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Preparation and Application of a Solid Superbase Catalyst

A solid super base, catalyst technology, applied in the preparation of organic compounds, the preparation of carboxylic acid nitrile, organic chemistry and other directions, can solve the problems of high reaction temperature and long reaction time, achieve small dosage, save time and energy consumption, Easy to prepare effects

Inactive Publication Date: 2016-12-28
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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  • Preparation and Application of a Solid Superbase Catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Weigh 3.846 grams of Mg(NO 3 ) 2 ·6H 2 O and 1.876 grams of Al(NO 3 ) 3 9H 2 Dissolve O in 40mL water and 40mL ethanol to make a solution; while stirring, add 1mol / L KOH dropwise into the solution through a constant pressure funnel until the pH of the solution is 10-12, stop the dropwise addition, and continue stirring for 1h ; Heat up to 93°C in an oil bath, condense and reflux for 24 hours, centrifuge, wash with 50ml of water, dry overnight, and then place in a roasting furnace, N 2 Under protection, the room temperature was raised to 550°C at a rate of 5°C / min, and kept at 550°C for 3 hours to obtain a 10.32% potassium-doped magnesia-alumina solid superbase catalyst.

[0020] Take by weighing 0.212 gram benzaldehyde and 0.226 gram ethyl cyanoacetate respectively, add in the reaction vessel, add 1ml DMF as solvent, the solid super base catalyst that 0.019 gram present example makes is joined in the reactor; Under stirring condition, React at room temperature for...

Embodiment 2

[0022] Weigh 3.846 grams of Mg(NO 3 ) 2 ·6H 2 O and 1.876 grams of Al(NO 3 ) 3 9H 2 O was dissolved in 40mL water and 40mL ethanol to make a solution; while stirring, an excess of 1mol / L KOH was added dropwise to the solution through a constant pressure funnel until the pH of the solution was 10-12, stop the dropwise addition, and continue Stir for 1h; heat up to 93°C in an oil bath, condense and reflux for 24h, centrifuge, wash with 200ml water until neutral, dry overnight, then place in a roaster, N 2 Under protection, the room temperature was raised to 550°C at a rate of 5°C / min, and kept at 550°C for 3 hours to obtain a solid base catalyst of magnesia aluminum oxide.

[0023] Weigh 0.212 grams of benzaldehyde and 0.226 grams of ethyl cyanoacetate respectively, add to the reaction vessel, add 1ml of DMF as a solvent, and add 0.019 grams of the catalyst prepared in this example into the reactor; under stirring conditions, react at room temperature for 1 hour , filtered...

Embodiment 3

[0025] Weigh 2.564 grams of Mg(NO 3 ) 2 ·6H 2 O and 1.876 grams of Al(NO 3 ) 3 9H 2 O was dissolved in 40mL water and 40mL ethanol to make a solution; while stirring, an excess of 1mol / L KOH was added dropwise to the solution through a constant pressure funnel until the pH of the solution was 10-12, stop the dropwise addition, and continue Stir for 1h; heat up to 93°C in an oil bath, condense and reflux for 24h, centrifuge, wash with 200ml water until neutral, dry overnight, then place in a roaster, N 2 Under protection, the room temperature was raised to 550°C at a rate of 5°C / min, and kept at 550°C for 3 hours to obtain a solid base catalyst of magnesia aluminum oxide.

[0026] Weigh 0.212 grams of benzaldehyde and 0.226 grams of ethyl cyanoacetate respectively, add to the reaction vessel, add 1ml of DMF as a solvent, and add 0.019 grams of the catalyst prepared in this example into the reactor; under stirring conditions, react at room temperature for 1 hour , filtered...

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Abstract

The invention provides a preparation method of a composite metal-oxide-based solid super alkali catalyst. According to the method, magnesium nitrate and aluminum nitrate with a molar ratio of [1:1]-[7:1] are prepared into a solution; 1mol / L of NaOH or KOH is used for regulating the pH to 10-12; refluxing is carried out for 12-72h; a precipitate is washed by using water with different amounts; the precipitate is dried, and is heated to 400-700 DEG C in a tube furnace under a nitrogen atmosphere; roasting is carried out for 1-5h, such that the solid super alkali catalyst with K or Na mass content of 1-20% is obtained. According to the solid super alkali catalyst preparation method, synthesizing and modification are carried out simultaneously, wherein modification object K or Na and carrier magnesium-aluminum oxide are simultaneously produced during the roasting process, such that time and energy consumption are saved. When the catalyst is applied in a Knoevenagel condensation reaction, catalyst dose is low, reaction conditions are mild, and catalytic activity is high. The catalyst can be repeatedly used through centrifugal separation.

Description

【Technical field】 [0001] The invention relates to the field of catalysts, in particular to the preparation and application of a solid superbasic 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 is the base strength (Hammert function H - ) is greater than 26 alkaline substances, which can also be considered as neutral substances with higher intensity than (H - = 7) Higher by 19 units of alkalinity. It has been reported that H - >37 solid super base catalyst. As a catalyst, 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 product, and simple process; ( 3) The catalyst can be used repeatedly or continuously; (4) It is less corrosive to the reaction equipment and the aftertreatment is simple. In add...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/04C07C253/30C07C255/41C07D307/54
Inventor 尹双凤赵进兰东辉谢军
Owner HUNAN UNIV
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