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A kind of heteropolyacid modified catalyst and its preparation and application

A technology of heteropolyacid and catalyst, which is applied in the field of heteropolyacid modified catalyst and its preparation and catalyzed oil esterification reaction system, which can solve problems such as difficult recovery, achieve high catalytic activity, mild esterification reaction conditions, and easy operation simple effect

Inactive Publication Date: 2016-05-11
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, heteropolyacids have high solubility in polar solvents (such as water), and there is also the problem of difficult recovery in polar reaction systems. Therefore, at present, heteropolyacids are mostly used as solid acids by loading and ion modification. method

Method used

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  • A kind of heteropolyacid modified catalyst and its preparation and application

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Effect test

Embodiment 1

[0027] Dissolve 18.25g of 12-phosphomolybdic acid in 15ml of distilled water, dissolve 1.23g of 2-picolinic acid in 10ml of distilled water, and configure it into an aqueous solution. Under stirring conditions, add the 2-picolinic acid aqueous solution dropwise to the phosphomolybdic acid solution, add dropwise After stirring for 2 hours, the generated solid was separated and recovered, and dried at 100°C to obtain a 2-picolinic acid modified phosphomolybdic acid catalyst.

[0028] 1.41g of oleic acid, 1.602g of methanol and 0.14g of catalyst were added to a 25ml kettle reactor, reacted at 80°C for 8h, the catalyst was separated by centrifugation, and the reaction product was analyzed by GC-MS.

[0029] Under the above conditions, the conversion rate of oleic acid esterification reaches 100%.

Embodiment 2

[0031] Dissolve 18.25g of 12-phosphomolybdic acid in 15ml of distilled water, and dissolve 4.77g of 3-pyridinesulfonic acid in 15ml of distilled water to form an aqueous solution. Under stirring conditions, add the 3-pyridinesulfonic acid aqueous solution dropwise to the phosphomolybdic acid solution, After the dropwise addition was completed, the mixture was stirred for 6 h, and the generated solid was separated and recovered, and dried at 120° C. to obtain a 2-picolinic acid modified phosphomolybdic acid catalyst.

[0032] 1.41g of oleic acid, 1.92g of methanol and 0.07g of catalyst were added to a 25ml kettle reactor, reacted at 60°C for 10h, the catalyst was separated by centrifugation, and the reaction product was analyzed by GC-MS.

[0033] Under the above conditions, the conversion rate of oleic acid esterification reaches 100%.

Embodiment 3

[0035] Dissolve 28.8g of 12-phosphotungstic acid in 20ml of distilled water, and dissolve 3.18g of 3-pyridinesulfonic acid in 15ml of distilled water to form an aqueous solution. Under stirring, add the aqueous solution of 3-pyridinesulfonic acid dropwise to the phosphotungstic acid solution, After the dropwise addition was completed, the mixture was stirred for 4 hours, and the generated solid was separated and recovered, and dried at 100 °C to obtain a 2-pyridinesulfonic acid modified phosphotungstic acid catalyst.

[0036] 1.41g of oleic acid, 1.602g of methanol and 0.14g of catalyst were added to a 25ml kettle reactor, reacted at 80°C for 6h, the catalyst was separated by centrifugation, and the reaction product was analyzed by GC-MS.

[0037] Under the above conditions, the conversion rate of oleic acid esterification reaches 100%.

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Abstract

The invention relates to a heteropoly acid modified catalyst. A preparation method comprises the following steps: (1) aqueous solution preparation: respectively dissolving heteropoly acid and pyridine carboxylic acid or pyridine sulfonic acid into water to prepare an aqueous solution; (2) reaction: mixing an aqueous solution of heteropoly acid with an aqueous solution of pyridine carboxylic acid or pyridine sulfonic acid by virtue of dropping, and stirring for reacting; and (3) separation and drying: separating to obtain solids produced by reaction, and drying at 100-120 DEG C to obtain a modified heteropoly acid catalyst. The prepared heteropoly acid modified catalyst disclosed by the invention is simple in preparation method, excellent in catalytic performance and easy to separate and recycle, and therefore, the heteropoly acid modified catalyst has very good industrial application prospects.

Description

technical field [0001] The invention relates to a method for catalyzing oleic acid esterification to synthesize oleic acid ester, in particular to a heteropolyacid modified catalyst and its preparation and catalyzing oleic acid esterification reaction system. Background technique [0002] Acid-catalyzed reaction is an important type of reaction in chemical production and organic synthesis. Commonly used inorganic acids, such as sulfuric acid and phosphoric acid, are widely used due to their high catalytic activity. The solid acid catalyst can just make up for the shortcomings of inorganic acid due to its advantages of easy recovery and recyclability. Heteropolyacids have strong B acid and show strong acidity. As a solid acid with great application potential, they have attracted people's attention. There are a lot of reports on the application of heteropolyacids in acid-catalyzed reactions. [0003] However, heteropolyacids have greater solubility in polar solvents (such as ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/18B01J31/16C07C67/08C07C69/587C07C69/24
Inventor 翟庆辉王红红刘丽君卢静
Owner LIAOCHENG UNIV
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