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Solid silicon-based Waugh-type molybdenum-containing heteropolyacid catalyst and application thereof

A technology of heteropolyacid and solid silicon, applied in the field of catalysis, can solve the problems of high cost, low catalytic efficiency, poor recovery, etc., and achieve the effects of easy recovery, improved oxidation rate, and shortened process time.

Inactive Publication Date: 2019-11-29
WENGFU (GRP) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalytic efficiency of the currently used catalysts is relatively low, the recovery is poor, and the cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Catalyst preparation:

[0022] Put 1.000g of diatomaceous earth and 5ml of N,N-diethyl-3-(trimethoxysilyl)propylamine solution in a dilute acid solution with a pH of 3 prepared by sulfuric acid, and add 0.2g of Waugh-type manganese-molybdic acid Ammonium heteropoly acid, 1ml dodecyltrimethylammonium chloride, magnetically stirred at room temperature for 24h, then ultrasonically oscillated for 1h, moved into a hydrothermal reaction kettle, and the reaction temperature was changed from room to room within 1 hour by using a temperature-programmed oven. The temperature was raised to 150°C, maintained at this temperature for 48 hours, and then cooled down to room temperature naturally, rinsed with ultrapure water and ethanol several times, filtered, and dried for 12 hours to obtain a sample for use.

[0023] Catalyst evaluation

[0024] (1) The catalyst embodiment:

[0025] Dissolve 1.6667g of potassium iodide in an appropriate amount of deionized water, transfer it to a 1...

Embodiment 2

[0041] Catalyst preparation:

[0042] Put 1.000g of diatomaceous earth and 5ml of N,N-diethyl-3-(trimethoxysilyl)propylamine solution in a dilute acid solution with a pH of 3 prepared by sulfuric acid, and add 0.2g of isopolymolybdic acid Ammonium, 1ml dodecyltrimethylammonium chloride, magnetically stirred at room temperature for 24h, then ultrasonically oscillated for 1h, moved into a hydrothermal reaction kettle, and used a temperature-programmed oven to raise the reaction temperature from room temperature to 150°C, keep the temperature for 48 hours, then cool down to room temperature naturally, rinse with ultrapure water and ethanol several times, filter, and dry for 12 hours to obtain samples for later use.

[0043] Catalyst evaluation:

[0044] Dissolve 1.6667g of potassium iodide in an appropriate amount of deionized water, transfer it to a 100mL volumetric flask, and adjust the volume to 0.01mol / L iodine solution, take 10mL of iodine solution, add stoichiometric molar...

Embodiment 3

[0046] Catalyst preparation:

[0047] Put 1.000g of diatomaceous earth and 5ml of N,N-diethyl-3-(trimethoxysilyl)propylamine solution in a dilute acid solution with a pH of 3 prepared by sulfuric acid, and add 0.2g of Waugh-type nickel-molybdenum acid Ammonium heteropoly acid, 1ml dodecyltrimethylammonium chloride, magnetically stirred at room temperature for 24h, then ultrasonically oscillated for 1h, moved into a hydrothermal reaction kettle, and the reaction temperature was changed from room to room within 1 hour by using a temperature-programmed oven. The temperature was raised to 150°C, maintained at this temperature for 48 hours, and then cooled down to room temperature naturally, rinsed with ultrapure water and ethanol several times, filtered, and dried for 12 hours to obtain a sample for use.

[0048] Catalyst evaluation:

[0049] Dissolve 1.6667g of potassium iodide in an appropriate amount of deionized water, transfer it to a 100mL volumetric flask, and adjust the v...

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PUM

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Abstract

The invention discloses a solid silicon-based Waugh-type molybdenum-containing heteropolyacid catalyst and application thereof. A preparation method for the solid silicon-based Waugh-type molybdenum-containing heteropolyacid catalyst comprises the following steps: adding a siliceous porous material and an amido functional group coupling agent into a dilute acid solution with a pH value of 3-4, carrying out magnetic stirring at room temperature for 12-24 h, then adding Waugh-type molybdenum-containing heteropoly acid and a surfactant, performing ultrasonic oscillation for 0.5-1 h, transferringthe formed substance into a hydrothermal reactor, raising a reaction temperature from room temperature to 150-180 DEG C within 0.5-1 h by using a temperature-programmed oven, keeping the temperature for 48-72 h, then carrying out natural cooling to room temperature, performing rinsing with ultrapure water and ethanol several times separately, and carrying out filtering and drying for 10-12 h. Thecatalyst of the invention can efficiently catalyze hydrogen peroxide to oxidize iodine ions under heterogeneous conditions so as to produce elemental iodine; and the catalyst has the advantages of mild reaction conditions, high utilization rate of hydrogen peroxide, friendliness to environment, no pollution, no peroxidation and good thermal stability, can be repeatedly reused a plurality of times,and is easy to recycle.

Description

technical field [0001] The invention belongs to the field of catalysis, and in particular relates to a preparation and application method of a solid silicon-based Waugh-type molybdenum-containing heteropolyacid catalyst for recovering iodine. Background technique [0002] Iodine is a halogen element, easy to sublimate, and easy to desublimate after sublimation. With the development of science and technology, the use of iodine has expanded from traditional iodine, dyes, test paper and other fields to iodine compounds with multiple functions. At the same time, iodine is also one of the essential trace elements for the human body. A certain amount of iodine is often added to table salt to make iodized salt to prevent the occurrence of certain diseases. With the continuous expansion of new uses of iodine, its usage and market value are also undergoing great changes. However, iodine is rare in nature, and there are almost no independent iodine minerals. Most of it exists in var...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/34B01J27/188C01B7/04
CPCB01J31/34B01J27/188C01B7/04
Inventor 郭军蔡丽丽解田史连军张丹李文飞
Owner WENGFU (GRP) CO LTD
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