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Synthesizing method of heteropolyacid imidazolium salt catalyst

A technology of acid imidazolium salt and synthesis method, applied in the field of chemical synthesis

Active Publication Date: 2013-10-23
杭州师恩科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] During the research, it was also found that the products prepared according to the traditional thinking and method of preparing ionic liquids of heteropolyacid salts contained a large amount of other anionic impurities, which would bring a series of problems to the use of target products in many application fields. question

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Weigh 43g of refined sodium tungstate, wherein the water content of sodium tungstate is calculated as 12%, add 220g of water to dissolve. Under the condition of 20° C., the stirring speed was 300 rpm, and 1.23 g of phosphoric acid was slowly added, and the addition process took 150 minutes. After the addition was complete, the reaction was continued for 6h. After the reaction is completed, the molar mass of the phosphotungstate ion that can be prepared is 0.01mol. The experimental device of bipolar membrane electrodialysis with 5 pairs of membranes was used to remove sodium, the operation time was 7 hours, and the detected sodium ion content was 0.0043%. Move the reaction solution from which sodium ions have been removed to a three-necked flask, place it on an iron stand, and prepare hot oil at the bottom for heating. Weigh 1.35 g (0.012 mol) of 1-ethyl-3-methylimidazole into the reaction system, and mix at 300 rpm for 1 h. Turn on the heater, start heating, and stri...

Embodiment 2

[0038] Weigh 43g of refined sodium tungstate, add 220g of water to dissolve. Under the condition of 20° C., the stirring speed was 300 rpm, and 1.23 g of phosphoric acid was slowly added, and the addition process took 140 minutes. After the addition was complete, the reaction was continued for 6h. The molar mass of phosphotungstate ion that can be prepared is 0.01mol. The experimental device of bipolar membrane electrodialysis with 5 pairs of membranes was used to remove sodium, the operation time was 8 hours, and the detected sodium ion content was 0.0033%. Move the reaction solution from which sodium ions have been removed to a three-necked flask, place it on an iron stand, and prepare hot oil at the bottom for heating. Weigh 1.89 g (0.012 mol) of 1-butyl-3-methylimidazole into the reaction system, and mix at 300 rpm for 1 h. Turn on the heater, start heating, and strictly control the heating rate to ensure that the temperature rise should not be higher than 20°C per hour...

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Abstract

The invention relates to a synthesizing method of a heteropolyacid imidazolium salt catalyst. The method belongs to the technical field of chemical synthesis. According to the invention, sodium tungstate and phosphoric acid are adopted as raw materials. Through the steps such as phosphotungstic acid synthesis, sodium ion removing, phosphotungstic acid imidazolium salt preparation, filtering, and spray drying, heteropolyacid imidazolium salt is obtained. The ionic liquid heteropolyacid imidazolium salt catalyst synthesized with a liquid synthesis route has catalytic activity substantially better than that of a heteropolyacid catalyst prepared with a traditional method. At least, the catalyst has an excellent performance in a reaction for synthesizing PTMEG through tetrahydrofuran polymerization.

Description

technical field [0001] A method for synthesizing a heteropolyacid imidazolium salt catalyst belongs to the technical field of chemical synthesis. Background technique [0002] The present inventor has long been engaged in the research on the synthesis and application of heteropolyacid catalysts. Heteropolyacids are a class of heteropolyacids composed of heteroatoms (such as P, Si, Fe, Co, etc.) and polyatoms (such as Mo, W, V, Nb, Ta, etc.) Oxygen polyacid has high catalytic activity, it is not only acidic, but also has redox properties, and is a multifunctional new catalyst. [0003] Most heteropolyacids will form a "pseudo-liquid phase" phenomenon in organic solvents, that is, a solid state that exists in a solution with the rheological performance of a liquid; in addition, the solubility of heteropolyacids in organic solvents and their The amount of crystallization water contained in itself is related to the water content in the organic solvent, but because its own crys...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18
Inventor 吕涛蔡天锡纪敏
Owner 杭州师恩科技有限公司
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