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Method for preparing piperazine

A technology of piperazine and hydroxyethylpiperazine, applied in the field of preparation of piperazine, can solve the problems of low yield selectivity and high separation energy consumption, achieve high yield, improve catalytic activity, high selectivity and conversion rate Effect

Pending Publication Date: 2022-05-06
CHINA PETROLEUM & CHEM CORP +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 overcome the technical defect that the yield and selectivity are low when preparing piperazine that exists in the prior art, so that the separation energy consumption is high, and provide a kind of N-hydroxyethyl piperazine or / and N-ammonia The method for preparing piperazine from ethylpiperazine

Method used

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  • Method for preparing piperazine
  • Method for preparing piperazine
  • Method for preparing piperazine

Examples

Experimental program
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Embodiment approach

[0022] According to the present invention, the alumina precursor used in the carrier is prepared by adding silicon oxide precursor and / or molecular sieve precursor, etc., which can further greatly improve the diffusivity and pore structure stability of the catalyst after being prepared as a carrier. Therefore, according to a preferred embodiment of the present invention, the content of the alumina carrier in the carrier accounts for more than 70% by weight of the total amount of the alumina carrier and other carriers, preferably 80-97% by weight.

[0023] According to a preferred embodiment of the present invention, the content of the doping element accounts for 0.05-5% by weight of the content of the carrier, preferably 0.08-3% by weight.

[0024] According to a preferred embodiment of the present invention, the doping element in the alumina precursor of the carrier is doped with at least one of borate ions, fluoride ions, phosphate ions, sulfate ions and selenate ions. The d...

preparation example 1

[0048] Pseudoboehmite powder (specific surface area 380m 2 / g, pore volume 1.02ml / g, pseudoboehmite powder contains doping element S, relative to 100g Al 2 o 3 The calculated pseudo-boehmite powder contains 2.15g of S element; during the preparation of the pseudo-boehmite powder, SiO is added at the beginning 2 Precursor water glass (sodium silicate aqueous solution), so that after sintering, the carrier is derived from SiO 2 Precursor of SiO 2 The mass accounts for 4% of the total mass of the carrier) kneaded with dilute acid water containing 5vol% nitric acid, extruded into strips with a diameter of 5mm after kneading, cut into 4mm lengths, dried at 120°C for 8h, and then calcined at 650°C for 5h. Make the desired carrier.

[0049] 186.5g cobalt nitrate hexahydrate (industrial grade, purity 98%), 6.83g zinc nitrate hexahydrate (analytical pure) and 5.65g copper nitrate trihydrate (analytical pure) were dissolved in water into 148mL solution, which was sprayed twice This...

preparation example 2

[0051] Pseudo-boehmite powder prepared by aluminum sulfate method (specific surface area 375m 2 / g, pore volume 0.98ml / g, pseudoboehmite powder contains doping element B, relative to 100g Al 2 o 3 The calculated pseudo-boehmite powder contains 0.53g of B element; during the preparation of the pseudo-boehmite powder, SiO is added at the beginning 2 Precursor water glass (sodium silicate aqueous solution), so that after sintering, the carrier is derived from SiO 2 Precursor of SiO 2 The mass accounts for 11% of the total mass of the carrier)) kneaded with dilute acid water containing 5vol% nitric acid, extruded into a 3mm thick clover shape after kneading, dried at 100°C for 12h, and then calcined at 590°C for 8h to obtain the required carrier.

[0052] Dissolve 151.7g nickel nitrate hexahydrate (industrial grade, purity 98%), 6.83g zinc nitrate hexahydrate (analytical pure) and 5.65g copper nitrate trihydrate (analytical pure) into 156mL solution with water, and use spray d...

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Abstract

The invention relates to the field of piperazine preparation, and discloses a method for preparing piperazine. The method comprises the following steps: in the presence of hydrogen and a catalyst, N-hydroxyethylpiperazine or / and N-aminoethylpiperazine is contacted with an ammonia source for reaction, the molar ratio of N-hydroxyethylpiperazine or / and N-aminoethylpiperazine to the ammonia source is 1: (5-30), the catalyst comprises a carrier, an active component and an optional auxiliary agent, the active component and the optional auxiliary agent are loaded on the carrier, and the active component and the optional auxiliary agent are supported on the carrier. The active component comprises cobalt and / or nickel, and the auxiliary agent is a combination of at least one of VIB group metals, at least one of IB group metals and at least one of IIB group metals. According to the method, piperazine can be generated through reaction, monoethylamine is co-produced, and piperazine selectivity is high.

Description

technical field [0001] The invention relates to the field of preparation of piperazine, in particular to a method for preparing piperazine from N-hydroxyethylpiperazine or / and N-aminoethylpiperazine. Background technique [0002] Piperazine is an important ethylene amine product. The English name is Piperazine, or PIP for short. The molecular formula is C4H10N2. Piperazine and its derivatives are very important fine chemical products, mostly used in medicine, pesticides, and dye intermediates. It is widely used in the field of medicine and is the raw material of various pharmaceutical products. With the continuous expansion of the demand for medicine, especially the demand for quinolones, the market demand for piperazine and its derivatives continues to rise. [0003] Monoethylamine, also known as ethylamine, aminoethane, ethaneamine, the English name is monoethylamine, and the molecular formula is C2H7N. It is a multi-purpose fine chemical product that can be widely used in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/023B01J23/80B01J23/89B01J23/888B01J23/885
CPCC07D295/023B01J23/80B01J23/8953B01J23/888B01J23/885
Inventor 向良玉唐国旗田保亮
Owner CHINA PETROLEUM & CHEM CORP
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