Novel nano solid super-strong alkali catalyst and preparation and application thereof

A technology of solid super-strong base and catalyst, applied in organic chemistry, etc., can solve problems such as low yield, high reaction temperature, and long reaction time, and achieve the effects of small dosage, high catalytic activity, and simple composition

Inactive Publication Date: 2013-01-30
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, the reaction time is long, and the yield is low.

Method used

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  • Novel nano solid super-strong alkali catalyst and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Weigh 0.520 g of PVP, dissolve in 50 ml of deionized water, and stir to dissolve at room temperature. According to the ratio of Sn and Mg molar ratio of 1:1, weigh 0.766 g SnCl 4 ·5H 2 O and 0.633 g Mg(NO 3 ) 2 ·6H 2 O was successively added to the above solution and stirred for 12 h. Add 0.1 mol / L KOH solution drop by drop, adjust the pH of the system to 12-14, continue to stir for 2 h, then transfer to the hydrothermal reaction kettle, set at 180 o C in a homogeneous reactor for 24 h. After the reaction, cool to room temperature, centrifuge, wash the obtained precipitate with water until the washing liquid is neutral, wash off the surfactant with ethanol, and then place it at 120 o C oven dried for 24 h. Then take out the sample, grind it, and put it in the roaster under N 2 Atmosphere, with 5 o C / min heating rate, heating up to 600 o C is calcined for 2 h to obtain the catalyst (alkali strength is 26.5≤H_<33.0, and the corresponding alkali content is as hi...

Embodiment 2

[0037] Weigh 0.508 g CTAB, dissolve it in 60 ml deionized water, and stir to dissolve at room temperature. According to the molar ratio of Sn and Mg of 1:1, weigh 0.784 g SnCl 4·5H 2 O and 0.745g Mg(NO 3 ) 2 ·6H 2 O was added to the above solution successively and stirred for 2 h. Add 0.5 mol / L NaOH solution drop by drop, adjust the pH of the system to 12-13, continue to stir for 4 h, then transfer to the hydrothermal reaction kettle, at 180 o C in a homogeneous reactor for 24 h. After the reaction, cool to room temperature, centrifuge, wash the obtained precipitate with water until the washing liquid is neutral, wash off the surfactant with ethanol, and then place it at 120 o C oven dried for 24 h. Then take out the sample, grind it, and put it in the roaster under N 2 Atmosphere, with 8 o C / min heating rate, heating up to 550 o C was calcined for 2 h to obtain the catalyst (alkali strength 26.5≤H_≤33.0, corresponding alkali amount up to 0.423mmol / g).

[0038] Tak...

Embodiment 3

[0040] Weigh 0.521 g of P123, dissolve in 50 ml of deionized water, and stir to dissolve at room temperature. According to the ratio of Sn and Mg molar ratio of 1:1, weigh 0.763 g SnCl 4 ·5H 2 O and 0.569 g Mg(NO 3 ) 2 ·6H 2 O was successively added to the above solution and stirred for 5 h. Add 0.5 mol / L KOH solution drop by drop, adjust the pH of the system to 12-13, continue to stir for 2 h, then transfer to the hydrothermal reaction kettle, at 180 o C in a homogeneous reactor for 24 h. After the reaction, cool to room temperature, centrifuge, wash the obtained precipitate with water until the washing liquid is neutral, wash off the surfactant with ethanol, and then place it at 120 o C oven dried for 24 h. Then take out the sample, grind it, and put it in the roaster under N 2 Atmosphere, with 2 o C / min heating rate, heating up to 600 o C was calcined for 2 h to obtain the catalyst (alkali strength 26.5≤H_≤33.0, corresponding alkali amount up to 0.418mmol / g).

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Abstract

The invention discloses a nano solid super-strong alkali catalyst. The nano solid super-strong alkali catalyst comprises 50 to 80 molar percent of magnesium oxide and 20 to 50 molar percent of tin oxide, and has a cubic crystal form, and the side length of the cube is 60 to 150nm. The invention also provides a preparation method of the nano solid super-strong alkali catalyst and application of the nano solid super-strong alkali catalyst in catalysis. The nano solid super-strong alkali catalyst has simple components and high catalytic activity, is easy and convenient to prepare, is present in a small amount, does not corrode a reactor and ensures mild reaction conditions when applied to the catalysis of one-pot condensation reaction, belongs to an environment-friendly catalyst, and can be used for multiple times through centrifugal separation after the reaction is finished.

Description

【Technical field】 [0001] The invention relates to the technical field of catalysis and organic chemical synthesis, in particular to a nanometer solid superbase catalyst and its preparation and application. 【Background technique】 [0002] Solid super alkali refers to solid alkaline material with alkali strength H_≥26. As a catalyst, solid superbase shows excellent effects in various reactions: (1) high catalytic activity, mild reaction conditions, and good heat resistance as an inorganic solid material; (2) extremely high selectivity, the product It has high purity, is easy to separate from the product, and has a simple process; (3) the catalyst can be reused and can also be used continuously; (4) it is less corrosive to reaction equipment and has less waste water. These advantages of solid superbases meet the requirements of the development of green chemistry. Therefore, the research on solid superbases has become one of the hotspots in the field of catalysis. [0003] Com...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D309/04
Inventor 尹双凤张树国韦玉丹罗胜联赵进周永波
Owner HUNAN UNIV
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