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Combined preparation method for ethylene diamine and aminoethylpiperazine

An amine ethyl piperazine and a combined preparation technology are applied in the field of joint preparation of ethylenediamine and amine ethyl piperazine, can solve the problem of low yield of ethyl piperazine and the like, and achieve the effect of improving the yield

Inactive Publication Date: 2010-07-07
山西玉龙化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to solve the problem that the yield of ethylenediamine and aminoethylpiperazine is not high, it is necessary to avoid the generation of diethylenetriamine by-product in the amination reaction

Method used

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  • Combined preparation method for ethylene diamine and aminoethylpiperazine
  • Combined preparation method for ethylene diamine and aminoethylpiperazine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1.1 Preparation of catalyst

[0024] a. Phosphorus-modified mordenite catalyst

[0025] Take 80g of mordenite, add 20g of alumina and 5mL of water, granulate, shape, press into Φ5×5mm cylindrical particles, dry and roast at 500°C for 2 hours to obtain a catalyst precursor;

[0026] 50 g of the catalyst precursor was added to a solution prepared by 54 mL of n-hexane and 3.4 g of trimethyl phosphate for impregnation, and the n-hexane was distilled off at 90°C. The residue after evaporating to dryness was heated up to 550° C. in a muffle furnace at 3° C. / min, calcined for 5 hours, and cooled naturally to obtain a 1.5% phosphorus-modified mordenite catalyst.

[0027] b. Silicon modified ZSM-5 zeolite catalyst

[0028] Take 80g of ZSM-5 zeolite, add 20g of alumina and 5mL of water, granulate, shape, press into Φ5×5mm cylindrical particles, dry and roast at 500°C for 2 hours to obtain the catalyst precursor;

[0029] 50 g of catalyst precursor was added to a solution prepa...

Embodiment 2

[0035] 2.1 Preparation of catalyst

[0036] a. Phosphorus-modified mordenite catalyst

[0037] The catalyst preparation process is basically the same as in Example 1, except that the solution prepared by 58 mL of n-hexane and 4.7 g of trimethyl phosphate is used for impregnation to obtain a 2.1% phosphorus-modified mordenite catalyst.

[0038] b. Silicon modified ZSM-5 zeolite catalyst:

[0039] The catalyst preparation process is basically the same as in Example 1, except that the solution prepared by 50 mL of n-hexane and 17.5 g of phenyltrimethoxysilane is used for impregnation to obtain a 5.0% silicon-modified ZSM-5 zeolite catalyst.

[0040] 2.2 Amination reaction

[0041] Mix ethanolamine and ammonia, preheat and vaporize, pass into a fixed-bed reactor, and react in the presence of a condensation amination catalyst of 2.1% phosphorus-modified mordenite catalyst, the pressure is 5.0MPa, the temperature is 300°C, the weight of ammonia and ethanolamine The ratio is 6:1, ...

Embodiment 3

[0045] 3.1 Preparation of catalyst

[0046] a. Phosphorus-modified mordenite catalyst

[0047] The catalyst preparation process is basically the same as in Example 1, except that the solution prepared by 70 mL of n-hexane and 4.1 g of trimethyl phosphate is used for impregnation to obtain a 1.8% phosphorus-modified mordenite catalyst.

[0048] b. Silicon modified ZSM-5 zeolite catalyst

[0049] The catalyst preparation process is basically the same as in Example 1, except that the solution prepared by 50 mL of n-hexane and 8.8 g of phenyltrimethoxysilane is used for impregnation to obtain a 2.5% silicon-modified ZSM-5 zeolite catalyst.

[0050] 3.2 Amination reaction

[0051] Mix ethanolamine and ammonia, preheat and vaporize, pass into a fixed-bed reactor, and react in the presence of a condensation amination catalyst of 1.8% phosphorus-modified mordenite, with a pressure of 2.0 MPa and a temperature of 350°C. The weight ratio of ammonia to ethanolamine is The ratio is 12:...

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Abstract

The invention discloses a combined preparation process of ethane diamine and aminoethyl piperazine, aiming to solve the problem low yield when prepared associated ethane diamine and aminoethyl piperazine. The invention comprises the steps as flowed that firstly mixing ethane diamine and ammonia to react under the conditions of the exist of mordenite of condensed amination catalyst phosphorous modification, 2.0MPa-5.0MPa pressure, 300-350 DEG C temperature, 6-12:1 of ammonia and aminoethyl alcohol weight ratio, 20-30 seconds of reaction contact time, distilling and separating product liquid toobtain aminoethyl alcohol product, secondly reacting piperazine which is obtained in first step and aminoethyl alcohol under the conditions of the exist of ZSM-5 zeolite of condensed amination catalyst silicon modification, 4.0MPa-8.0MPa pressure, 350-400 DEG C temperature, 0.5-1.5:1 of piperazine and aminoethyl alcohol weight ratio, and 10-20 seconds of reaction contact time, distilling and separating product liquid to obtain aminoethyl piperazine product. The invention is mainly combined to be used to prepare ethane diamine and aminoethyl piperazine.

Description

technical field [0001] The invention relates to a combined preparation method of ethylenediamine and aminoethylpiperazine. technical background [0002] Ethylenediamine and aminoethylpiperazine are two chemical raw materials that are in short supply in the market, and are widely used in the fields of epoxy resin curing agents, pesticides, and high molecular polymers. [0003] In the preparation method of ethylenediamine, when ethanolamine, ammonia and hydrogen are used as raw materials for amination reaction, the amination product is ethylenediamine, accompanied by a certain amount of piperazine and aminoethylpiperazine. In the preparation method of aminoethylpiperazine, when ethanolamine and piperazine are used as raw materials for amination reaction, the amination product is aminoethylpiperazine. [0004] Usually, because the intermediate amine produced by the amination reaction has higher reactivity than ammonia, it further reacts with ethanolamine to form a cyclic amine...

Claims

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Application Information

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IPC IPC(8): C07C211/10C07C209/60C07D295/13B01J29/18
Inventor 吕剑杨建明赵锋伟谷玉杰寇联岗
Owner 山西玉龙化工有限公司
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