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Synthetic method of n-hydroxyethylpiperazine co-production piperazine

The technology of a kind of hydroxyethylpiperazine and synthesis method is applied in the field of synthesis of N-hydroxyethylpiperazine co-production piperazine, which can solve the problems of high reaction pressure, low production efficiency, low yield, etc., and achieve low reaction pressure , high safety and simple process

Inactive Publication Date: 2018-06-29
JIANGXI SCI & TECH NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN1067246A reports a method for synthesizing N-hydroxyethylpiperazine with piperazine and ethylene oxide as raw materials, but this method uses piperazine as a raw material, resulting in high cost, and ethylene oxide is a dangerous chemical raw material , the storage of ethylene oxide in industrial production is a big problem
Chinese patent CN102432565A discloses a method for obtaining N-hydroxyethylpiperazine by catalytic ring closure using dihydroxyethylethylenediamine as a raw material in a hydrogen atmosphere. This method is also difficult to obtain raw materials, but it can be found that the raw materials are also made of cyclic It is produced by the reaction of ethylene oxide and ethylenediamine. If you prepare raw materials yourself, you will also face the storage problem of ethylene oxide
There are many studies on the synthesis of piperazine at home and abroad. Japanese patents JP49,11,712 and JP74,125,375 report the process route for preparing piperazine by hydrogenation and cyclization of N-β-hydroxyethylethylenediamine as raw material. Such methods are based on Oxides of metals such as copper, chromium, manganese are catalysts, and the yield can reach more than 90%, but the reaction pressure is too high, generally at 8-26MPa, and it is intermittent production, and the production efficiency is low; Catalytic hydrogenation of ketone and N-β-hydroxyethylethylenediamine as raw materials to obtain a mixture of N-alkylpiperazine and piperazine, but the yield is low

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Embodiment 1

[0022] 1) adopt co-precipitation extruding method to prepare catalyst: 148.65g nickel nitrate hexahydrate, 38.46g chromium nitrate nonahydrate, 21.64g ferric nitrate nonahydrate are all made into mass fraction as 40% nitrate aqueous solution, and 77.74g sodium carbonate is formulated The mass fraction is 40% sodium carbonate aqueous solution, and then under rapid mechanical stirring in a water bath at 70°C, add the nitrate aqueous solution and sodium carbonate aqueous solution dropwise into a beaker filled with 400mL deionized water at the same time, and maintain the pH value between 7 and 8 , aged for 1 hour after the precipitation was complete, filtered, washed the filter cake with deionized water until neutral, dried the filter cake at 110°C for 6-10 hours, crushed the filter cake and mixed with 62g of γ-Al 2 o 3 Mix, add appropriate amount of water to fully stir, grind, and then use extruder to extrude into shape, put it in an oven at 110°C and fully dry it, then slowly he...

Embodiment 2

[0027] 1) adopt co-precipitation extrusion method to prepare catalyst: 198.2g nickel nitrate hexahydrate, 38.46g chromium nitrate nonahydrate, 21.64g ferric nitrate nonahydrate are all made into mass fraction and be 50% nitrate aqueous solution, 95.72g sodium carbonate is formulated The mass fraction is 50% sodium carbonate aqueous solution, and then under rapid mechanical stirring in a water bath at 70°C, dropwise into a beaker filled with 400mL deionized water at the same time, maintain the pH value between 7 and 8, age for 1h after the precipitation is complete, and filter , wash the filter cake with deionized water until neutral, dry the filter cake at 110°C for 6 to 10 hours, crush the filter cake and mix it with 52g of diatomaceous earth, add an appropriate amount of water to fully stir, grind, and then use an extruder Extrude into a strip, place it in an oven at 110°C and fully dry it, then slowly raise the temperature to 500°C in a muffle furnace and bake for 4 hours to...

Embodiment 3

[0032] 1) adopt co-precipitation extruding method to prepare catalyst: 148.65g nickel nitrate hexahydrate, 38.46g chromium nitrate nonahydrate, 21.64g ferric nitrate nonahydrate are all made into mass fraction as 30% nitrate aqueous solution, and 77.74g sodium carbonate is formulated The mass fraction is 30% sodium carbonate aqueous solution, and then under rapid mechanical stirring in a water bath at 70°C, dropwise add it into a beaker filled with 400mL deionized water at the same time, maintain the pH value between 7 and 8, age for 1h after the precipitation is complete, and filter , wash the filter cake with deionized water until neutral, dry the filter cake at 110°C for 6-10 hours, crush the filter cake and mix it with 62g of titanium dioxide, add an appropriate amount of water to fully stir, grind, and then extrude with an extruder Shaped, placed in an oven at 110°C and fully dried, then slowly heated to 500°C in a muffle furnace and calcined for 4 hours to obtain the desi...

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Abstract

The invention discloses a method for synthesizing N-hydroxyethylpiperazine co-production piperazine. Diethanolamine and ethanolamine are used as raw materials, and N-hydroxyethylpiperazine and piperazine are obtained after catalyst catalyzed ring closure in a solvent in a fixed-bed reactor under a hydrogen atmosphere. The catalyst prepared by the invention has good selectivity and long service life. The whole process of the synthesis method of the invention has low reaction pressure, high safety, continuous synthesis, and co-production of piperazine while preparing N-hydroxyethyl piperazine. The quality of the prepared product conforms to the first-class industrial product standard, the content of N-hydroxyethylpiperazine and piperazine is not less than 99.5%, and the purity of N-hydroxyethylpiperazine and piperazine is above 99.0%. The invention has simple process and is suitable for industrialized continuous production.

Description

technical field [0001] The invention relates to a synthesis method of an organic intermediate, in particular to a synthesis method of N-hydroxyethylpiperazine co-production piperazine. Background technique [0002] N-Hydroxyethylpiperazine is an important class of chemical products, widely used in surfactants, electronic chemicals, and currently the most popular desulfurization and decarburization detergents. Chinese patent CN1067246A reports a method for synthesizing N-hydroxyethylpiperazine with piperazine and ethylene oxide as raw materials, but this method uses piperazine as raw material, resulting in high cost, and ethylene oxide is a dangerous chemical raw material , the storage of ethylene oxide in industrial production is a big problem. Chinese patent CN102432565A discloses a method for obtaining N-hydroxyethylpiperazine by catalytic ring closure using dihydroxyethylethylenediamine as a raw material in a hydrogen atmosphere. This method is also difficult to obtain r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/088C07D295/027C07D295/023B01J23/86
CPCB01J23/002B01J23/866B01J2523/00C07D295/023C07D295/027C07D295/088B01J2523/31B01J2523/67B01J2523/842B01J2523/847B01J2523/41B01J2523/47
Inventor 王晓季刘帅孙猛黄双平冷晓林爽杰黄飞飞
Owner JIANGXI SCI & TECH NORMAL UNIV