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Method of selectively synthesizing triethylene diamine

A technology of triethylenediamine and selectivity, applied in the direction of organic chemistry, can solve the problems of large amount of by-product piperazine, increased difficulty and cost of separation of triethylenediamine, low selectivity of triethylenediamine, etc.

Inactive Publication Date: 2003-09-17
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The problem with existing methods is that most of them use ethylenediamine, piperazine and their derivatives as synthetic raw materials. These raw materials are not only costly, but also have limited resources.
A few use relatively cheap and easy-to-obtain monoethanolamine as a synthetic raw material, but the conversion rate of monoethanolamine is low, the selectivity of the main product triethylenediamine is low, and the amount of by-product piperazine is large
The large amount of piperazine and the large amount of unreacted monoethanolamine (boiling point is 170.8°C) will increase the difficulty and cost of separating triethylenediamine (boiling point is 174°C)
In addition, some methods require to be carried out under pressurized, carrier gas (hydrogen or nitrogen) or step-by-step reaction conditions, and the operation cost is high
The above problems make the existing methods, especially the method of taking monoethanolamine as a synthetic raw material, difficult for industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation Embodiment 1

[0033] Catalyst Preparation Example 1: A non-modified hydrogen-type catalyst was prepared by using a small-grain sodium-type ZSM-5 zeolite with a grain size of 20-50 nanometers.

[0034](1) Removal of organic amine template agent treatment: take the small-grain sodium-type ZSM-5 zeolite raw powder with a grain size of 20-50 nm, dry it at 110°C for 3 hours, and then perform temperature-programmed roasting in a muffle furnace , the heating method is as follows: from room temperature to 300°C at a heating rate of 1°C / min, and keep the temperature at 300°C for 1 hour; then raise the temperature to 400°C at the same heating rate, and hold at 400°C for 1 hour; The heating rate was raised to 500°C, and the temperature was kept at 500°C for 1 hour; then the temperature was raised to 550°C at the same heating rate, and the temperature was kept at 550°C for 12 hours. (2) Molding: According to the weight ratio of zeolite and alumina on a dry basis of 8:2, take 80 grams (dry basis) of sod...

preparation Embodiment 2

[0035] Catalyst Preparation Example 2: Preparation of an unmodified hydrogen-type catalyst with a small-grain sodium-type ZSM-5 zeolite with a grain size of 500 nanometers

[0036] Repeat Example 1, but the grain size of the used small grain sodium type ZSM-5 zeolite raw powder is 500 nanometers. Accordingly, the obtained hydrogen-type catalyst was designated as HZSM-5 (8 / 2, 500 nm).

preparation Embodiment 3

[0037] Catalyst preparation example 3 (comparative example): an unmodified hydrogen-type catalyst was prepared from a large-grain sodium-type ZSM-5 zeolite with a grain size of 1000-2000 nanometers.

[0038] Repeat Example 1, but the used sodium type ZSM-5 zeolite raw powder grain size is a large crystal grain of 1000-2000 nanometers. Correspondingly, the obtained hydrogen-type catalyst was designated as HZSM-5 (8 / 2, 1000-2000 nm).

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Abstract

A process for selectively synthesizing trivinyldiamine features the reaction of monoethanol amine and small-grain zeolite catalyst in fixed-bed reactor under feeding ammonia and water. The said small-grain zeolite may be ZSM-5, ZSM-8, ZSM-11, ZSM-5 / ZSM0-11, ZSM-23 and MCM-22. Its advantages are high output rate and selectivity, and less by-product and pollution.

Description

technical field [0001] The invention belongs to the technical field of fine chemical synthesis. The catalyst preparation technology and reaction technology related to the synthesis of triethylenediamine provide a selective synthesis of triethylenediamine (TEDA) using monoethanolamine (MEOA) raw materials under normal pressure and no carrier gas, and simultaneously separate three A method for recycling the mother liquor of ethylenediamine. The present invention is applicable to the situation that ethylenediamine, piperazine, N-aminoethylpiperazine, N-hydroxyethylpiperazine, and any mixture of these amine-containing organic substances including monoethanolamine are used as raw materials. Background technique [0002] Triethylenediamine (TEDA or DABCO), also known as triethylenediamine, is an important catalyst for the production of polyurethane foam. In addition, triethylenediamine can also be used as a catalyst for the polymerization of acrylonitrile, an initiator for pesti...

Claims

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Application Information

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IPC IPC(8): C07C211/20C07D487/08
Inventor 郭洪臣赵凌雁李善军陈黎行王祥生
Owner DALIAN UNIV OF TECH
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