Modified molecular sieve catalyst for piperidine preparation, preparation method and applications thereof

A molecular sieve and catalyst technology, which is applied in the field of modified molecular sieve catalysts, can solve the problems of no large-scale industrial production, difficulties in product refining and recycling, and expensive catalysts, so as to suppress high-boiling point by-products, improve catalytic activity, and reduce waste. Effect

Active Publication Date: 2015-08-19
CATHAY (JINXIANG) BIOMATERIAL CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the method for the synthesis of piperidine by the above-mentioned catalyst, adopting silica gel as the fixed-bed gas-solid phase reaction of the catalyst has a low yield and a large amount of high-boiling point by-products, which brings great difficulties to the refining and recovery of the product, and improves the production efficiency of the product. Production cost; although the yield of piperidine synthesis method with noble metal as catalyst has been improved, the catalyst is expensive, the reaction conditions are harsh, and there is no potential for large-scale industrial production

Method used

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  • Modified molecular sieve catalyst for piperidine preparation, preparation method and applications thereof
  • Modified molecular sieve catalyst for piperidine preparation, preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Weigh Fe(NO 3 ) 3 9H 2 O (60.60g, 150.0mmol), Mn (NO 3 ) 2 4H 2 O (2.01g, 8.0mmol), Ca (NO 3 ) 2 .4H 2 O (1.53g, 6.5mmol) and KNO 3 (0.08g, 0.8mmol) in the beaker (wherein the mass percent of metal catalyst in the modified molecular sieve catalyst is 4.95%), add 1000ML deionized water, stirring and dissolving makes aqueous solution, this aqueous solution is poured into molecular sieve carrier ( Wherein, mass percentage HZSM-5 molecular sieve 40%, binder alumina 60%; In the beaker that the silicon-aluminum molar ratio of HZSM-5 molecular sieve is 100), stir, impregnate 24 hours, after drying at 130 ℃, grind 60 Mesh sieve, mechanically formed into spherical shape, put into muffle furnace and bake at 550°C for 4 hours, take it out and cool in desiccator to make 20-mesh solid particles to obtain modified molecular sieve catalyst.

[0052] Get about 100ml of the above-mentioned modified molecular sieve catalyst and pack it into a stainless steel reactor. The catalys...

Embodiment 2

[0055] Weigh Fe(NO 3 ) 3 9H 2 O (48.48g, 120.0mmol), Ba(NO 3 ) 2 (2.35g, 9.0mmol), Zr(NO 3 ) 4 ·5H 2 O (0.86g, 2.0mmol) and KNO3 (0.08g, 0.8mmol) in the beaker (wherein the mass percent of metal catalyst in the modified molecular sieve catalyst is 4.16%), add 1000ML deionized water, stirring and dissolving makes aqueous solution, Pour the aqueous solution into a beaker equipped with a molecular sieve carrier (wherein, the mass percent HZSM-5 molecular sieve is 40%, the binder alumina is 60%; the silicon-aluminum molar ratio of the HZSM-5 molecular sieve is 100), stirred, and soaked for 24 hours , after drying at 130°C, grind through a 60-mesh sieve, mechanically form a ball, put it into a muffle furnace and bake at 550°C for 4 hours, take it out and cool it in a desiccator, and make 20-mesh solid particles to obtain a modified molecular sieve catalyst .

[0056] Get about 100ML of the modified molecular sieve catalyst and put it into a stainless steel reactor. The cata...

Embodiment 3

[0059] Weigh Fe(NO 3 ) 3 9H 2 O (48.48g, 120.0mmol), Ba(NO 3 ) 2 (2.09g, 8.0mmol), Ga(NO 3 ) 3 (0.51g, 2.0mmol), Ce(NO 3 ) 4 (0.31g, 0.8mmol) and NaNO 3 (0.03g, 0.3mmol) in the beaker (wherein the mass percent of metal catalyst in the modified molecular sieve catalyst is 4.19%), add 1000ML deionized water, stir and dissolve and obtain aqueous solution, this aqueous solution is poured into molecular sieve carrier ( Wherein mass percent HZSM-5 molecular sieve 40%, binder aluminum oxide 60%; The silicon-aluminum molar ratio of HZSM-5 molecular sieve is 150) in the beaker, stir, impregnate 24 hours, after drying at 130 ℃, grind through 60 mesh sieves , into a spherical shape mechanically, put into a muffle furnace and roast at 550°C for 4 hours, take it out and cool it in a desiccator, and make 20-mesh solid particles to obtain a modified molecular sieve catalyst.

[0060] Get about 100ml of the modified molecular sieve catalyst and pack it into a stainless steel reactor ...

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PUM

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Abstract

The present invention discloses a modified molecular sieve catalyst for piperidine preparation, a preparation method and applications thereof, wherein the modified molecular sieve catalysts comprises 90-99.9% by mass of a molecular sieve carrier and 0.1-10% by mass of a metal catalyst, and the metal catalyst is supported on the molecular sieve carrier. According to the present invention, the molecular sieve is adopted as the catalyst carrier to prepare the high-dispersity active component supported solid catalyst, wherein the metal catalyst consumption is substantially reduced, the production cost is reduced, the catalyst exhibits high activity and high selectivity, and the target product selectivity can achieve more than or equal to 99%. Compared with the method in the prior art, the method of the present invention further has advantages of simple process, high yield, less waste and the like.

Description

technical field [0001] The invention relates to the technical field of supported solid catalysts, in particular to a modified molecular sieve catalyst for preparing piperidine and its preparation and application. Background technique [0002] Piperidine (molecular formula (CH 2 ) 5 NH, CAS No. 110-89-4), also known as hexahydropyridine, is a cyclic aliphatic secondary amine, which belongs to medium strong base. It is a colorless fuming liquid at room temperature, and has a pungent smell similar to ammonia and pepper. As a very important fine chemical intermediate, piperidine has a wide range of uses, such as the synthesis of pharmaceuticals, agricultural chemicals and rubber products. have been developed and applied. In recent years, with the expansion of piperidine's application fields, especially the emergence of a large number of new drugs containing piperidine structure, the demand for high-purity piperidine has greatly increased, and its application prospects are bro...

Claims

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Application Information

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IPC IPC(8): B01J29/48B01J29/46B01J29/78B01J29/16C07D295/027C07D295/023
Inventor 黄浩秦兵兵刘驰
Owner CATHAY (JINXIANG) BIOMATERIAL CO LTD
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