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A kind of preparation method of special catalyst for synthetic piperazine reaction of ethylenediamine

A technology of ethylenediamine and catalyst is applied in the field of preparation of special catalyst for ethylenediamine synthesis piperazine reaction, can solve the problems of less by-products, low production efficiency and high reaction pressure, and achieves the effect of high selectivity

Active Publication Date: 2017-10-20
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Japanese patent JP4922024 discloses a process route for preparing piperazine by hydrogenation and cyclization of hydroxyethylethylenediamine as a raw material. The method uses metal oxides such as copper, chromium, and manganese as catalysts, and has the advantages of less by-products, The yield is high, but the reaction pressure is too high, generally 6-26MPa, and it is produced intermittently, and the production efficiency is low

Method used

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  • A kind of preparation method of special catalyst for synthetic piperazine reaction of ethylenediamine
  • A kind of preparation method of special catalyst for synthetic piperazine reaction of ethylenediamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Prepare 1L ion-exchange liquid, wherein the concentrations of potassium chloride, nickel nitrate and zinc nitrate are 2mol / L, 0.1mol / L and 0.01mol / L respectively, take 300g HZSM-5 molecular sieve and dissolve in 900ml ion-exchange liquid, Exchange 20 hours;

[0038] The exchanged liquid was suction-filtered and dried at 150 degrees Celsius for 5 hours to obtain 308.7 g of powdered product;

[0039] Get 50g of powdered product, mix it with 25g sodium carboxymethylcellulose, and treat the obtained product with steam for 8 hours to make the pores in the HZSM-5 molecular sieve more uniform; then, use a concentration of 0.3mol / L The sodium hydroxide solution was soaked for 2 hours, the aluminum in the HZSM-5 molecular sieve was dissolved, suction filtered and dried to obtain 68.13g of a semi-finished catalyst;

[0040] Prepare a solution containing alumina carrier, calcium nitrate, iron nitrate and copper nitrate, the concentration of each component in the solution is 2mol / ...

Embodiment 2

[0043]Prepare 1L of ion-exchange solution, wherein the concentrations of potassium chloride, nickel nitrate and zinc nitrate are 1.5mol / L, 0.1mol / L and 0.01mol / L respectively, and 300g of HZSM-5 molecular sieves are dissolved in 1200ml of ion-exchange solution. Exchange at room temperature for 20 hours;

[0044] The exchanged liquid was suction-filtered and dried at 120 degrees Celsius for 5 hours to obtain 305.7 g of powdered product;

[0045] Get 50g of powdered product, mix it with 15g sodium carboxymethyl cellulose, and treat the obtained product with steam for 8 hours to make the pores in the HZSM-5 molecular sieve more uniform; then, use a concentration of 0.5mol / L Sodium hydroxide solution impregnated for 4 hours, the aluminum in the HZSM-5 molecular sieve was dissolved, suction filtered and dried to obtain 61.45 g of catalyst semi-finished product;

[0046] Prepare a solution containing alumina carrier, calcium nitrate, iron nitrate and copper nitrate, the concentrati...

Embodiment 3

[0049] Prepare 1L ion-exchange liquid, wherein the concentrations of potassium chloride, nickel nitrate and zinc nitrate are 1mol / L, 0.05mol / L and 0.005mol / L respectively, take 300g HZSM-5 molecular sieve and dissolve it in 1000ml ion-exchange liquid, at room temperature Exchange 20 hours;

[0050] The exchanged liquid was suction-filtered and dried at 160 degrees Celsius for 10 hours to obtain 307.3 g of powdered product;

[0051] Get 50g of powdered product, mix it with 45g sodium carboxymethyl cellulose, and treat the obtained product with steam for 8 hours to make the pores in the HZSM-5 molecular sieve more uniform; then, with a concentration of 0.8mol / L Sodium hydroxide solution impregnated for 2 hours, the aluminum in the HZSM-5 molecular sieve was dissolved, suction filtered and dried to obtain 64.83 g of catalyst semi-finished product;

[0052] Prepare a solution containing alumina carrier, calcium nitrate, iron nitrate and copper nitrate, the concentration of each c...

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Abstract

The invention relates to a method for preparing a special catalyst for the synthesis of piperazine from ethylenediamine, comprising the following steps: preparing an ion exchange liquid, adding HZSM‑5 molecular sieves to the ion exchange liquid; Mix the mixture to obtain a product of a certain shape; steam the product, soak it in a sodium hydroxide solution for a period of time, filter it, and dry it to obtain a powdery solid; prepare a product containing alumina carrier, calcium nitrate, and ferric nitrate and the solution of copper nitrate, the product obtained as a powdery solid is immersed in the solution for 6-8 hours, and then suction filtered, dried and roasted. The effect and benefit of the invention is to prepare the molecular sieve catalyst for synthesizing piperazine at low cost, so that the target product piperazine has higher selectivity.

Description

technical field [0001] The invention belongs to the field of preparation of molecular sieve catalysts, and relates to a preparation method of a special catalyst for the synthesis of piperazine from ethylenediamine. Background technique [0002] Piperazine, also known as hexahydropyrazine and piperazine, is an important organic chemical raw material. In medicine, it is mainly used to prepare quinolone antibiotics pipemidic acid, ciprofloxacin, norfloxacin and rifampicin. In terms of surfactants, it is used to synthesize emulsifiers, defoamers, dispersants, rubber vulcanization accelerators, stabilizers, antioxidants, corrosion inhibitors, foaming agents, etc. In addition, piperazine can also be used in synthetic resin, fiber and leather. In recent years, with the increasing awareness of environmental protection, piperazine has developed rapidly in the field of recycling heavy metals in wastewater and sequestering carbon. [0003] At present, the raw materials for preparing...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/46C07D295/023C07D295/027
Inventor 刘红梅郑学明尚会建
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY