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Method for preparing phthalide by benzoic anhydride liquid phase hydrogenation with gold-base catalyst

A technology for hydrogen preparation and phthalic anhydride liquid, which is applied in the field of phthalide preparation by liquid-phase hydrogenation of phthalic anhydride, can solve the problems of no metal oxide gold-based hydrogenation catalyst, no gold catalyst, etc., and achieve excellent hydrogenation activity and selectivity , High single-pass yield, no environmental pollution

Inactive Publication Date: 2008-11-12
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But so far, there is no literature report on the use of gold catalysts in the selective hydrogenation of phthalic anhydride.
In addition, there have been no research reports on metal oxides regulating the performance of gold-based hydrogenation catalysts so far.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] TiO 2 The carrier was roasted at 500°C for 4 hours; the chloroauric acid with a gold content of 2% by weight was dissolved in a certain amount of deionized water, and the NaOH aqueous solution of 1mol / L was added to adjust its pH value to 7-8, and then the treated The carrier was added to the above solution, the precipitation temperature was controlled at 80 ° C, and the pH value was maintained at 7 to 8. After the precipitation process was completed, it was left at room temperature for 3 hours, filtered, and the filter cake was washed with water until the washing liquid was washed with AgNO 3 The solution does not detect Cl - , then dried at 110°C for 12 hours, calcined at 300°C for 4 hours, and heated at 200°C with H 2 Restoration for 3 hours.

[0029]Dissolve 6 grams of phthalic anhydride in 50ml of solvent γ-butyrolactone, add to the autoclave, and add 1.2 grams of gold catalyst; replace the air in the kettle with hydrogen for 4 times, then fill the hydrogen press...

Embodiment 2

[0031] TiO 2 The carrier was roasted at 500° C. for 4 hours; the chloroauric acid with a gold content of 1.5% by weight was dissolved in a certain amount of deionized water, and the NaOH aqueous solution of 1mol / L was added to adjust its pH value to 7-8, and then the carrier TiO 2 Add it to the above solution, control the precipitation temperature at 80°C, and maintain the pH value at 7-8. After the precipitation process is over, let it stand at room temperature for 3 hours, filter, and wash the filter cake with water until the washing liquid is washed with AgNO 3 The solution does not detect Cl - , then dried at 110°C for 12 hours, calcined at 300°C for 4 hours, and heated at 200°C with H 2 Restoration for 3 hours.

[0032] Dissolve 6 grams of phthalic anhydride in 50ml of solvent γ-butyrolactone, add to the autoclave, and add 1.2 grams of gold catalyst; replace the air in the kettle with hydrogen for 4 times, then fill the hydrogen pressure and maintain 3.2MPa, raise the t...

Embodiment 3

[0034] TiO 2 The carrier was roasted at 500°C for 4 hours; the chloroauric acid with a gold content of 2% by weight was dissolved in a certain amount of deionized water, and the NaOH aqueous solution of 1mol / L was added to adjust its pH value to 7-8, and then the treated The carrier was added to the above solution, the precipitation temperature was controlled at 80 ° C, and the pH value was maintained at 7 to 8. After the precipitation process was completed, it was left at room temperature for 3 hours, filtered, and the filter cake was washed with water until the washing liquid was washed with AgNO 3 The solution does not detect Cl - , then dried at 110°C for 12 hours, calcined at 400°C for 4 hours, and heated at 200°C with H 2 Restoration for 3 hours.

[0035] Dissolve 7 grams of phthalic anhydride in 50ml of solvent γ-butyrolactone, add to the autoclave, and add 0.84 grams of gold catalyst; pass hydrogen to replace the air in the kettle for 4 times, then fill the hydrogen ...

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PUM

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Abstract

The invention discloses a method for preparing phthalide through phthalic anhydride liquid phase hydrogenation under the action of au-base catalyst. The gold-base catalyst used in the preparation method takes SiO2, ZnO, La2O3, CeO2, TiO2, ZrO2 or Fe2O3 as a carrier and takes gold as an active component, and the loading of gold is between 0.05 and 20 percent. As the gold-base catalyst used in the preparation method has excellent hydrogenation activity and selectivity under mild catalytic reaction conditions, the conversion rate of phthalic anhydride can be more than 95 percent, and the selectivity of phthalide can be more than 93 percent, thereby the single pass yield of the target product phthalide is high. Moreover, the gold-base catalyst is very good in performance stability, and more particularly, the gold-base catalyst after metal oxide modification can still maintain the selectivity over 92 percent even through the activity of the gold-base catalyst declines slightly after repeated recycling use. In addition, the gold-base catalyst provided is simple to prepare and does not pollute the environment. Therefore, the preparation method has significant advantages.

Description

(1) Technical field [0001] The invention relates to a method for preparing phthalide through liquid-phase hydrogenation of phthalic anhydride. (2) Background technology [0002] Phthalide (o-hydroxymethylbenzoic acid lactone), English name Phthalide, molecular formula C 8 h 6 o 2 , is an intermediate of fine chemicals, used in the production of anticoagulant drugs phenylindandione and phenthiazine, anxiolytic drugs doxepin, and laxatives, etc.; used in the production of fungicide tetrachlorobenzene in pesticides Phthale; In addition, it can also be used in the synthesis of dye intermediates 1,4-dichloroanthraquinone and 1-chloroanthraquinone. [0003] The synthesis methods of phthalide mainly include phthalimide method and phthalic anhydride method. The former is the reaction of phthalimide and sodium hydroxide to generate phthalide, and the yield is 80%. The raw material price of this method is relatively high, and the environmental pollution is relatively serious duri...

Claims

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Application Information

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IPC IPC(8): C07D307/88B01J23/52B01J23/89
Inventor 刘迎新邢铁锋严巍
Owner ZHEJIANG UNIV OF TECH
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