Solid super basic catalyst and preparation method and application thereof

A technology of solid super-strong base and catalyst, which is applied in chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc. It can solve the problems of high reaction temperature and long reaction time, and achieve small dosage and easy preparation performance, high catalytic activity and selectivity

Inactive Publication Date: 2010-12-29
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these catalysts have certain catalytic activity for this reaction, the required reaction temperature is high and the reaction time is long.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of magnesium-lanthanum binary composite oxide carrier:

[0024] a. Weigh 4.949 grams of Mg(NO 3 ) 2 ·6H 2 O and 2.096 g La(NO 3 ) 3 Dissolve in 25mL water to make solution A;

[0025] b. Weigh 2.806 grams of KOH and 1.797 grams of K respectively 2 CO 3 Dissolve in 26mL water to make solution B;

[0026] c. While stirring, add solution A dropwise to solution B through a constant pressure funnel until the pH of the solution is 10-11, stop adding dropwise, and continue stirring for 1 hour;

[0027] d. Transfer the mixed solution into a crystallization kettle, and crystallize at 100°C for 16 hours;

[0028] e. Centrifuge the crystallized product, dry it, then heat it up from room temperature to 650°C at 10°C / min in a roasting furnace, and keep it at 650°C for 3 hours.

[0029] Preparation of composite metal oxide-based novel solid superbase catalyst:

[0030] Weigh 0.171 grams of potassium hydroxide and 0.855 grams of the magnesium-lanthanum binary com...

Embodiment 2

[0033] Weigh 0.184 grams of potassium fluoride and 0.569 grams of the magnesium-lanthanum binary composite oxide prepared in Example 1 respectively, place them in a mortar, add water and grind them, dry them, grind them again, and finally place them in a roasting furnace at N 2 Under the atmosphere, the temperature was raised to 500°C at a heating rate of 5°C / min, and then calcined for 4 hours to obtain a solid superbase catalyst.

[0034] Weigh respectively 0.196 gram of methanol and 0.312 gram of acrylonitrile, add in the reaction vessel, add 0.026 gram of the solid superbase catalyst prepared in this example into the reactor; under stirring condition, react at room temperature for 2 hours, filter, and the It is separated from the reaction liquid, and the reaction liquid is analyzed by gas chromatography. The conversion rate of acrylonitrile is 98.8%, and the selectivity of the product is greater than 99.0%.

Embodiment 3

[0036] Weigh respectively 0.232 grams of potassium nitrate and 1.160 grams of the magnesium-lanthanum binary composite oxide carrier prepared in Example 1, place them in a mortar, add water and grind them, dry them, grind them again, and finally place them in a roasting furnace at N 2 Under the atmosphere, the temperature was raised to 500° C. at a rate of 5° C. / min, and then calcined for 4 hours to obtain the catalyst.

[0037] Weigh respectively 0.192 gram of methanol and 0.314 gram of acrylonitrile, add in the reaction vessel, add 0.026 gram of the solid superbase catalyst prepared in this example into the reactor; under stirring condition, react at room temperature for 2 hours, filter, and the It is separated from the reaction liquid, and the reaction liquid is analyzed by gas chromatography. The conversion rate of acrylonitrile is 98.5%, and the selectivity of the product is greater than 99.0%.

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PUM

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Abstract

The invention discloses a novel compound metallic oxide base solid super basic catalyst, comprising 60-93 wt% of Mg-La binary composite oxide and 7-40 wt% of modified component, wherein Mg-La binary composite oxide comprises 11-33 wt% of magnesium oxide and 67-89 wt% of lanthanum oxide, and the modified component is potassium hydroxide, potassium nitrate, potassium fluoride or sodium hydroxide. The invention also provides a preparation method and the catalysis application thereof of the novel solid super basic catalyst. The solid super basic catalyst provided by the invention has simple component, high catalytic activity and simple and easy preparation; when applied to catalytic cyanogen ethylation reaction, the solid super basic catalyst has small catalyst dosage, does not corrode a reactor, has moderate reaction condition and belongs to an environmentally-friendly catalyst. After the reaction ends, the catalyst can be reused for several times by centrifugal separation.

Description

【Technical field】 [0001] The invention relates to the technical field of catalysis and organic chemical synthesis, in particular to the preparation and application of a novel solid superbase catalyst. 【Background technique】 [0002] Solid base refers to a solid that can chemically adsorb acidic substances or that can change the color of an acid indicator. A solid superbase refers to an alkaline substance whose base strength (Hammert's function H-) is greater than 26, and can also be considered as an alkaline substance whose strength is 19 units higher than that of a neutral substance (H_=7). It has been reported that a solid superbase catalyst with H_>37 has been found. As a catalyst, the solid superbase shows excellent performance in various reactions: (1) high catalytic activity and mild reaction conditions; (2) high selectivity, high product purity, easy separation from the product, and simple process; ( 3) The catalyst can be used repeatedly or continuously; (4) The...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/25B01J27/12B01J23/10C07C255/13C07C253/30
Inventor 尹双凤韦玉丹罗胜联张树国邱仁华
Owner HUNAN UNIV
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