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Process for catalytic synthesis of phthalide from phthalic anhydride

A technology of phthalide and phthalic anhydride, which is applied in the field of catalytic synthesis of phthalide from phthalic anhydride, which can solve the problems of environmental pollution and easy crushing of catalysts, and achieve the effects of environmental friendliness, high activity and stability, and low post-processing cost

Inactive Publication Date: 2006-12-27
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the Raney Ni catalyst will cause environmental pollution during preparation, and there is a problem that the catalyst is easily crushed during the reaction process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Preparation of catalyst by impregnation method:

[0017] 1) Pretreatment of the carrier, the SiO 2 The carrier is calcined at 400-600°C for 3-5 hours;

[0018] 2) loading active components, the carrier pretreated in step 1) is impregnated with an aqueous nickel nitrate solution with a nickel content of 10% by weight for 6 hours at 20° C., then dried at 110° C., and calcined at 500° C. for 4 hours, Finally, the catalyst for the hydrogenation of phthalic anhydride to phthalide can be obtained after reduction at 500° C. for 3 hours in a hydrogen atmosphere.

[0019] 700 mg Ni / SiO 2 The catalyst was added into a 100 ml autoclave, and then 17.8 grams of phthalic anhydride and 41.5 grams of solvent phthalide were added into the autoclave. The reaction temperature was 150° C., the reaction hydrogen pressure was 3.0 MPa, and the reaction time was 4 hours. The conversion rate of phthalic anhydride was 85.5%, and the recovery of phthalide The rate is 69.7%.

Embodiment 2

[0021] Catalyst preparation process is the same as embodiment 1, and difference is that catalyst uses TiO 2 -ZrO 2 As a carrier, the nickel content is 15wt%. 700 mg Ni / TiO 2 -ZrO 2 The catalyst was added into a 100 ml autoclave, the reaction temperature was 170° C., the reaction hydrogen pressure was 3.2 MPa, other conditions were the same as in Example 1, and the reaction time was 5 hours. The conversion rate of phthalic anhydride was 93.3%, and the yield of phthalide was 88.7%.

Embodiment 3

[0023] Catalyst preparation process is the same as embodiment 2, and difference is that catalyst uses TiO 2 -SiO 2 as the carrier. 700 mg Ni / TiO 2 -SiO 2 The catalyst was added into a 100 ml autoclave, the reaction temperature was 180° C., the reaction hydrogen pressure was 3.0 MPa, other conditions were the same as in Example 1, and the reaction time was 6 hours. The conversion rate of phthalic anhydride was 98.5%, and the yield of phthalide was 91.4%.

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Abstract

The invention relates to a method for synthesizing phthalide catalyzed by benzoic anhydride in liquid phase, especially relates to method with loading nickel catalyst. Said method employs phthalide as reacting solvent, prepares phthalide through selective hydrogenation with benzoic anhydride under catalysis of loading nickel catalyst; the ratio by weight between said benzoic anhydride and phthalide is 1: 0.1-10, the reacting temperature is 130-200 Deg. C, reacting pressure is 1.0-5.0 Mpa; said loading nickel catalyst is catalyst with nickel loaded on SiO2, diatom earth, activated char, TiO2, ZrO2, TiO2-SiO2, TiO2-Al2O3 or TiO2-ZrO2, and the loading amount of nickel is 5-50 wt.%. The invention is characterized by high activity and stability of used loading nickel catalyst, no pollution of process, direct usage of phthalide as solvent, low cost for post treatment, and simple process.

Description

(1) Technical field [0001] The invention relates to a method for catalytically synthesizing phthalide by phthalic anhydride liquid-phase hydrogenation, in particular to a method for catalytically synthesizing phthalide with phthalic anhydride under the action of a loaded nickel catalyst. (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 phth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/88B01J23/755B01J32/00
Inventor 刘迎新严巍王桂林施介华王纪康
Owner ZHEJIANG UNIV OF TECH
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