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Catalyst for catalytically synthesizing N-methyl ethanol amine compound and application thereof

A technology of methylethanolamine and catalysts, which is applied in the direction of organic compound/hydride/coordination complex catalysts, preparation of organic compounds, preparation of aminohydroxyl compounds, etc., which can solve the problems of low yield and selectivity, long reaction time, difficult Continuous reaction and other problems to achieve the effect of good selectivity, simple preparation and good dispersion performance

Active Publication Date: 2013-05-01
NINGBO ZHETIE JIANGNING CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation of MMEA and DMEA products by methylation of ethanolamine has been reported at home and abroad, such as Pakistan Ahmed Ali et al. (Asian Journal of Chemistry 2011, Vol (23): 5411-5418) using ZnCl 2 , NaBH 4 As a catalyst, ethanolamine and methanol are used to synthesize MMEA and DMEA products, but the yield is only 72%, and the reaction time is long
Japanese Takeuchi et al. (Journal of Physical Organic Chemistry, 1995, Vol (8) 2: 121-127) used modified H-β molecular sieve as catalyst, benzene as solvent, ethanolamine and methyl diazonium salt as raw materials. MMEA and DMEA products are synthesized. Although the comprehensive yield of the two can reach more than 85%, but because the raw material methyl diazonium salt is unstable and prone to side reactions, there are many types of impurities, and it is difficult to separate, and it is difficult to apply to continuous reaction
In summary, the use of current catalysts for the preparation of N-methylethanolamine series products has problems such as low yield and selectivity. Therefore, it is of great significance to find a catalyst suitable for the catalytic synthesis of N-methylethanolamine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Preparation of PPh 3 -Cs-Al 2 o 3 catalyst

[0031] Weigh 23.5g mesoporous γ-Al 2 o 3 The particles were impregnated in 500ml, 0.5mol / L CsNO 3 In aqueous solution, the CsNO 3 The aqueous solution is just submerged in γ-Al 2 o 3 Particles and soaked at 20 ℃ for 40h, so that the solution is fully mixed. Put all the impregnation liquid and the impregnation into an oven for drying, the temperature of the oven is 80° C., and the drying time is 8 hours to obtain a solid mixture. Under an air atmosphere, put the obtained solid mixture into a high-temperature furnace for calcination. The calcination temperature is 400°C, the calcination time is 10 hours, and the calcination heating rate is 8°C / min. After cooling, take out to obtain Cs-Al 2 o 3 Uniform particles. The uniform particles were completely submerged in 120mL, 0.8mol / L PPh 3impregnated in ethanol solution, the immersion temperature is 20°C, and the immersion time is 40h, and the impregnation mixture is put ...

Embodiment 2

[0036] Preparation of PPh 3 -Cs-Al 2 o 3 catalyst

[0037] Weigh 122g of mesoporous γ-Al 2 o 3 The particles were impregnated in 800mL, 2.2mol / L CsNO 3 In aqueous solution, the CsNO 3 The aqueous solution is just submerged in γ-Al 2 o 3 Particles and soaked at 80 ℃ for 40h, so that the solution is fully mixed. Put all the impregnating liquid and the impregnating matter into an oven for drying, the temperature of the oven is 150° C., and the drying time is 3 hours to obtain a solid mixture. Under the air atmosphere, put the obtained solid mixture into a high-temperature furnace for calcination, the calcination temperature is 600°C, the calcination time is 10 hours, the calcination heating rate is 10°C / min, and the uniform particle Cs-Al is obtained by cooling and taking out 2 o 3 . The uniform particles were completely submerged in 130mL, 2.0mol / L PPh 3 Immersed in ethanol solution, the immersion temperature is 80°C, the immersion time is 40h, take it out and put it...

Embodiment 3

[0041] Preparation of PPh 3 -Cs-Al 2 o 3 catalyst

[0042] Weigh 28.9g mesoporous γ-Al 2 o 3 The particles were impregnated in 1000ml, 0.5mol / LCsNO 3 In aqueous solution, the CsNO 3 The aqueous solution is just submerged in γ-Al 2 o 3 Particles were soaked at 70°C for 6 hours to make the solution fully mixed. Put all the impregnation liquid and the impregnation into an oven for drying, the temperature of the oven is 140° C., and the drying time is 3.5 hours to obtain a solid mixture. Under the air atmosphere, put the obtained solid mixture into a high-temperature furnace for calcination, the calcination temperature is 500°C, the calcination time is 5 hours, the calcination heating rate is 10°C / min, and the Cs-Al is obtained by cooling. 2 o 3 Uniform particles. The uniform particles were completely submerged in 120mL, 0.8mol / L PPh 3 immersion in ethanol solution, the immersion temperature is 20°C, the immersion time is 40h, take it out and put it into a drying oven ...

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PUM

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Abstract

The invention provides catalyst for catalytically synthesizing an N-methyl ethanol amine compound and a preparation method thereof. The catalyst adopts a mesopore Al2O3 as a carrier; after modifying the carrier, alkali metal salt is dipped in organic solution of triphenylphosphine, and is dried to obtain the catalyst; and in the catalyst, the substance amount ratio of thetriphenylphosphine to an alkali metal element to an aluminum element is 1: (2.5-7.5): (4.5-9.3). The catalyst has the characteristics of simplicity in preparation, excellent dispersivity, large specific surface area, long service life and the like. The catalyst is applied in the reaction of N methyl ethanol amine organic amine (MMEA, DMEA), so that the conversion rate is high, and the selectivity is good.

Description

technical field [0001] The invention relates to a catalyst for catalyzing and synthesizing N-methylethanolamine compounds, a preparation method and application thereof. Background technique [0002] N-methyl monoethanolamine (MMEA) and N,N-dimethyl aminoethanol (DMEA) are basic chemical and pharmaceutical raw materials, and are widely used in the manufacture of polyurethane foam Coatings, paints, inks, water-soluble coating resin synthesis, polyurethane coatings, resins, water treatment agents, gas treatment agents, ion exchange resins and other chemical products. In addition, it can also be used as semi-finished products of insecticides, emulsifiers, fabric auxiliaries, intermediates of antitumor drug nitrogen mustard hydrochloride, catalysts for urethane coatings, fiber auxiliaries, etc. dry agent. [0003] The preparation of MMEA and DMEA products by methylation of ethanolamine has been reported at home and abroad, such as Pakistan Ahmed Ali et al. (Asian Journal of Che...

Claims

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Application Information

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IPC IPC(8): B01J31/26C07C213/08C07C215/08
Inventor 饶金土陈爱民肖晓辉胡军毛正余
Owner NINGBO ZHETIE JIANGNING CHEM
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