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 p

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

Example Embodiment

[0050] Example 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 a beaker (where the mass percentage of the metal catalyst in the modified molecular sieve catalyst is 4.95%), add 1000ML deionized water, stir to dissolve to prepare an aqueous solution, pour the aqueous solution into the molecular sieve carrier ( Among them, the mass percentage of HZSM-5 molecular sieve is 40%, and the binder alumina is 60%; the HZSM-5 molecular sieve has a silicon-to-aluminum molar ratio of 100). Stir and immerse for 24 hours. After drying at 130°C, it is ground for 60%. The mesh sieve is mechanically formed into a spherical shape, put into a muffle furnace at 550°C for 4 hours, and then taken out and cooled in a desiccator to prepare 20 mesh solid particles to obtain the modified molecular sieve catalyst.

[0052] About 100ml of the above-mentioned modified molecular sieve catalyst is loa...

Example Embodiment

[0054] Example 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) are placed in a beaker (where the mass percentage of the metal catalyst in the modified molecular sieve catalyst is 4.16%), add 1000ML deionized water, stir to dissolve to prepare an aqueous solution, Pour the aqueous solution into a beaker containing a molecular sieve carrier (among which, the mass percentage of HZSM-5 molecular sieve is 40%, the binder alumina is 60%; the HZSM-5 molecular sieve has a silicon-to-aluminum molar ratio of 100), stirred and immersed for 24 hours After drying at 130°C, it is ground through a 60 mesh sieve, mechanically shaped into a spherical shape, put into a muffle furnace at 550°C for 4 hours, taken out and cooled in a desiccator to make 20 mesh solid particles, which is the modified molecular sieve catalyst .

[0056] Take about 100ML of modified molecular sieve catalyst and load the ...

Example Embodiment

[0058] Example 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 a beaker (where the mass percentage of the metal catalyst in the modified molecular sieve catalyst is 4.19%), add 1000ML deionized water, stir to dissolve to prepare an aqueous solution, pour the aqueous solution into the molecular sieve carrier ( Among them, the mass percentage of HZSM-5 molecular sieve is 40%, and the binder alumina is 60%; the molar ratio of silicon to aluminum of HZSM-5 molecular sieve is 150) in a beaker, stirring, immersing for 24 hours, drying at 130°C, and grinding through a 60 mesh sieve , Mechanically into a spherical shape, put it in a muffle furnace at 550°C for 4 hours, take it out and cool it in a desiccator to make 20 mesh solid particles, which is the modified molecular sieve catalyst.

[0060] Take about 100ml of the modified molecular sieve catalyst and load...

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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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