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Solid carbon-based germanium-molybdenum heteropolyacid catalyst and application thereof

A technology of heteropoly acid and solid carbon, applied in the field of catalysis, can solve the problems of poor recovery, high cost, low catalytic efficiency, etc., and achieve the effects of simple preparation method, easy recovery and improved catalytic performance

Inactive Publication Date: 2019-11-12
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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  • Solid carbon-based germanium-molybdenum heteropolyacid catalyst and application thereof
  • Solid carbon-based germanium-molybdenum heteropolyacid catalyst and application thereof
  • Solid carbon-based germanium-molybdenum heteropolyacid catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Catalyst preparation:

[0021] Put 1.000g of activated carbon and 5ml of o-carboxyphenylacetic acid solution in a dilute acid solution with a pH of 3 prepared by sulfuric acid, add 0.2g of Keggin type germanium-molybdenum heteropolyacid, 1ml of N,N-dimethylformamide, and Magnetically stirred for 24 hours, then ultrasonically oscillated for 1 hour, moved into a hydrothermal reaction kettle, and used a temperature-programmed oven to raise the reaction temperature from room temperature to 150 °C within 1 hour, and maintained the temperature for 48 hours, and then naturally cooled to room temperature. Rinse several times with ultrapure water and ethanol, filter, and dry for 12 hours to obtain samples for later use.

[0022] Catalyst evaluation:

[0023] (1) The catalyst embodiment:

[0024] 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...

Embodiment 2

[0038] Catalyst preparation:

[0039] Put 1.000g of activated carbon and 5m of o-carboxyphenylacetic acid solution in a dilute acid solution with a pH of 3 prepared by sulfuric acid, add 0.2g of Keggin type germanium molybdenum heteropolyacid, 1ml of N,N-dimethylformamide, 0.041g Ferrous sulfate, magnetically stirred at room temperature for 24 hours, then ultrasonically oscillated for 1 hour, moved into a hydrothermal reaction kettle, and used a temperature-programmed oven to raise the reaction temperature from room temperature to 150°C within 1 hour, and kept the temperature for 48 hours, and then Naturally cool down to room temperature, wash with ultrapure water and ethanol several times, filter, and dry for 12 hours to obtain samples for later use.

[0040] Catalyst evaluation:

[0041] 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 i...

Embodiment example 3

[0045] Catalyst preparation:

[0046] Put 1.000g of activated carbon and 5ml of o-carboxyphenylacetic acid solution in a dilute acid solution with a pH of 3 prepared by sulfuric acid, add 0.2g of Keggin type germanium molybdenum heteropolyacid, 1ml of N,N-dimethylformamide, 0.0456g Zinc sulfate, magnetically stirred at room temperature for 24 hours, then ultrasonically oscillated for 1 hour, moved into a hydrothermal reaction kettle, and used a temperature-programmed oven to raise the reaction temperature from room temperature to 150°C within 1 hour, and kept the temperature for 48 hours, and then naturally Cool down to room temperature, rinse with ultrapure water and ethanol several times, filter, and dry for 12 hours to obtain samples for later use.

[0047] Catalyst evaluation:

[0048] 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 i...

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Abstract

The invention discloses a solid carbon-based germanium-molybdenum heteropolyacid catalyst and an application thereof. The preparation method of the catalyst comprises the following steps: adding a carbonaceous porous material and a carboxyl functional group coupling agent into a dilute acid solution with the pH value of 3-4, performing magnetic stirring for 12-24 h at room temperature, adding a Keggin type germanium-molybdenum heteropolyacid, an inorganic metal salt and a surfactant, performing ultrasonic oscillation for 0.5-1 h, transferring the product into a hydrothermal reaction kettle, performing heating from room temperature to 150 DEG C within 1 h by using a programmed heating oven, keeping the temperature for 48 h, then performing natural cooling to room temperature, respectively performing washing by using ultrapure water and ethanol for several times, performing filtering and performing drying for 12 h. The catalyst provided by the invention can efficiently catalyze oxidationof iodide ions by hydrogen peroxide to generate iodine elementary substances under a heterogeneous condition, has the advantages of mild reaction conditions, a high hydrogen peroxide utilization rate, environmental friendliness, no pollution, no peroxidation and good thermal stability, can be repeatedly recycled for multiple times, and is easy to recycle.

Description

technical field [0001] The invention belongs to the field of catalysis, and in particular relates to a solid carbon-based germanium-molybdenum heteropolyacid catalyst for iodine recovery and a preparation method thereof. Background technique [0002] Iodine is an important chemical raw material, and its chemical products are widely used in many industries such as food, medicine, dye, metallurgy, synthetic rubber, agriculture, and national defense cutting-edge technology. With the continuous expansion of the application field of iodine resources, the global demand for iodine is also becoming stronger. Iodine is a scarce resource. The world's iodine ore resources mainly include Chilean saltpeter, seaweed, underground brine, and marine sedimentary phosphate rock. Although the storage of iodine is large, it does not solve the shortage of iodine resources. Trace it to its cause no matter be from associated iodine or seaweed, brine and industrial waste water extraction and recov...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/16C01B7/14
CPCB01J23/881B01J27/19C01B7/14Y02P20/584
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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