 1.6mol / L was placed in a hydrothermal kettle, reacted at 180°C for 20h, cooled to room temperature, and the formed Fe 3 o 4 Perform magnetic separation, wash several times with distilled water, and dry in a vacuum oven at 60°C; the obtained Fe 3 o 4 The grain size is 40nm;

[0034] (2) Weigh 5.36g CuCl 2 2H 2 O, 0.27g BiCl 3 , 10.08g MgCl 2 ·6H 2 O, dissolved in water, prepared into a mixed solution with a total concentration of metal ions of 1.5mol / L;

[0035] (3) Take 9.5g ethyl orthosilicate and configure SiO 2 Concentration is the ethanol solution of 1.2mol / L, adds the Fe prepared in 1.5g (1) 3 o 4 , ultrasonically di...

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Abstract

The invention provides a magnetic copper and bismuth catalyst and a preparation method of the magnetic copper and bismuth catalyst. The catalyst uses Fe3O4-MgO-SiO2 as a carrier, wherein the content of CuO is 20-40 wt%, the content of Bi2O3 is 1-5 wt%, the content of Fe3O4 is 8-30 wt%, the content of SiO2 is 20-46 wt%, and the content of MgO is 2-25 wt%. The preparation method comprises the following steps: placing a mixed solution consisting of a trivalent iron salt, glycol and sodium acetate in a hydrothermal kettle, reacting to obtain Fe3O4; preparing a mixed water solution containing a copper salt, a bismuth salt and a magnesium salt; ultrasonically dispersing the prepared Fe3O4 in an ethanol solution of an organic silicon source to form a turbid liquid; dropwise adding the prepared mixed solution in the turbid liquid; adjusting the pH value by using an alkali liquor to obtain a mixed precipitate, centrifuging, washing, further ageing, washing, drying and roasting in an inert atmosphere to obtain the catalyst. The catalyst is applied to the reaction of synthesizing 1,4-butynediol through ethinylation of formaldehyde, has high catalytic activity and selectivity, and can be effectively separated under the action of an applied magnetic field.

Description

technical field [0001] The invention relates to a catalyst, in particular to a magnetic copper-bismuth catalyst used for synthesizing 1,4-butynediol by acetylation of formaldehyde and a preparation method thereof. Background technique [0002] 1,4-butynediol is usually synthesized by the Reppe method, that is, formaldehyde and acetylene react under the action of a catalyst to generate 1,4-butynediol. A large number of experiments have proved that the alkyne compounds of groups I B and II B in the periodic table of elements are active in catalyzing the ethynylation of formaldehyde, and the catalyst with CuO as the main active component has the most ideal effect. In addition, adding Bi 2 o 3 Can improve the specific surface area, selectivity and activity of the catalyst, at the same time, Bi 2 o 3 It can also inhibit the formation of acetylene oligomers. [0003] The copper-bismuth catalysts reported in previous patents are divided into two types: unsupported catalysts and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/843C07C33/046C07C29/42
Inventor 赵永祥李海涛王俊俊孙自瑾骆彩萍刘绍波
Owner SHANXI UNIV
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