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Catalyst for [gamma]-butyrolactone preparation through dimethyl maleate hydrogenation, and preparation method thereof

A dimethyl maleate, catalyst technology, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of catalyst activity and γ-butane Low lactone selection, complex catalyst preparation process, etc., to achieve high activity and selectivity, simple preparation method, and low environmental pollution.

Active Publication Date: 2015-03-11
中科合成油内蒙古技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst is used for the hydrogenation of dimethyl maleate to prepare γ-butyrolactone. Although it does not contain chromium with serious pollution and strong toxicity, the preparation process of the catalyst is complicated, and the catalyst activity and γ-butyrolactone selection also lower

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1, the preparation of catalyst and catalytic performance

[0036] (1) Preparation of catalyst

[0037] Weigh copper nitrate 111g, 30wt% acidic silica sol 110g, 50wt% manganese nitrate aqueous solution 8.57g, dissolve them in 500g deionized water, prepare metal salt solution, wherein, the molar concentration of copper nitrate is 0.92M, the molar concentration of manganese nitrate The concentration is 0.048M, and the molar concentration of acidic silica sol is 1.10M. Stir the salt solution and 1M ammonium bicarbonate aqueous solution precipitant at 50°C, co-precipitate, the precipitation pH is controlled at 6.2, the time required for precipitation is about 1 hour, after the precipitation is completed, aging for 1 hour, the precipitate is washed and filtered , dried at 110°C for 24 hours, and fired at 450°C for 5 hours. Finally, 1 wt% graphite powder was added to the precipitate and pressed into a tablet to obtain a catalyst sample.

[0038] The mass percent ...

Embodiment 2

[0044] Embodiment 2, the preparation of catalyst and catalytic performance

[0045] (1) Preparation of catalyst

[0046] Weigh 115.44g of copper nitrate, 107.39g of 30wt% acidic silica sol, 5.73g of 50wt% manganese nitrate aqueous solution, and other conditions are the same as in Example 1.

[0047] The mass percent composition of the catalyst sample (active ingredient) prepared in this embodiment is composed of: CuO 53.12%, SiO 2 44.94% and MnO 2 1.94%.

[0048] (2) Catalytic performance of the catalyst

[0049] The catalyst prepared above was used to catalyze the synthesis of γ-butyrolactone from dimethyl maleate, and the specific steps and dosage were the same as those in Example 1.

[0050]Wherein, the above reaction is carried out under the following conditions: the reaction temperature is 227°C, the pressure is 0.05MPa, and the liquid space velocity is 0.53h -1 , The hydrogen / ester molar ratio is 25:1.

[0051] After testing, the catalytic performance of the cataly...

Embodiment 3

[0053] Embodiment 3, the preparation of catalyst and catalytic performance

[0054] (1) Preparation of catalyst

[0055] Weigh 121.1 g of copper nitrate, 100.2 g of 30 wt % acidic silica sol, 7.3 g of 50 wt % manganese nitrate aqueous solution, and other conditions are the same as in Example 1.

[0056] The mass percent composition of the catalyst sample (active ingredient) prepared in this embodiment is composed of: CuO 55.68%, SiO 2 41.85% and MnO 2 2.47%.

[0057] (2) Catalytic performance of the catalyst

[0058] The catalyst prepared above was used to catalyze the synthesis of γ-butyrolactone from dimethyl maleate, and the specific steps and dosage were the same as those in Example 1.

[0059] Wherein, the above reaction is carried out under the following conditions: the reaction temperature is 231°C, the pressure is 0.05MPa, and the liquid space velocity is 0.58h -1 , The hydrogen / ester molar ratio is 20:1.

[0060] After testing, the catalytic performance of the c...

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Abstract

The present invention discloses a catalyst for [gamma]-butyrolactone preparation through dimethyl maleate hydrogenation, and a preparation method thereof, wherein the active components of the catalyst comprise CuO, SiO2 and MnO2, and the mass contents of CuO, SiO2 and MnO2 in the catalyst are respectively 51-56%, 41-46% and 1.0-3.0%. The catalyst preparation method comprises: (1) respectively preparing a soluble salt solution of copper, a soluble salt solution of manganese and an acid silica sol solution, and mixing to obtain a mixed solution; (2) adding an alkaline precipitating agent to the mixed solution, and carrying out cocurrent flow co-precipitation; and (3) aging after completing the cocurrent flow co-precipitation, filtering to obtain the precipitate, sequentially drying and calcinating the precipitate, and then adding graphite powder to form so as to obtain the finished product. Compared with the catalyst in the prior art, the catalyst of the present invention has advantages of no chromium, low environmental pollution, simple preparation method, high activity and high selectivity, wherein the dimethyl maleate conversion rate is up to 100%, and the [gamma]-butyrolactone selectivity is up to 92-93%.

Description

technical field [0001] The invention relates to a catalyst for hydrogenating dimethyl maleate to prepare gamma-butyrolactone and a preparation method thereof, belonging to the field of fine chemicals. Background technique [0002] γ-butyrolactone is an important organic chemical raw material and intermediate, widely used in medicine, pesticide, petrochemical and other fields. In medicine, γ-butyrolactone is mainly used to synthesize pyrrolidone, N-methylpyrrolidone, vinylpyrrolidone, etc. In addition, because γ-butyrolactone has the advantages of high boiling point, strong solubility, high conductivity, and good stability, it is often used as an extractant, absorbent, and electrolyte solution. [0003] At present, the production methods of γ-butyrolactone in industry include 1,4-butanediol dehydrogenation method, maleic anhydride hydrogenation method and maleic acid dialkyl ester hydrogenation method. Wherein, the dialkyl maleate in the hydrogenation method of dialkyl male...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/889C07D307/33
Inventor 李显清朱玉雷杨勇李永旺付子斌边定国侯潇云周明君
Owner 中科合成油内蒙古技术研究院有限公司
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