Method for preparing n-methylpyrrolidone from 1,4-butanediol

A technology of methylpyrrolidone and butanediol, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc. Reduce activity and other issues, achieve the effects of inhibiting the formation of by-products, prolonging catalyst life, and improving cost-effectiveness

Inactive Publication Date: 2011-05-25
SK INNOVATION CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] However, the above catalytic methods require frequent regeneration of the catalyst and separation of the product due to reduced catalyst activity.
As a result, it is difficult to use the catalyst for a long time, and the catalyst-free method is more economically efficient

Method used

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  • Method for preparing n-methylpyrrolidone from 1,4-butanediol
  • Method for preparing n-methylpyrrolidone from 1,4-butanediol
  • Method for preparing n-methylpyrrolidone from 1,4-butanediol

Examples

Experimental program
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Effect test

Embodiment 1

[0049] Copper nitrate, zinc nitrate, and aluminum nitrate were dissolved in distilled water (500 mL) to provide a metal precursor solution, followed by vacuum drying at 70°C. Then, the dry powder was fired at 500° C. for 4 hours in an air atmosphere. Here, each metal nitrate is weighed and dissolved in such a manner that each metal nitrate conforms to the composition of the final metal oxide obtained after firing.

[0050] As a result, a catalyst in the form of an oxide was obtained with the following elemental composition: CuO 51% by weight, ZnO 31% by weight and Al 2 o 3 18% by weight.

[0051] The catalyst (5 g) in the form of the resulting powder was charged into a fixed-bed reactor made of SUS with an inner diameter of 3 / 4 inch. Then, at 4kg / cm 2 The reduction was carried out using hydrogen at a pressure of G and a temperature of 250° C. for 4 hours. After the reduction reaction of the catalyst, at a reaction temperature of 240°C, the weight hourly space velocity (W...

Embodiment 2

[0054] N-Methylpyrrolidone was prepared in the same manner as described in Example 1, except that the final catalyst had a composition of CuO 53 wt%, ZnO 32 wt%, Al 2 o 3 12.5% ​​by weight, Ce 2 o 3 2% by weight and Na 2 O 0.5% by weight mode weighed and used each metal nitrate.

Embodiment 3

[0056] N-Methylpyrrolidone was prepared in the same manner as described in Example 1, except that the final catalyst had a composition of CuO 76% by weight, SiO 2 19.5 wt%, MgO3 wt% and Cr 2 o 3 Each metal nitrate was weighed and used in a manner of 1.5% by weight.

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Abstract

The invention provides a method for preparing gamma-butyrolactone (GBL) and N-methylpyrrolidone (NMP), more specifically, a method for preparing NMP, comprising introducing 1,4-butanediol in a reactor, performing dehydrogenation in the presence of metallic oxide catalyst to provide GBL; supplying monomethyl amine (MMA) aqueous solution and GBL to the reactor; separating the NMP generated by the reaction of the MMA and the GBL from the water; mixing the separated water with the MMA to provide the MMA aqueous solution; and leading the MMA aqueous solution back into the reactor. Since the GBL is prepared from the butanediol in the presence of the catalyst, the water generated from the reaction of the MMA and the GBL is collected to provide the MMA aqueous solution, and the MMA aqueous solution is returned to the reactor, the prepared NMP has the advantages that energy is saved and simple separation of the product NMP is realized.

Description

technical field [0001] The present invention relates to a method for preparing N-methylpyrrolidone (NMP), more particularly, to a method for preparing N-methylpyrrolidone as follows, wherein 1,4-butanediol (BDO) is introduced into a reactor In, and in the presence of metal oxide catalyst dehydrogenation to provide γ-butyrolactone (GBL); supply monomethylamine (MMA) aqueous solution and γ-butyrolactone to the reactor; will be produced by monomethylamine and γ- The N-methylpyrrolidone produced by the reaction of butyrolactone is separated from water; the separated water is mixed with monomethylamine to provide an aqueous solution of methylamine, which is then returned to the reactor. Background technique [0002] Several methods are known for the preparation of gamma-butyrolactone (GBL), which is used as an intermediate for the preparation of pyrrolidones such as N-methyl-2-pyrrolidone (NMP), by dehydrogenation of butanediol. [0003] Japanese Patent Publication No. 2-27349 a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/267B01J23/80B01J23/83B01J23/86B01J23/889
CPCB01J27/25C07D207/263C07D207/267C07D207/27
Inventor 朴玟奎刘永甲崔奎津李诚浩李在镐尹永植郑起男李成俊崔先吴承勋金希洙
Owner SK INNOVATION CO LTD
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