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Catalytic synthesis method of N-substituted ethanol amine compound

A technology for amine compounds and ethanolamines, which is applied in the field of catalytic synthesis of N-substituted ethanolamine compounds, can solve the problems of unfavorable purification, product separation, and high preparation costs, and achieves easy industrial scale-up production, mild reaction conditions, and specific surface area. big effect

Inactive Publication Date: 2016-04-20
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The color purity of the product obtained after distillation is very high, but homogeneous water is prone to side reactions of epoxy compounds, which is not conducive to purification and separation, and the catalyst is expensive and the preparation cost is high
[0004] Therefore, in the unfavorable circumstances such as the high cost of catalyst preparation in the prior art, many side reactions, low reutilization rate and complicated product separation and purification, it is of great significance to find a catalyst that can efficiently catalyze the synthesis of N-substituent ethanolamine compounds under solvent-free conditions. Significance

Method used

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  • Catalytic synthesis method of N-substituted ethanol amine compound
  • Catalytic synthesis method of N-substituted ethanol amine compound
  • Catalytic synthesis method of N-substituted ethanol amine compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Preparation of Ti-MCM-41 molecular sieve:

[0032] Weigh 2.67g of sodium hydroxide and 5.94g of cetyltrimethylammonium bromide (CTAB) into 147g of deionized water, and stir vigorously to obtain a colorless transparent solution. Then weigh 14.45 g of tetraethyl silicate (TEOS) and add it dropwise into the above solution, stirring while adding dropwise. After stirring vigorously for 5 hours, use 1.0 mol / L sulfuric acid to adjust the pH of the solution to 9.0. At this time, a large amount of white precipitates are produced in the reaction solution; then weigh 0.657 g of isopropyl titanate and add 15 mL of water to form a solution, Add it dropwise to the above reaction solution, and stir vigorously for 5 hours at a temperature of 20°C to obtain a gel, then transfer the obtained gel to a stainless steel hydrothermal reaction kettle, crystallize at 100°C for 48 hours, and then Filtered, washed with deionized water, and dried at 80°C. After drying, grind the blocky white sol...

Embodiment 2

[0036] Preparation of Ti-MCM-41 molecular sieve:

[0037]The amount of isopropyl titanate in Example 1 was changed to 0.9865g, the sulfuric acid concentration was changed to 0.8mol / l, the crystallization time was changed to 24h, the heating rate was changed to 10°C / min, and the calcination temperature was changed to 600°C. The calcination time was changed to 5h. Others are the same as embodiment 1. 2.2g of Ti-MCM-41 molecular sieve catalyst was prepared, which has a mesoporous structure as detected by XRD, in which the molar ratio of Si:Ti is 1:0.05, and the specific surface area is 869.03m2 as detected by nitrogen adsorption and desorption. 2 / g.

[0038] Ti-MCM-41 molecular sieve catalyst catalyzes the reaction of dimethylamine and ethylene oxide:

[0039] The reaction adopts a high-pressure reactor reactor, and dimethylamine (78.89g, 1.75mol) is mixed with ethylene oxide (22.03g, 0.5mol), and the catalyst 1.0g prepared above is mixed at a reaction temperature of 140°C an...

Embodiment 3

[0041] Preparation of Ti-MCM-41 molecular sieve:

[0042] Change the mass of isopropyl titanate in Example 1 to 1.973g, the sulfuric acid concentration to 0.6mol / l, the crystallization time to 36h, the heating rate to 12°C / min, and the calcination temperature to 650°C, The calcination time was changed to 7h. Others are the same as in Example 1, and 2.1 g of Ti-MCM-41 molecular sieve catalysts are obtained, which has a mesoporous structure as detected by XRD, wherein, the molar ratio of Si:Ti is 1:0.1, and the specific surface area is 681.95 m by nitrogen adsorption and desorption detection. 2 / g.

[0043] Ti-MCM-41 molecular sieve catalyst catalyzes the reaction of aniline and phenyloxirane:

[0044] The reaction adopts a high-pressure reactor reactor, aniline (162.98g, 1.75molmol) is mixed with phenyloxirane (60.08g, 0.5mol), and the catalyst 0.2g prepared above is mixed at a reaction temperature of 160°C and a reaction pressure of The reaction was carried out under the co...

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Abstract

The invention provides a catalytic synthesis method of an N-substituted ethanol amine compound. The synthesis method includes the steps that an epoxy compound shown by the formula (II) (please see the specification), an amine compound shown by the formula (III) (please see the specification) and a metal-heteroatom-modified MCM-41 molecular-sieve-mesoporous catalyst are mixed and reacted for 40-100 min under the condition that the reaction temperature ranges from 60 DEG C to 190 DEG C, and the reaction pressure ranges from 1 MPa to 3.5 MPa, the catalyst in the reaction liquid is filtered out, and the N-substituted ethanol amine compound is obtained. According to the catalytic synthesis method, the catalyst is easy to prepare, large in specific surface area and long in service life, has abundant acidity active sites, and has the quite good catalytic performance in the process of synthesizing N-substituted ethanol amine through amine and an epoxy compound with the liquid phase method; the conversion rate of the amine is high, the selectivity of the N-substituted ethanol amine is good, the reaction condition is mild, and industry enlargement production is facilitated.

Description

(1) Technical field [0001] The invention relates to a catalytic synthesis method of N-substituent ethanolamine compounds, in particular to a method for catalytically synthesizing N-substituent ethanolamine compounds with a metal heteroatom-modified MCM-41 molecular sieve mesoporous catalyst. (2) Background technology [0002] N-substituent ethanolamine compounds are important fine chemical products, which are widely used in desulfurization and decarburization agents in chemical fertilizer plants, synthetic ammonia plants, oil refineries, and pharmaceutical plants, as well as in the production of pharmaceutical intermediates, coating solvents, and non-ionic detergents. agents, emulsifiers, and activators. It can be used to prepare polyurethane foam, coatings, paints, inks, and can also be used in the synthesis of water-soluble coating resins, water treatment of polyurethane coatings, gas treatment, ion exchange resins, papermaking additives and leather, textile additives, esp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/60C07C215/08C07C215/16C07C215/30B01J29/03
CPCC07C209/60B01J29/0308B01J29/0333B01J2229/183B01J2229/186C07C215/08C07C215/16C07C215/30
Inventor 陈爱民王后勇刘锐薄盈盈胡军
Owner ZHEJIANG UNIV OF TECH
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