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Synthesis method of diethyltoluenediamine

A technology of diethyltoluenediamine and toluenediamine, which is applied in the chemical field, can solve problems such as low catalytic activity, strong toxicity, and high price, and achieve the effects of overcoming easy coking, easy control, and mild reaction conditions

Active Publication Date: 2017-07-14
ANYANG INST OF TECH
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Problems solved by technology

The invention overcomes the disadvantages of the traditional synthesis of DETDA aluminum-based catalysts such as low catalytic activity, easy coking, high price, and strong toxicity. 180 °C, the comprehensive benefit evaluation of the process scheme found that 3% CeO 2 doped CeO 2 -CuO / ZnO / Al 2 o 3 Highest catalytic activity

Method used

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  • Synthesis method of diethyltoluenediamine
  • Synthesis method of diethyltoluenediamine

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Experimental program
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Embodiment Construction

[0026] 1. Control cabinet, 2. High-pressure reaction kettle, 3. Toluenediamine feeding pump, 4. Toluenediamine storage tank, 5. Transfer tank, 6. Distillation tower, 7. Bottom reflux pump, 8. Boiler, 9. Tower bottom product storage tank, 10. Tower top total condenser, 11. Tower top reflux pump, 12. Tower top storage tank, 13. Toluenediamine circulation pump, 14. Rectification feed pump

[0027] combine Figure 1~2 , a kind of catalytic synthesis diethyltoluenediamine process of the present invention, under the condition of 80 ℃ constant temperature water bath, prepare the aqueous solution of copper nitrate, zinc nitrate, aluminum nitrate, cerium nitrate, according to molar ratio n (硝酸铜) :n (硝酸锌) :n (硝酸铝) :n (硝酸铈) =1:1:2:0.06, that is, the molar ratio of copper nitrate, zinc nitrate, aluminum nitrate, and cerium nitrate is 1:1:2:0.06, the solution is blue, fully stirred for 0.5 h, and then according to the molar ratio n (柠檬酸) :n (硝酸铜+硝酸锌+硝酸铝+硝酸铈) =1.2:1, that is, the mola...

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Abstract

The invention relates to a synthesis method of diethyltoluenediamine (DETDA). According to the synthesis method, sol-gel method is adopted to prepare catalyst CeO2-CuO / ZnO / Al2O3; feeding is carried out at a toluenediamine (TDA) : ethylene : the catalyst metal atom molar ratio of 1.1:2.2:0.05; H2 is introduced into the high pressure reaction kettle for reduction and activation of the catalyst, TDA is added, full stirring is carried out, and ethylene gas is added to replace H2; the temperature is increased to 220 to 230 DEG C via temperature programming, reaction pressure is maintained to be 3.0MPa, and reaction is carried out for 3h; an appropriate amount of water is added into the high pressure reaction kettle, and reduced pressure distillation is carried out so as to obtain DETDA. The DETDA selectivity and the yield of the synthesis method are 85.2% and 93.7% respectively, the purity is 99.1%, the quality is capable of satisfying requirements of the national quality standards, and the synthesis method is green and clean, and is friendly to the environment.

Description

technical field [0001] The present invention relates to the synthetic technique of diethyltoluenediamine, specifically refers to catalyst CeO 2 -CuO / ZnO / Al 2 o 3 The invention discloses a process for catalytically synthesizing diethyltoluenediamine, which belongs to the field of chemistry. Background technique [0002] There are two types of amine chain extenders, aliphatic amines and aromatic amines. 3,3'-dichloro-4,4'-diaminodiphenylmethane (MOCA) used to occupy the dominant position of aromatic amine chain extenders, although the obtained The product has good mechanical properties. According to the latest clinical findings, 3,3'-dichloro-4,4'-diaminodiphenylmethane (MOCA) has certain carcinogenicity and is harmful to people's physical and mental health. Some countries in Europe and the United States have Strictly restricting its use, the development of new environmentally friendly aromatic amine chain extenders has gradually become an urgent task in the modern chemical...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/68C07C211/51B01J23/83
CPCC07C209/68B01J23/002B01J23/83B01J2523/00C07C211/51B01J2523/17B01J2523/27B01J2523/31B01J2523/3712
Inventor 贾太轩王鑫杨立国张允宋海香侯绍纲
Owner ANYANG INST OF TECH
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