Anhydrous piperazine preparation method

An anhydrous piperazine and a part of the technology, which is applied in the field of preparation of anhydrous piperazine by catalytic hydrogenation of iminodiacetonitrile, can solve the problems of loss of active components of the catalyst, fast deactivation and short life, and achieve the goal of not being easily deactivated , less by-products, long service life

Active Publication Date: 2013-03-06
WANHUA CHEM GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a kind of preparation method of anhydrous piperazine, has solved the shortcomings such as the catalyst active component loss that adopts organic acid treat

Method used

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  • Anhydrous piperazine preparation method

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0040] Carrier preparation

[0041] Carrier 1: Preparation of Mo-ZSM-5 molecular sieve

[0042] Weigh 40g of dried ZSM-5 molecular sieve (silica-aluminum ratio 30-40); weigh 1.2g of ammonium molybdate and dissolve it in 60ml of purified water to prepare an ammonium molybdate solution, and pour the solution into the above-mentioned ZSM-5 In the molecular sieve, after uniformly stirring, stand for 12 hours, dry at 120°C, and activate at 550°C for 4 hours to obtain a modified Mo-ZSM-5 molecular sieve. Through the analysis of the aforementioned method, the highest acid strength on the surface of Mo-ZSM-5 molecular sieve is shown in Table 1.

[0043] Carrier 2: Fe-ZSM-5 molecular sieve preparation

[0044] Weigh 40g of dried ZSM-5 molecular sieve (silica-to-aluminum ratio 30-40); weigh 4.25g ferric nitrate nonahydrate and dissolve it in 60ml purified water to prepare ferric nitrate dipping solution, and slowly pour the solution into the above-mentioned dry In the ZSM-5 molecular sieve, a...

Example Embodiment

[0056] Example 1

[0057] The hydrogenation reactor is a stainless steel tubular reactor of φ25mm×1500mm, and the upper part of the reaction tube is filled with 80ml of catalyst one with a particle size of 0.6-1mm. The catalyst was reduced by a mixture of hydrogen and nitrogen (volume ratio 1:10) under normal pressure at 600°C for 3 hours before use.

[0058] Take an appropriate amount of iminodiacetonitrile (IDAN) and 2760ml of tetrahydrofuran (THF) with a water content of 1000 ppm and mix them and dissolve by heating. After the measurement, the concentration of IDAN is 22wt%, and it is fed into the reactor at a set speed from the top to keep the addition of IDAN The amount is 9g / h, and another pipeline is set to supply 42 standard liters / h of hydrogen. After the raw material is mixed with hydrogen, it enters the bed containing the catalyst for hydrogenation-cyclization reaction. The reaction temperature is 75℃, and the reaction pressure is 6Mpa. The reaction liquid is collected...

Example Embodiment

[0059] Example 2

[0060] The hydrogenation reactor is a stainless steel tubular reactor of φ25mm×1500mm, 80ml of catalyst 3 with a particle size of 0.6-1mm is taken, and the bottom of the reaction tube is filled with inert quartz sand. The catalyst was reduced under normal pressure with a mixture of hydrogen and nitrogen (volume ratio 1:10) at 600°C for 3 hours before use.

[0061] Take an appropriate amount of iminodiacetonitrile (IDAN) and 5500ml of tetrahydrofuran (THF) with a water content of 1%, mix and heat to dissolve. After the measurement, the concentration of IDAN is 15%, and it is fed into the reactor at a set speed from the top to keep the addition of IDAN. The amount is 15g / h, and another pipeline is set to supply 50.5 standard liters / h of hydrogen. The raw materials and hydrogen are mixed and enter the bed containing the catalyst for hydrogenation-cyclization reaction. The reaction temperature is 90℃, and the reaction pressure is 4Mpa. The reaction liquid is collec...

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Abstract

The invention relates to an anhydrous piperazine preparation method. The method comprises the following steps: a hydrogenation reactor is adopted to dissolve iminodiacetonitrile in an organic solvent, iminodiacetonitrile and hydrogen undergo a hydrogenation-cyclization reaction at 70-110DEG C under 1-10Mpa in the presence of a supported catalyst, and the obtained reaction solution is purified to obtain the anhydrous piperazine and simultaneously obtain polyene polyamine which is a byproduct, wherein the supported catalyst comprises an active component, assistant elements and an acidic supporter, the active component comprises one or more of Fe, Co, Ni, Ru or Rh, and preferably Co and/or Ni, the mass of the active component is 10-60wt% of the mass of the supporter, and the mass of the assistant elements is 0-10wt% of the mass of the supporter. Piperazine is obtained in a high yield manner through the method, and the highest piperazine yield can reach above 90%.

Description

technical field [0001] The invention relates to a method for preparing anhydrous piperazine, in particular to a method for preparing anhydrous piperazine by catalytic hydrogenation of iminodiacetonitrile. Background technique [0002] Piperazine is a fatty diamine with a six-membered ring. It is an important pharmaceutical and chemical intermediate. Drugs synthesized from piperazine mainly include antibiotics, stable analgesics, and anthelmintics. It can also be used to manufacture dyestuffs, Surfactants, sulfur accelerators, anti-corrosion and antioxidants, etc. Its industrial products are divided into four specifications: anhydrous piperazine, trihydrate piperazine, hexahydrate piperazine and hexapentapiperazine (65% content), among which anhydrous piperazine has the highest value and the most widely used. [0003] The current source of piperazine, as described in "Kirk-Othmer Encyclopedia of Chemical Technology" Vol.8DIAMINES AND HIGHER AMINES, ALIPHATIC, P493, is mainly...

Claims

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Application Information

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IPC IPC(8): C07D295/027C07D295/023
Inventor 李付国黎源丁可赵文娟华卫琦
Owner WANHUA CHEM GRP
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