Catalyst for preparing gamma-butyrolactone by normal-pressure gas-phase dehydrogenation of 1,4-butanediol and preparation method thereof

A technology of butanediol and catalyst, applied in the field of catalyst preparation, can solve the problems of high price of 1,4-butanediol, increase the difficulty of manufacturing process, etc., improve the skeleton structure and pore structure, reduce the low and high shrinkage rate active effect

Active Publication Date: 2017-02-08
MAIQI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Usually γ-butyrolactone is obtained by dehydrogenating 1,4-butanediol as a raw material, but 1,4-butanediol is more expensive
Mitsubishi Chemical Corporation has developed a method for producing γ-butyrolactone from maleic anhydride in liquid phase hydrogenation, but this method needs to be reacted under high pressure conditions, which increases the difficulty of the manufacturing process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 1000ml of deionized water, add 152g of copper nitrate, 91.4g of zinc nitrate, 117.7g of aluminum nitrate in turn, fully dissolve and heat up to 65°C, add 250g of polyethylene glycol-800, stir well, and then add SiO 2 30g of silica gel with a content of 30%, stir well to make it evenly mixed, control the temperature of the mixed liquid at 55-65°C, lubricating oil precipitant 1.5M Na 2 CO 3 Solution, the pH value of the control liquid terminal system is 8.0, under stirring, the temperature of the mixed system is raised to 85 ° C, sinking for 5 hours, filtered, washed, and dried at 110 ° C for 15 hours, the dried product is in the Calcined at 545-555° C. for 4.5 hours, and when it was naturally cooled to room temperature, 1.5% graphite was added as a lubricant to prepare a molded Φ5×5mm catalyst sample.

[0026] Take 10ml of the above sample catalyst with a particle size of 20-40 mesh, put it into the isothermal section of a Φ12×600mm fixed-bed reactor, and start hea...

Embodiment 2

[0028] Take 800ml of deionized water, add 116.7g of copper nitrate, 127.9g of zinc nitrate, and 95.6g of aluminum nitrate in turn, fully dissolve and heat up to 70-80°C, add 200g of polyethylene glycol-1000, mix well, and add SiO 2 65g of silica sol with a content of 20%. After stirring evenly, control the temperature of the mixing system at 65-75°C, and add 1.5M NaHCO 3 Precipitating agent in the mixed system, control the end point pH value to 7.5, settle at 80°C for 8 hours, filter, wash with deionized water, dry at 110-120°C for 12 hours, bake at 450°C for 6 hours, cool down to room temperature naturally, add 1.5% graphite was used as a lubricant to prepare a molded Φ5×5mm catalyst sample.

[0029] The catalyst activation conditions are the same as Example 1, the reaction temperature is 240°C, the hydrogen-alcohol ratio is 10, and the liquid hourly pore velocity is 2.0h -1 , The conversion rate of the catalyst to 1,4-butanediol is 99.1%, and the selectivity of 1,4-butaned...

Embodiment 3

[0031] Take 800ml of deionized water, add 167g of copper nitrate, 73.5g of zinc nitrate, and 75g of aluminum nitrate in sequence. After fully dissolving, heat up to 80-90°C, add 130g of polyethyl alcohol-1500, mix well, and add SiO 2 100g of silica sol with a content of 15%, stir well, mix evenly, control the temperature of the mixture at 75-85°C, add 1.5M Na 2 CO 3 and NaHCO 3 Composite precipitant (Na 2 CO 3 : NaHCO 3 =1:1 molar ratio), control the pH value of the precipitation end point to 7.5, sink at 90°C for 4 hours, filter, wash, and dry the filter cake at 100-110°C for 18 hours, and the dried product is at 645-655°C Roast for 4 hours, cool down to room temperature naturally, add 1.5% graphite as a lubricant, and prepare a molded Φ5×5mm catalyst sample.

[0032] The catalyst activation conditions are the same as in Example 1, the reaction temperature is 300°C, and the liquid hourly pore velocity is 2.75h -1 , the ratio of hydrogen to alcohol is 8, the conversion r...

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Abstract

The invention relates to a catalyst for preparing gamma-butyrolactone by gaseous phase dehydrogenation of 1, 4-butanediol under normal pressure and a preparation method thereof. The catalyst is composed of CuO, ZnO, Al2O3 and SiO2, and the unreduced catalyst is prepared from the following ingredients by weight percentage: 30-60% of CuO, 15-50% of Zn, 5-25% of Al2O3 and 10-30% of SiO2. The grain diameter of the catalyst is phi 5*5mm, and the catalyst is easy to restore, and has high activity and high selectivity, and long service life under a reaction process condition; the conversion rate of 1, 4-butanediol is greater than or equal to 99%, and the selectivity of the 1,4-butanediol for generating gamma-butyrolactone is greater than or equal to 96.5%.

Description

technical field [0001] The patent of the present invention relates to a preparation method of a γ-butyrolactone catalyst. Background technique [0002] r-butyrolactone is a chemical reagent in great demand, for example, as a solvent for polyacrylonitrile, ester fiber, polystyrene, shellac and resins, etc., and as a raw material for the preparation of important economic products, such as: pyrrolidone, N-methylpyrrolidone and polyvinylpyrrolidone. [0003] Usually γ-butyrolactone is obtained by dehydrogenating 1,4-butanediol as a raw material, but 1,4-butanediol is more expensive. Mitsubishi Chemical Corporation has developed a method for producing γ-butyrolactone from maleic anhydride in liquid phase hydrogenation, but this method needs to be reacted under high pressure conditions, which increases the difficulty of the manufacturing process. About taking maleic acid dialkyl ester as raw material, the method for preparing gamma-butyrolactone by gas-phase hydrogenation mode a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/80C07D307/33
Inventor 肖强宋国全崔炳春杨国松杨理闫广学夏成浩吴彦彬
Owner MAIQI CHEM CO LTD
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