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Catalyst for producing piperazidine and triethylenediamine and preparation method thereof

A triethylenediamine and catalyst technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of low selectivity of triethylenediamine, total yield of piperazine and triethylenediamine products Low efficiency and other problems, to achieve the effect of good industrial development prospects, good life, high selectivity

Inactive Publication Date: 2013-08-14
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] The present invention solves the shortcomings of low triethylenediamine selectivity and low total yield of piperazine and triethylenediamine products in previous literatures, and provides a novel method for producing synthetic piperazine and triethylenediamine from ethanolamine or diethanolamine. Amine catalyst and preparation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] H-ZSM-5 (silicon-aluminum ratio: 20) was steam-treated at 400°C for 4h, then the steam-treated H-ZSM-5 was soaked in NaOH solution with a concentration of 0.1mol / L for 0.5h, and then filtered without Wash to dry. Then the processed carrier was calcined in a muffle furnace at 800° C. for 4 hours. Prepare a solution of strontium nitrate with a concentration of 1mol / L, take 50ML of the above-prepared solution and add it to a beaker, weigh 10g of the treated H-ZSM-5 molecular sieve and add it to a straight condenser tube, and seal the upper and lower ends with filter paper , then both ends were plugged with stainless steel tube rubber stoppers, and the prepared solution was connected to the stainless steel tubes at both ends through the rubber tube through the peristaltic pump, and circulated into the inner shell of the condenser tube containing ZSM-5, and the solution feed rate was 10ml / h. The processing time is 10h. The shell of the condenser tube is heated by an oil ba...

Embodiment 2

[0036] H-ZSM-5 (silicon-aluminum ratio: 20) was steam-treated at 400°C for 4h, then the steam-treated H-ZSM-5 was soaked in NaOH solution with a concentration of 0.1mol / L for 0.5h, and then filtered without Wash to dry. Then the processed carrier was calcined in a muffle furnace at 800° C. for 4 hours. Prepare a solution of strontium nitrate with a concentration of 1mol / L, add 50ml of the above-prepared solution into a beaker, weigh 20g of the treated H-ZSM-5 molecular sieve and add it to a straight condenser tube, and seal the upper and lower ends with filter paper , then both ends are plugged with stainless steel tube rubber stoppers, and the prepared solution is connected to the stainless steel tubes at both ends through the rubber tube through a peristaltic pump, and circulated into the inner shell of the condenser tube containing ZSM-5, and the solution feed rate is 20ml / h. The processing time is 10h. The shell of the condenser tube is heated by an oil bath with a circu...

Embodiment 3

[0039] H-ZSM-5 (silicon-aluminum ratio: 20) was steam-treated at 400°C for 4h, then the steam-treated H-ZSM-5 was soaked in NaOH solution with a concentration of 0.1mol / L for 0.5h, and then filtered without Wash to dry. Then the processed carrier was calcined in a muffle furnace at 800° C. for 4 hours. Prepare a solution of strontium nitrate with a concentration of 1mol / L, take 50ML of the above-prepared solution and add it to a beaker, weigh 10g of the treated H-ZSM-5 molecular sieve and add it to a straight condenser tube, and seal the upper and lower ends with filter paper , then both ends were plugged with stainless steel tube rubber stoppers, and the prepared solution was connected to the stainless steel tubes at both ends through the rubber tube through the peristaltic pump, and circulated into the inner shell of the condenser tube containing ZSM-5, and the solution feed rate was 10ml / h. The processing time is 10h. The shell of the condenser tube is heated by an oil ba...

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Abstract

The invention relates to a catalyst for producing piperazidine and triethylenediamine and a preparation method thereof, and belongs to the technical field of a zeolite molecular sieve catalyst. The preparation method comprises the following steps of: sequentially carrying out water vapor treatment, NaOH solution soaking, 600-800 DEG C roasting on H-ZSM-5; then adding to a straight type condensation tube; sealing both ends of a molecular sieve by respectively using filter papers; plugging rubber plugs with stainless steel tubes on both ends of the condensation tube; circularly accessing a metal nitrate solution into the condensation tube through a peristaltic pump; carrying out 60-110 DEG C oil bath on the shell of the condensation tube; taking out the molecular sieve, carrying out suction filtration, placing a filter cake into a quartz glass tube, placing into liquid nitrogen in a sealing way, and taking out the filter cake for drying; and placing into muffle furnace for roasting. The catalyst disclosed by the invention keeps high selectivity on the triethylenediamine, keeps the activity still good with the change of time and has long life.

Description

technical field [0001] The present invention relates to a zeolite molecular sieve catalyst and preparation method for producing piperazine and triethylenediamine, in particular, relates to a synthetic production of piperazine and triethylenediamine with amine compounds (ethanolamine, diethanolamine) A catalyst and a preparation method thereof belong to the technical field of zeolite molecular sieve catalysts. Background technique [0002] Piperazine, also known as piperazine and hexahydropyrazine, is an important pharmaceutical intermediate, mainly used in the production of anthelmintic drugs piperazine phosphate, piperazine citrate, as well as tranquilizers, tradine, rifampicin , as well as synthetic applications for some antibacterial drugs (norfloxacin, ciprofloxacin). Dissolve piperazine hexahydrate in ethanol, add glacial acetic acid to stir and cool to precipitate piperazine acetate, which is used to synthesize hormone drug prednisolone sodium phosphate. Piperazine h...

Claims

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Application Information

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IPC IPC(8): C07D487/08C07D295/023B01J29/46B01J29/40C07D295/027
Inventor 黄崇品张亮李英霞陈标华臧杰
Owner BEIJING UNIV OF CHEM TECH
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