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Controllable preparation method of phosphorus molybdenum tungsten heteropolyacid catalyst

A heteropolyacid and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, tungsten compounds, etc., can solve problems such as high reaction temperature, high consumption of concentrated sulfuric acid, and controllable and adjustable ratio of molybdenum and tungsten , to achieve the effect of low reaction temperature and low addition amount

Active Publication Date: 2018-06-15
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] To sum up, the problem of preparing the catalyst by the above method is that the reaction temperature is high, the reaction easily generates by-products and consumes a large amount of concentrated sulfuric acid. The most important thing is that the molybdenum-tungsten ratio has not been controlled and adjustable in a wide range

Method used

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  • Controllable preparation method of phosphorus molybdenum tungsten heteropolyacid catalyst
  • Controllable preparation method of phosphorus molybdenum tungsten heteropolyacid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (A) acidification of disodium hydrogen phosphate and sodium molybdate aqueous solution

[0043] 0.7166g of Na 2 HPO 4 12H 2 O dissolved in 4ml of water and 5.32g of Na 2 MoO 4 2H 2 O was dissolved in 8ml of water to form an aqueous solution, stirred at room temperature until completely dissolved, and then added to Na 2 HPO 4 12H 2 98% concentrated H was added dropwise to aqueous O 2 SO 4 , to adjust the pH to 1.5, to Na 2 MoO 4 2H 2 98% concentrated H was added dropwise to aqueous O 2 SO 4 , adjust the pH to 1.5, stir respectively for 0.5 hours to complete the acidification of disodium hydrogen phosphate and sodium molybdate aqueous solution; 0.66g of Na 2 WO 4 2H 2 O was dissolved in 4 mL of water to prepare an aqueous solution for use.

[0044] (B) Preparation of phosphomolybdic acid intermediate

[0045] will acidify Na 2 HPO 4 12H 2 O aqueous solution was moved to a 41°C water bath, and stirred to make the temperature of the solution consistent ...

Embodiment 2

[0048] (A) acidification of disodium hydrogen phosphate and sodium molybdate aqueous solution

[0049] 0.7166g of Na 2 HPO 4 12H 2 O dissolved in 4ml of water and 5.32g of Na 2 MoO 4 2H 2 O was dissolved in 8ml of water to form an aqueous solution, stirred at room temperature until completely dissolved, and then added to Na 2 HPO 4 12H 2 98% concentrated H was added dropwise to aqueous O 2 SO 4 , to adjust the pH to 1.5, to Na 2 MoO 4 2H 2 98% concentrated H was added dropwise to aqueous O 2 SO 4 , adjust the pH to 1.5, stir respectively for 0.5 hours to complete the acidification of disodium hydrogen phosphate and sodium molybdate aqueous solution; 0.66g of Na 2 WO 4 2H 2 O was dissolved in 4 mL of water to prepare an aqueous solution for use.

[0050] (B) Preparation of phosphomolybdic acid intermediate

[0051] will acidify Na 2 HPO 4 12H 2 O aqueous solution was moved to a 43°C water bath, and stirred to make the temperature of the solution consistent ...

Embodiment 3

[0054] (A) acidification of disodium hydrogen phosphate and sodium molybdate aqueous solution

[0055] 0.7166g of Na 2 HPO 4 12H 2 O dissolved in 4ml of water and 2.9034g of Na 2 MoO 4 2H 2 O was dissolved in 8ml of water to form an aqueous solution, stirred at room temperature until completely dissolved, and then added to Na 2 HPO 4 12H 2 98% concentrated H was added dropwise to aqueous O 2 SO 4 , to adjust the pH to 1.5, to Na 2 MoO 4 2H 2 98% concentrated H was added dropwise to aqueous O 2 SO 4 , adjust the pH to 1.5, stir respectively for 0.5 hour to complete the acidification of disodium hydrogen phosphate and sodium molybdate aqueous solution, and 3.9582g Na 2 WO 4 2H 2 O was dissolved in 8 mL of water to prepare an aqueous solution for use.

[0056] (B) Preparation of phosphomolybdic acid intermediate

[0057] will acidify Na 2 HPO 4 12H 2 O aqueous solution was moved to a 43°C water bath, and stirred to make the temperature of the solution consist...

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Abstract

The invention relates to a method for preparing a phosphorus molybdenum tungsten heteropolyacid catalyst of a Keggin structure. According to the method, a large amount of concentrated sulfuric acid issaved, an operation process is simplified, reaction temperature is low, and particularly controllability and adjustability of a tungsten-molybdenum ratio within a large range are realized. The methodcomprises the following steps: acidifying a disodium hydrogen phosphate aqueous solution and a sodium molybdate aqueous solution step by step, then dropwise adding the acidified sodium molybdate solution into the acidified disodium hydrogen phosphate aqueous solution at 20 to 60 DEG C to prepare a phosphomolybdic acid intermediate, and dropwise adding a sodium tungstate solution into the phosphomolybdic acid intermediate aqueous solution at 20 to 40 DEG C, and adding diethyl ether for extraction, liquid separation and weathering after the reaction ends, thereby obtaining the final phosphorusmolybdenum tungsten heteropolyacid catalyst.

Description

technical field [0001] The invention relates to a method for preparing a phosphomolybdenum-tungsten heteropolyacid catalyst with a Keggin structure, more precisely, it relates to a step-by-step acidification temperature control to prepare phosphomolybdenumtungsten heteropolyacids with a Keggin structure with different molybdenum-tungsten ratios The catalyst method is characterized in that step-by-step acidification is used and temperature is controlled to prepare phosphorus-molybdenum-tungsten heteropolyacid catalysts with Keggin structures with different molybdenum-tungsten ratios, and the reaction time is short, the reaction temperature is low, and the amount of sulfuric acid is small. Background technique [0002] Heteropolyacids have various forms, among which Keggin structure heteropolyacids have relatively good thermal stability, and are widely used in Homogeneous, biphasic and heterogeneous catalytic processes, especially combined with green chemistry, have developed ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18B01J27/19C01G41/00
CPCB01J27/19C01G41/006C01P2002/72C01P2002/82
Inventor 刘华彦范铭晨汪月刘树马校彬朱秋莲卢晗锋张泽凯
Owner ZHEJIANG UNIV OF TECH