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Organic-inorganic hybrid solid super strong alkali and preparation method thereof

A solid super base and catalyst technology, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve limited applications, complex processes, equipment, and preparation steps cumbersome and other problems, to achieve the effect of high selectivity and easy operation

Inactive Publication Date: 2009-08-12
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantages of these two methods are: both require high vacuum and high temperature devices, and the process and equipment are complicated.
The third preparation method is to dissolve metal K in liquid ammonia and impregnate it on the carrier, so that potassium can be dispersed to obtain a solid super alkali. On the one hand, this preparation method is due to the corrosion of equipment by liquid ammonia, and the volatile ammonia will bring Environmental pollution limits its application. On the other hand, the preparation steps are cumbersome, which is not conducive to industrial application

Method used

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  • Organic-inorganic hybrid solid super strong alkali and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] in N 2 Quickly cut 0.05g of metal potassium from the stream, add it to a three-necked bottle containing 10ml of n-hexane, heat and stir to 75°C under the protection of high-purity nitrogen, and keep it for about 1h. At this time, K is in hexane Disperses as tiny blue particles. Add 0.95g of hydrotalcite activated in a nitrogen stream at 500°C to the hexane with K dispersed, the activation time is 2 hours, stir, and evaporate the excess n-hexane at 80°C to form a blue powder K n R / MgAl(O) samples. in N 2 Add 20ml of benzaldehyde solution that has been purified and dried beforehand under the protection of Stir and react at 140°C. After 30 minutes, the product is taken out for analysis. The yield of benzyl benzoate is 63.5%, and the selectivity is 97.4%.

Embodiment 2

[0028] in N 2 Quickly cut 0.1g of metal potassium from the stream, add it to a three-necked bottle containing 10ml of n-hexane, heat and stir to 75°C under the protection of high-purity nitrogen, and keep it for about 1h. At this time, K is in hexane Disperses as tiny blue particles. Add 0.9g of hydrotalcite activated in a nitrogen stream at 500°C to the hexane dispersed with K, the activation time is 2 hours, stir, and evaporate excess n-hexane at 80°C to produce blue powder K n R / MgAl(O) samples. in N 2 Add 20ml of benzaldehyde solution that has been purified and dried beforehand under the protection of Stir and react at 140°C. After 30 minutes, the product is taken out for analysis. The yield of benzyl benzoate is 75%, and the selectivity is 99.9%.

Embodiment 3

[0030] in N 2 Quickly cut 0.2g of metered metal potassium from the stream, add it to a three-necked bottle containing 10ml of n-hexane, heat and stir to 75°C under the protection of high-purity nitrogen, and keep it for about 1h. At this time, K is in hexane Disperses as tiny blue particles. Add 0.8 g of K dispersed in hexane and activate (2h) the hydrotalcite at 773K in a nitrogen stream. Stir and steam excess n-hexane at 80°C to produce blue powder K n R / MgAl(O) samples. in N 2 Add 20ml of benzaldehyde solution that has been purified and dried beforehand under the protection of Stir and react at 140°C. After 30 minutes, the product is taken out for analysis. The yield of benzyl benzoate is 99.8%, and the selectivity is 100%.

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Abstract

The invention discloses a highly active organic-inorganic hybrid solid superbase catalyst and a preparation method thereof. The catalyst comprises organic potassium metal clusters and a porous carrier, and the characteristic molecular formula is: KnR / MO, wherein K is an alkali metal Potassium, n is the degree of polymerization n=1-6, R is an alkyl group containing C6-C8 carbon atoms, and MO is a porous carrier. The invention loads organic potassium on a porous carrier in low-carbon straight-chain alkanes near the boiling point of potassium to form organic potassium cluster solid superbase. The solid superbase has extremely high activity and selectivity for base-catalyzed reactions such as solvent-free Tishchenko reaction and olefin isomerization. And without activation, it can be directly used to catalyze organic reactions. The method does not pollute the environment, is simple to operate, does not require high temperature and high vacuum, and the hexane can be recovered and recycled. This organic-inorganic composite catalytic material has great application prospects and economic value.

Description

1. Technical field [0001] The invention relates to a high-activity environment-friendly solid base catalyst, in particular to a high-activity organic-inorganic hybrid solid superbase catalyst and a preparation method thereof. . 2. Background technology [0002] Environmental pollution is a global problem that threatens human existence, and it is also a challenge for chemical research in the 21st century. The modern chemical process requires a pollution-free, zero-emission, and efficient green production process. With the development of industry and the enhancement of people's awareness of environmental protection, basic catalysis is required to gradually transition from a liquid homogeneous catalysis process to a heterogeneous catalysis process. Since solid base is an environmentally friendly catalyst, it can be used with high efficiency under mild conditions. It catalyzes reactions such as alkylation, condensation and isomerization, and is widely used in fine chemical ind...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/12
Inventor 王英刘健韩小伟季安史丽英高玲
Owner NANJING UNIV
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