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Process for preparing of [gamma]-butyrolactone and n-methyl pyrrolidone from 1,4-butanediol

A technology of butyrolactone and butanediol, which is applied in the field of preparing γ-butyrolactone and N-methylpyrrolidone from 1,4-butanediol, which can solve the problem of reduced catalyst activity and difficulty in using the catalyst for a long time, etc. problem, to achieve the effect of reducing the formation of by-products, improving selectivity and yield, and high cost efficiency

Active Publication Date: 2011-04-27
SK INNOVATION CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Due to the reduction of catalyst activity, the above catalytic methods require frequent regeneration of the catalyst and separation of the product
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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  • Process for preparing of [gamma]-butyrolactone and n-methyl pyrrolidone from 1,4-butanediol
  • Process for preparing of [gamma]-butyrolactone and n-methyl pyrrolidone from 1,4-butanediol
  • Process for preparing of [gamma]-butyrolactone and n-methyl pyrrolidone from 1,4-butanediol

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preparation example Construction

[0035] Preparation of the present invention The method for preparing gamma-butyrolactone (GBL) comprises reacting 1,4-butanediol in the presence of a non-chromium catalyst containing oxides of Cu and Zr to obtain gamma-butyrolactone.

[0036] More specifically, the method of the present invention for producing γ-butyrolactone comprises reacting 1,4-butanediol in the presence of a binary catalyst (oxides of Cu and Zr) to obtain γ-butyrolactone.

[0037] In the binary catalyst, the element composition Cu:Zr is 1:0.001-80.

[0038] In the first embodiment of the method of the present invention which provides excellent yield and selectivity of γ-butyrolactone and shows prolonged catalyst life, in the presence of a non-chromium catalyst represented by Chemical Formula 1, 1,4- Butanediol reacts (dehydrogenates).

[0039] [chemical formula 1]

[0040] Cu a Zr b m c o x

[0041] In Chemical Formula 1, M is one or more elements selected from metals or metalloid elements other than...

Embodiment 1

[0090] Preparation of γ-butyrolactone

[0091] First, 11.630g of Cu(NO 3 ) 2 2.5H 2 O, 1.616g of Ce(NO 3 ) 3 ·6H 2 O and 8.232g of ZrO(NO 3 ) 2 ·xH 2 O was dissolved in distilled water (500 mL) to prepare a precursor solution, followed by vacuum drying at 70 °C. The dried powder was heat-treated at 500° C. for 4 hours under an air atmosphere to provide a non-chromium catalyst.

[0092] After heat treatment, the catalyst is obtained in oxide form. The obtained catalyst had the following element composition: 30.7% by weight of metallic copper, 5.4% by weight of metallic cerium, and 40.6% by weight of metallic zirconium.

[0093] A non-chromium catalyst (2 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 of the catalyst, the weight hourly space velocit...

Embodiment 2

[0095] Preparation of γ-butyrolactone

[0096] First, 11.630g of Cu(NO 3 ) 2 2.5H 2 O, 1.616g of Ce(NO 3 ) 3 ·6H 2 O and 8.232g of ZrO(NO 3 ) 2 ·xH 2 O was dissolved in distilled water (500 mL) to prepare a precursor solution, followed by vacuum drying at 70 °C, and the dried powder was heat-treated at 700 °C for 4 h in an air atmosphere to provide a non-chromium catalyst. γ-butyrolactone was obtained in the same manner as described in Example 1 except that the temperature of the heat treatment was changed.

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Abstract

The invention provides a process for preparing of [gamma]-butyrolactone (GBL) and n-methyl pyrrolidone (NMP) from 1,4-butanediol with the existence of a non-chromium catalyst. More specifically, the invention provides a method for preparing GBL with the existence of a non-chromium catalyst in an environmental friendly manner. The preparing process has high cost efficiency and high yield and selectivity. The process can be used for preparing NMP in a highly productive and stable manner. No catalyst is used in the process under a mild condition, and the obtained GBL and methylamine (MMA) aqueous solution are feed to a reactor so that the GBL and MMA aqueous solution are interreacting with each other.

Description

technical field [0001] The present invention relates to a process for the preparation of gamma-butyrolactone from 1,4-butanediol and the preparation of N-methylpyrrolidone (NMP) from 1,4-butanediol in the presence of a non-chromium catalyst, more specifically, The present invention provides a process for the environmentally friendly production of gamma-butyrolactone in the presence of a chromium-free, non-chromium catalyst, which is highly cost-effective and requires only low cost, has very high yield and selectivity, and then described method prepares N-methylpyrrolidone stably with high yield, long-term, and this preparation does not use catalyst under mild condition by the gamma-butyrolactone obtained and a monomethylamine (MMA) aqueous solution are supplied to the reactor to allow γ-butyrolactone and monomethylamine to react with each other. Background technique [0002] Many methods for producing γ-butyrolactone, which is used as an intermediate in the production of py...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72C07D207/267B01J23/80B01J23/83B01J23/86C07D307/58
CPCB01J21/066B01J23/72C07D207/267C07D307/33
Inventor 李诚浩尹永植金希洙吴承勋刘永甲朴玟奎崔奎津金庆録郑起男李在镐李成俊
Owner SK INNOVATION CO LTD
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