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Method for preparing N, N-diisopropylethylamine

A technology for diisopropylethylamine and diisopropylamine, which is applied in the field of preparing N,N-diisopropylethylamine, can solve the problems of high waste water treatment cost, high stirring requirements, equipment corrosiveness, etc. Low requirements, good selectivity, and the effect of avoiding corrosion

Inactive Publication Date: 2022-02-25
山东达民化工股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction generates salt, which requires high equipment stirring, and the reaction generates hydrogen halide, which is corrosive to the equipment, and the cost of wastewater treatment is very high;
[0005] 2) In the document "Synthesis of N,N-diisopropylethylamine", a method for synthesizing DIPEA with diisopropylamine and diethyl sulfate as raw materials is reported, with a yield of 90% and a simple process. The commonly used route, but diethyl sulfate is more toxic and seriously pollutes the environment;
But the catalyst is expensive and the yield is low

Method used

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preparation example Construction

[0064] 1. The preparation process of the catalyst: Al(OH)3 is prepared into sodium metaaluminate solution with 40% NaOH, and the precipitate is neutralized with nitric acid. After aging, filtering and washing, it is rolled into a ball, dried and roasted to obtain a diameter of 3mm. The spherical Al2O3 carrier, the nitrates of Mo, Ni, and Cu are made into a mixed solution in proportion, the Al2O3 carrier is impregnated, dried and placed in a muffle furnace for 6 h at 490°C, and mixed with Mo, Ni, and Cu nitrates again after cooling Solution impregnated, after roasting under the same conditions, the prepared content is Mo8%, Ni25%, Cu5%, and the rest is Al2O3 Mo-Ni-Cu / Al2O3 catalyst, after the catalyst is loaded into the reactor, use pure hydrogen at 0.05MPa pressure, The finished catalyst was obtained by reduction for 24 hours at a temperature of 460°C and a space velocity of 1000h-1;

[0065] 2. The reaction conditions are reaction pressure: 0.8-1.6Mpa, hydrogen is used to mai...

Embodiment 1

[0070] Reaction conditions: Reaction pressure: 0.8Mpa, reaction temperature: 180°C, raw materials are ethanol and diisopropylamine to form a mixed solution with a molar ratio of 1.2:1.

[0071] The experimental data are:

[0072]

Embodiment 2

[0074] Reaction conditions: Reaction pressure: 0.8Mpa, reaction temperature: 200°C, raw materials are ethanol and diisopropylamine to form a mixed solution with a molar ratio of 1.2:1.

[0075] The experimental data are:

[0076]

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Abstract

The invention discloses a preparation method of N, N-diisopropylethylamine, which comprises the following step of: performing a reaction on ethanol and diisopropylamine as raw materials through the catalysis of a catalyst in a fixed bed reactor under the atmosphere of hydrogen to obtain N, N-diisopropylethylamine and simultaneously obtain diethylamine, triethylamine and isopropanol as by-products. The method for preparing N, N-diisopropylethylamine is simple in process, low in cost, high in conversion rate and good in selectivity. Meanwhile, gas-solid phase reaction is adopted in the method, corrosion of liquid-phase materials to reaction equipment under high-temperature and high-pressure conditions is avoided, the requirement for equipment materials is low, and full-continuous production can be achieved. Unreacted ethanol and diisopropylamine can continue to return to the reaction system as raw materials, and the obtained diethylamine, triethylamine and isopropanol can be sold as byproducts after being rectified and purified.

Description

technical field [0001] The invention belongs to the field of organic chemical intermediates, in particular to a method for preparing N,N-diisopropylethylamine. Background technique [0002] N,N-Diisopropylethylamine is an important organic chemical intermediate, which is mainly used in the following aspects: (1) an important pharmaceutical and pesticide synthesis intermediate; (2) can also be used as a condensation Mixing agent, such as for the condensation reaction of carbon monoxide, amine and alkyl halide to form urethane; (3) As a catalyst for ester hydrolysis and other reactions. [0003] According to comprehensive literature reports, there are currently three main synthetic methods for N,N-diisopropylethylamine: [0004] 1) Patent CN101759571 reports a method to generate DIPEA by reacting diisopropylamine and alkyl halide, the reaction pressure is 0.4-2.5MPa, and the yield is about 95%. However, the reaction generates salt, which requires high equipment stirring, and...

Claims

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Application Information

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IPC IPC(8): C07C209/16C07C211/08C07C209/08B01J23/883
CPCC07C209/16C07C209/08B01J23/883C07C211/08
Inventor 陈国建陈国华郭文杰
Owner 山东达民化工股份有限公司
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