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Preparation method of diethyltoluenediamine

A technology of diethyltoluenediamine and triethylaluminum, which is used in the preparation of amino compounds from amines, chemical instruments and methods, and purification/separation of amino compounds, etc. low rate and other problems, to achieve mild reaction conditions, lower production costs, and good safety effects

Inactive Publication Date: 2018-08-10
HUAIAN SHUANGYANG CHEM
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, the post-treatment in this process is complicated, mainly because the catalyst prepared with aluminum powder as raw material cannot be reused, and it is necessary to add water to the product system obtained after the reaction for hydrolysis reaction to obtain crude DETDA and aluminum hydroxide precipitation, which will be refined in the next step. The reaction yield is about 80-85%; if the subsequent rectification operation is carried out directly without hydrolysis reaction, the catalyst will block the rectification equipment
It can be seen that the reaction yield of this process is low, and hydrolysis steps are required, which increases equipment investment. At the same time, each ton of crude product in the hydrolysis process will produce 2 tons of waste water, and waste water treatment will also increase production costs.

Method used

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  • Preparation method of diethyltoluenediamine
  • Preparation method of diethyltoluenediamine

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preparation example Construction

[0019] The invention provides a kind of preparation method of diethyltoluenediamine, comprises the following steps:

[0020] Carrying out a complex reaction between m-toluenediamine and triethylaluminum to obtain a complex material containing an aluminum complex; the temperature of the complex reaction is 150-160° C., and the pressure is 0.4-0.6 MPa;

[0021] Alkylation reaction is carried out between the complex material containing aluminum complex and ethylene to obtain diethyltoluenediamine; the temperature of the alkylation reaction is 300-310° C., and the pressure is 4.6-5.0 MPa.

[0022] In the present invention, m-toluenediamine (TDA) and triethylaluminum are subjected to a complex reaction to obtain a complex material containing an aluminum complex; the temperature of the complex reaction is 150-160° C., and the pressure is 0.4-0.6 MPa . In the present invention, the reaction equation of described complexation reaction is specifically as follows:

[0023]

[0024]...

Embodiment 1

[0046] Put m-toluenediamine (2000kg) and triethylaluminum (35kg) in an evaporator, and under the protection of nitrogen, carry out complexation reaction at 160°C and 0.5MPa for 1.5h to obtain a complex materials;

[0047] Pump the complex material containing aluminum complex into the synthesis kettle, pass through ethylene (460kg), and carry out the alkylation reaction at 310°C and 4.6MPa for 6h under the protection of nitrogen;

[0048] Using the pressure of the synthesis tank, press the remaining ethylene in the synthesis tank after the alkylation reaction is completed into the ethylene recovery tank, and then turn on the membrane press to press the recovered ethylene into the synthesis tank for use; control the vacuum degree of the evaporation tank to ≤ -0.098MPa, the alkylation material obtained after the completion of the alkylation reaction is sucked into the evaporator, and the first vacuum distillation is carried out at 140°C. The distilled fraction is crude diethyltol...

Embodiment 2

[0053] Put m-toluenediamine (2t) and triethylaluminum (40kg) in an evaporator, and under the protection of nitrogen, carry out complexation reaction at 150°C and 0.6MPa for 2 hours to obtain complexed materials containing aluminum complexes ;

[0054] The complex material containing the aluminum complex is pumped into the synthesis kettle, and ethylene (480kg) is introduced, and under the protection of nitrogen, the alkylation reaction is carried out at 300°C and 5.0MPa for 7h, and then according to the method of Example 1 The step is post-treated to obtain the finished product of diethyltoluenediamine.

[0055] The yield of the final diethyltoluenediamine finished product is about 92%, and the purity is about 98.5%.

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Abstract

The invention provides a preparation method of diethyltoluenediamine. According to the method, 2,4 / 2,6-diaminotoluene and triethylaluminium take complex reaction; the reaction conditions are mild; thesafety is high; an obtained complex material containing an aluminum complex does not need aftertreatment and directly performs subsequent alkylation reaction, wherein the aluminum complex in the complex material is used as a catalyst; excessive 2,4 / 2,6-diaminotoluene in the complex material is catalyzed to take subsequent alkylation reaction with ethylene; after the alkylation reaction is finished, the aluminum complex can be recovered and reutilized; compared with a traditional process, the preparation method has the advantages that about 50 percent of solid waste can be reduced when each ton of target product of diethyltoluenediamine is produced; the production cost can be effectively reduced. The yield of the product obtained by the preparation method provided by the invention is highand can reach 90 percent; the purity is high and reaches 98.5 percent or higher.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a preparation method of diethyltoluenediamine. Background technique [0002] Diethyltoluenediamine (DETDA) is an important chemical raw material, widely used in curing agent, chain extender, polyurethane raw material, amine catalyst, lubricant, antioxidant of industrial oil, etc. [0003] The existing production process of DETDA is to use m-toluenediamine and aluminum powder as raw materials, react at about 285°C and 3-3.55MPa for about 5 hours to form a catalyst; then control the reaction temperature at 305°C and pressure at 4.5MPa , into ethylene, continue the reaction for about 8h, generate DETDA. However, the post-treatment in this process is complicated, mainly because the catalyst prepared with aluminum powder as raw material cannot be reused, and it is necessary to add water to the product system obtained after the reaction for hydrolysis reaction to obtain cr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/68C07C209/86C07C211/51B01J31/22
CPCB01J31/1805B01J2531/0213B01J2531/31C07C209/68C07C209/86C07C211/51
Inventor 林瑜琨马俊
Owner HUAIAN SHUANGYANG CHEM
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