Synthesis method of diethyl toluene diamine

A technology of diethyltoluenediamine and a synthesis method, which is used in the preparation of amino compounds from amines, chemical recycling, organic chemistry, etc., can solve problems such as unfavorable human health and environmental protection, expensive alkyl aluminum, and environmental pollution of waste materials. , to achieve the effect of being conducive to environmental protection, reducing catalyst costs, and reducing material viscosity

Inactive Publication Date: 2009-04-29
杭州崇舜化学有限公司
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0018] In the existing method for synthesizing diethyltoluenediamine, when using inorganic aluminum as a catalyst, the time to form the catalyst system is long (generally more than 3 hours), and the material is easy to coke under high temperature and high pressure
Single use of alkylaluminum as a catalyst, alkylaluminum is expensive and highly toxic, which

Method used

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  • Synthesis method of diethyl toluene diamine
  • Synthesis method of diethyl toluene diamine
  • Synthesis method of diethyl toluene diamine

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Put 2000g of TDA, 35g of AL powder (20-40 mesh), 15g of Zn powder (40 mesh), 50g of aluminum trichloride (anhydrous), and 10g of diethylaluminum chloride into a stirred 51 autoclave, and heat together. When the temperature rises to 150°C, hydrogen will be released, and the hydrogen will basically emit light at 200°C for nearly 1 hour; pass through ethylene to purge 2-3mim; continue to heat up to 320°C, fill with pressurized ethylene, and the pressure is 6.5-7.0Mpa , The amount of ethylene is about 990g, and the ethylene is completely absorbed after about half an hour. Then lower the temperature and reduce the pressure, add diphenyl ether to dilute the reactant, filter at 0.2-0.3Mpa, 150°C, and distill the filtrate to obtain the product 3.5-diethyl-2.4(2.6)-diaminotoluene, the yield is 73%, the product The content was analyzed by high pressure liquid chromatography to be 95%.

Embodiment 2

[0035] Put TDA2000g into the reactor, Al powder (20-40 mesh) 40g, Zn powder (40 mesh) 15g, aluminum trichloride

[0036] (anhydrous) 55g, diethylaluminum chloride 15g, all the other are identical with embodiment 1, add phenoxybiphenyl to dilute reactant before filtration, record yield and be 75%, product is analyzed by high pressure liquid chromatography and content is 97%.

Embodiment 3

[0038] Drop into reactor TDA2000g, AL powder (20-40 order) 35g, Zn powder (40 order) 15g, aluminum trichloride (anhydrous) 60g, monochlorodiethylaluminum 18g, all the other are identical with embodiment 1, measure Obtain product yield 80%, content 97%.

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Abstract

The invention discloses a method for preparing diethyltoluenediamine, which comprises the following steps: diaminotoluene and catalyst are added to a reactor; an 'aromatic amine-aluminum' catalyst system is formed after temperature rising and stirring, and ethylene is pumped into the reactor to purge the hydrogen produced by the reaction; high pressure ethylene gas is pumped in, and after complete alkylation, diphenyl ether or phenoxy biphenyl are added to dilute the reactants; the mixture is filtered, the materials at the bottom of the reactor are recycled, the filtrate is distilled, and diethyltoluenediamine is obtained. The method has the advantages that, aluminum, zinc, aluminum chloride and organic aluminum are used as the catalyst, so activity is increased, reaction pressure is lowered and reaction time is reduced; diphenyl ether or phenoxy biphenyl is added before filtration, so material viscosity can be lowered to facilitate filtration and separation, simultaneously, the 'aromatic amine-aluminum' catalyst system is not damaged; the catalyst can be recycled, so operation steps are reduced, catalyst cost is greatly lowered and environment protection is benefited.

Description

technical field [0001] The invention relates to the field of alkylation reactions of aromatic amines, in particular to a method for synthesizing diethyltoluenediamine with diaminotoluene. Background technique [0002] 3.5-diethyl-2.4(2.6)-diaminotoluene (English name: 3.5-diethl-2.4(2.6)-toluenediamine), molecular structure formula is [0003] [0004] It has a boiling point of 308°C, a freezing point of 9°C, and a viscosity of 280 centistokes at 20°C. It is a transparent amber liquid with a slight ammonia smell. It is mainly used as a hardener for polyurethane and epoxy resin and used in conjunction with E-300. It is widely used as the main chain extender and elastomer for reaction injection molding (RIM) of polyurethane and sprayed polyurethane polyurea elastomer (SPUA). Antioxidants of lubricating oil chemical intermediates, etc. [0005] According to scientific research reports, the reaction mechanism of alkylation of arylamine is: [0006] The first step: the reac...

Claims

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Application Information

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IPC IPC(8): C07C211/51C07C209/68
CPCY02P20/584
Inventor 蒋景岗钟文清
Owner 杭州崇舜化学有限公司
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