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A phthalide purification method and a method for preparing phthalide from phthalic anhydride

A technology of phthalide and phthalic anhydride, which is applied in the field of organic catalysis, can solve problems such as many by-products, poor catalyst stability, and limited loading of active components, and achieve the effects of simple process, easy-to-obtain raw materials, and high-purity products

Inactive Publication Date: 2017-11-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] CN103433043A discloses a catalyst for preparing phthalide by hydrogenation of phthalic anhydride with high selectivity, a supported monometallic and bimetallic catalyst prepared with hydrotalcite or hydrotalcite-like material as a precursor, which has high activity for hydrogenation of phthalic anhydride and high activity for phthalide Has high selectivity, yet the by-product in the phthalide crude product that obtains in the disclosed method of this prior art is many and is difficult for separation and purification
The catalyst obtained by this method is poorly stable, and the active ingredient Ni nanoparticles are easily agglomerated on the surface of the carrier.
In addition, using the prepared supported nickel-based catalyst, the loading amount of the active ingredient is limited to a certain extent, and it is difficult to prepare a catalyst with high dispersion and high loading amount.

Method used

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  • A phthalide purification method and a method for preparing phthalide from phthalic anhydride
  • A phthalide purification method and a method for preparing phthalide from phthalic anhydride

Examples

Experimental program
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Effect test

preparation example 1

[0052] Preparation Example 1: Ni / La-Al 2 o 3 catalyst

[0053] Calcining 20g of pseudo-boehmite at 600°C for 4h to obtain γ-Al 2 o 3 powder, then use 2mol / L La(NO 3 ) 3 The solution was impregnated in equal volume at 30°C for 12h, dried and calcined at 500°C for 12h to prepare lanthanum-modified γ-Al 2 o 3 carrier. Add ammonia water to 5mol / L nickel nitrate aqueous solution and stir at room temperature, then the lanthanum-modified γ-Al 2 o 3 Add the carrier into the solution, adjust the pH value to 10, react at 100°C for 3h, filter and dry, and roast at 400°C for 5h to obtain the catalyst Cat1.

[0054] Detected by atomic emission spectroscopy, in the lanthanum-modified γ-Al 2 o 3 In the carrier, the content of lanthanum as oxide is 2.1% by weight; in the catalyst Cat1, the content of nickel element as oxide is 24.8% by weight.

preparation example 2

[0056] Calcining 50g of pseudo-boehmite at 800°C for 8h to obtain α-Al 2 o 3 , and then use 1mol / L Ba(NO 3 ) 2 The solution was impregnated in equal volume at 35 °C for 12 h, dried and then calcined at 700 °C for 5 h to obtain barium-modified α-Al 2 o 3 carrier. Under stirring conditions at 55°C, the barium-modified α-Al 2 o 3 The carrier was placed in an aqueous solution containing nickel nitrate (6 mol / L) and molybdenum nitrate (4 mol / L) for 20 h. After being filtered and dried, it was calcined at 700° C. for 4 hours to obtain the catalyst Cat2.

[0057] Detected by atomic emission spectroscopy, in the barium-modified α-Al 2 o 3 In the carrier, the content of barium as oxide is 2.8% by weight; in the catalyst Cat2, the content of nickel as oxide is 25.2% by weight; the content of molybdenum as oxide is 16.3% by weight %.

preparation example 3

[0059] 100g of ZSM-22 powder was calcined at 600°C for 6h, and then 2mol / L of Ca(NO 3 ) 2 The solution was impregnated in equal volume at 40°C for 10h, dried and then calcined at 650°C for 8h to prepare the calcium-modified ZSM-22 carrier. Add ammonia water to 3mol / L nickel nitrate aqueous solution for stirring at room temperature, then add the calcium-modified ZSM-22 carrier into the solution, adjust the pH value to 10, react at 120°C for 6h, and filter and dry After that, it was calcined at 400°C for 5h to obtain the catalyst Cat3.

[0060] Detected by atomic emission spectroscopy, in the calcium-modified ZSM-22, the content of calcium in terms of oxides is 2.8% by weight; in the catalyst Cat3, the content of nickel in terms of oxides is 39.7% by weight %.

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Abstract

The invention relates to the field of organic catalysis and discloses a phthalide purification method. The method includes dissolving a phthalide crude product to be purified into an organic solvent, then adding one part of a solventing-out agent into the obtained solution, adding a phthalide crystal seed into the solution when the solution becomes muddy, and then adding the other part of the solventing-out agent into the solution under stirring. The organic solvent is at least one selected from ethanol, acetone, tetrahydrofuran, methanol and diethyl ether. The solventing-out agent is at least one selected from water, acetonitrile and cyclohexane. The invention also discloses a method for preparing phthalide from phthalic anhydride, and the method includes (1) a step of preparing a phthalide crude product, namely a step of subjecting phthalic anhydride to catalytic hydrogenation with the existence of a catalyst and a solvent to obtain the phthalide crude product; and (2) a step of phthalide purification, namely a step of purifying the phthalide crude product in the step (1) by adopting the phthalide purification method mentioned above. The methods when being used for phthalide crude product purification and phthalide preparation from phthalic anhydride have advantages of simple processes, easily available raw materials, and high purity of obtained products.

Description

technical field [0001] The invention relates to the field of organic catalysis, in particular to a method for purifying phthalide and a method for preparing phthalide from phthalic anhydride. Background technique [0002] Phthalide (o-hydroxymethylbenzoic acid lactone) is an important fine chemical intermediate, mainly used in the production of dye intermediates 1,4-dichloroanthraquinone, 1-chloroanthraquinone, anticoagulant benzene Indandione, fungicide tetrachlorophthalide, anxiolytic drug doxepin. In addition, phthalide can also be used as an intermediate in organic synthesis, for the synthesis of doxepin, dye vat brown BR, and butylphthalide for the treatment of ischemic stroke. [0003] In the traditional process, phthalide is mainly obtained by reduction of phthalimide or selective hydrogenation of phthalic anhydride. The selective hydrogenation of phthalic anhydride to prepare phthalide has the advantages of simple process, high product yield, good quality, low cost...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/88
CPCC07D307/88
Inventor 梁长海施俊林陈雷陈平靳少华梁大立杨凯旋张亮亮邸鑫
Owner CHINA PETROLEUM & CHEM CORP
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