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Preparation method of N, N-diisopropylethylamine

A technology of diisopropylethylamine and diisopropylamine, which is applied in the field of preparation of N,N-diisopropylethylamine, can solve the problems of high waste water treatment cost, equipment corrosivity, low yield, etc. Low material requirements, corrosion avoidance, high conversion rate

Inactive Publication Date: 2022-03-01
山东达民化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A preparation method of N,N-diisopropylethylamine, comprising the following steps:

[0029] S1. Obtain raw materials and catalysts. The raw materials are ethanol and diisopropylamine, and the catalysts are Mo-Ni-Cu / Al 2 o 3 ;Mo-Ni-Cu / Al 2 o 3 The composition of the catalyst is: Mo is 8%, Ni is 25%, Cu is 5%, and the rest is Al 2 o 3

[0030] Catalyst preparation steps are:

[0031] A1. 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 formed by ball rolling, dried and roasted to obtain spherical Al with a diameter of 3mm. 2 o 3 carrier;

[0032] A2, make the mixed solution of Mo, Ni, Cu nitrate in proportion, to Al 2 o 3 The carrier is impregnated;

[0033] A3, after drying, put it into the muffle furnace for roasting; the temperature of the muffle furnace is 490°C, and the roasting time is 6h;

[0034] A4 and A3 are cooled after roasting, impre...

Embodiment 2

[0044] A preparation method of N,N-diisopropylethylamine, comprising the following steps:

[0045] S1. Obtain raw materials and catalysts. The raw materials are ethanol and diisopropylamine, and the catalysts are Mo-Ni-Cu / Al 2 o 3 ;Mo-Ni-Cu / Al 2 o 3 The composition of the catalyst is: Mo is 8%, Ni is 25%, Cu is 5%, and the rest is Al 2 o 3

[0046] Catalyst preparation steps are:

[0047] A1. 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 formed by ball rolling, dried and roasted to obtain spherical Al with a diameter of 3mm. 2 o 3 carrier;

[0048] A2, make the mixed solution of Mo, Ni, Cu nitrate in proportion, to Al 2 o 3 The carrier is impregnated;

[0049] A3, after drying, put it into a muffle furnace for roasting; the temperature of the muffle furnace is 490°C, and the roasting time is 6h;

[0050] A4 and A3 are cooled after roasting, impregn...

Embodiment 3

[0060] A preparation method of N,N-diisopropylethylamine, comprising the following steps:

[0061] S1. Obtain raw materials and catalysts. The raw materials are ethanol and diisopropylamine, and the catalysts are Mo-Ni-Cu / Al 2 o 3 ;Mo-Ni-Cu / Al 2 o 3 The composition of the catalyst is: Mo is 8%, Ni is 25%, Cu is 5%, and the rest is Al 2 o 3

[0062] Catalyst preparation steps are:

[0063] A1. 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 formed by ball rolling, dried and roasted to obtain spherical Al with a diameter of 3mm. 2 o 3 carrier;

[0064] A2, make the mixed solution of Mo, Ni, Cu nitrate in proportion, to Al 2 o 3 The carrier is impregnated;

[0065] A3, after drying, put it into a muffle furnace for roasting; the temperature of the muffle furnace is 490°C, and the roasting time is 6h;

[0066] A4 and A3 are cooled after roasting, impregn...

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PUM

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Abstract

The invention relates to the technical field of N, N-diisopropylethylamine, and discloses a preparation method of N, N-diisopropylethylamine, which comprises the following steps: S1, raw materials and a catalyst are obtained, the raw materials are ethanol and diisopropylamine, and the catalyst is Mo-Ni-Cu / Al2O3; s2, preparing ethanol and diisopropylamine into a mixed solution with the molar ratio of (1.2-1.6): 1, and pumping the mixed solution into a vaporizer of a reaction system by using a metering pump; and S3, gasifying the heated mixed liquid of ethanol and diisopropylamine in the vaporizer by using a compressor with hydrogen in the system. The method is simple in process, low in cost, high in conversion rate and good in selectivity, meanwhile, gas-solid phase reaction is adopted, corrosion of liquid-phase materials to reaction equipment under the high-temperature and high-pressure conditions is avoided, the requirement for equipment materials is low, full-continuous production can be achieved, unreacted ethyl alcohol and diisopropylamine can continue to serve as raw materials to be returned into a reaction system, and the method is suitable for industrial production. And a plurality of products such as N, N-diisopropylethylamine, isopropanol, diethylamine and triethylamine can be produced at the same time.

Description

technical field [0001] The invention relates to the technical field of N,N-diisopropylethylamine, in particular to a preparation method of 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 stirrin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/08C07C209/84B01J23/885
CPCC07C209/16C07C209/84B01J23/885C07C211/08
Inventor 陈国建陈国华郭文杰
Owner 山东达民化工股份有限公司