Method for preparing N-methylpyrrolidine through catalysis

A methylpyrrolidine and catalytic preparation technology, applied in chemical instruments and methods, molecular sieve catalysts, physical/chemical process catalysts, etc., can solve the problems of high price of tetrahydropyrrole, increased difficulty in industrialization, and limited industrial application, etc. Raw material conversion rate and reaction selectivity, low price, low cost effect

Active Publication Date: 2018-07-20
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Application Information

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Problems solved by technology

Chen Yongsheng introduced in "Chemical Intermediates", 2008, 08: (19-21), using H-13X molecular sieves to catalyze tetrahydropyrrole and methanol to synthesize N-methylpyrrolidine. The reaction temperature of this method is 300 ° C, tetrahydropyrrole : Methanol=1:3, the yield of N-methylpyrrolidine is 83.8%, the raw material tetrahydropyrrole of this reaction is expensive, resulting in high cost and i

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Accurately weigh 4.5g 1,4-butanediol (0.05mol), 7.75g 40wt.% methylamine aqueous solution (containing 0.1mol methylamine), 0.45 g ZSM-5 (NKF-5-80HW) loaded with CuO and NiO Catalyst (Cu and Ni content are both 3%), in a 100mL reactor, in H 2 React under (1MPa) atmosphere, set the reaction temperature at 300°C, and finish the reaction after 6 hours of reaction. The conversion rate of 1,4-butanediol is greater than 99%, and the yield of N-methylpyrrolidine is 92%.

Embodiment 2

[0024] The specific feeding process and reaction mode are the same as in Example 1, and the reaction time is set to 4 hours. After the reaction, the conversion rate of 1,4-butanediol is greater than 92%, and the yield of N-methylpyrrolidine is 82%.

Embodiment 3

[0026] Weigh 9g of 1,4-butanediol, 23.2g of 40% methylamine aqueous solution (containing 0.3mol methylamine), 0.9g ZSM-5 (NKF-5-80HW) loaded CuO and NiO catalysts (Cu and Ni content are both is 3%), at H 2 The reaction was carried out under (1 MPa) atmosphere, the reaction temperature was set at 270°C, and the reaction was completed after 6 hours of reaction. The conversion rate of 1,4-butanediol was 92%, and the yield of N-methylpyrrolidine was 90%.

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PUM

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Abstract

The invention discloses a method for preparing N-methylpyrrolidine through catalysis. According to the method, 1,4-butanediol and a methylamine water solution which are used as raw materials react inan H2 reduction atmosphere at the reaction temperature of 230-330 DEG C and under the pressure of 4-10 Mpa for 1-8 h with a supported bimetal oxide as a catalyst to produce N-methylpyrrolidine. A supporter of the catalyst is an Al2O3, SiO2 or ZSM-5 molecular sieve, and active components are CuO and NiO. The method has the advantages that the reaction time is short, the catalyst is low in cost andreusable, the product yield is high and the like.

Description

technical field [0001] The invention relates to a method for preparing N-methylpyrrolidine from an aqueous solution of 1,4-butanediol and methylamine in the presence of a supported double metal oxide catalyst. Background technique [0002] N-Methylpyrrolidine is a cyclic secondary amine, which is mainly used for the preparation of broad-spectrum antibiotics cefepime and acetidine, and can also be used as a dye stabilizer, preservative, and ionic liquid. The existing N-methylpyrrolidine preparation methods mainly include: US4892959 adopts N-methylpyrrolidone and hydrogen to catalytic hydrogenation under the conditions of Cu-Al or Cu-Cr catalyst, the conversion rate is 85%, and the selectivity is 85%. The reaction pressure is as high as 150atm-280atm, which requires strict equipment and requires a large investment. CN1810787 adopts 1,4-dichlorobutane and monomethylamine to prepare N-methylpyrrolidine in a reactor, the reaction temperature is 50-180 ℃, and the reaction pressur...

Claims

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Application Information

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IPC IPC(8): C07D295/03C07D295/023B01J29/46B01J23/755
CPCB01J23/755B01J29/46C07D295/023C07D295/03
Inventor 邓友全龙焱刘士民卢六斤马祥元何昱德
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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