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Silica-based germanomolybdate heteropolyacid catalyst for iodine recycling and preparation method thereof

A technology of iodine recovery and catalyst, which is applied in the field of catalysis, can solve the problems of high cost, low catalytic efficiency, and poor recovery, and achieve the effects of easy recovery, improved catalytic performance, and reduced cost

Inactive Publication Date: 2019-08-09
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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  • Silica-based germanomolybdate heteropolyacid catalyst for iodine recycling and preparation method thereof
  • Silica-based germanomolybdate heteropolyacid catalyst for iodine recycling and preparation method thereof
  • Silica-based germanomolybdate heteropolyacid catalyst for iodine recycling and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Catalyst preparation:

[0020] Put 1.000g of diatomaceous earth and 5ml of ureapropyltriethoxysilane 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 octadecyl di Methyl hydroxyethylenediyl ammonium nitrate was magnetically stirred at room temperature for 24 hours, then ultrasonically oscillated for 1 hour, moved into a hydrothermal reaction kettle, and the reaction temperature was raised from room temperature to 150°C within 1 hour using a temperature-programmed oven, and the temperature was kept The temperature was 48 hours, and then the temperature was naturally lowered to room temperature, washed several times with ultrapure water and ethanol respectively, filtered, and dried for 12 hours to obtain samples for later use.

[0021] Catalyst evaluation:

[0022] (1) The catalyst embodiment:

[0023] Dissolve 1.6667g of potassium iodide in an appropriate amount of deionized...

Embodiment 2

[0037] Catalyst preparation:

[0038] Put 1.000g of diatomaceous earth and 5ml of ureapropyltriethoxysilane 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 octadecyl di Ammonium methyl hydroxyethylenediyl ammonium nitrate, 0.04g ferrous sulfate, magnetically stirred at room temperature for 24 hours, then ultrasonically oscillated for 1 hour, moved into a hydrothermal reaction kettle, and the reaction temperature was raised from room temperature within 1 hour by using a temperature-programmed oven. 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.

[0039] Catalyst evaluation:

[0040] Dissolve 1.6667g of potassium iodide in an appropriate amount of deionized water, transfer it to a 100mL volumetric flask, and adjust the volume...

Embodiment example 3

[0044] Catalyst preparation:

[0045] Put 1.000g of diatomaceous earth and 5ml of ureapropyltriethoxysilane 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 octadecyl di Methyl hydroxyethylenediyl ammonium nitrate, 0.0456g zinc sulfate, magnetically stirred at room temperature for 24 hours, then ultrasonically oscillated for 1 hour, transferred to a hydrothermal reaction kettle, and the reaction temperature was raised 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.

[0046] Catalyst evaluation:

[0047] 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,...

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Abstract

The invention discloses a silica-based germanomolybdate heteropolyacid catalyst for iodine recycling and a preparation method thereof. The method comprises the preparation steps that a silicious porous material and a functional group coupling agent are added into a dilute acid solution with pH being 3-4, magnetic stirring is performed under the room temperature for 12-24 h, Keggin type germanomolybdate heteropolyacid, inorganic metal salt, a surface active agent and a dispersing agent are added, ultrasonic oscillation is performed for 0.5-1 h, the mixture is moved into a hydrothermal reactionkettle, a drying oven heated through a program is adopted, the reaction temperature is increased to 150 DEG C from the room temperature within 1 h, the temperature is kept for 48 h, then, natural cooling is performed to room temperature, hyper pure water and ethyl alcohol are adopted for washing repeatedly, filtering is performed, and drying is performed for 12 h. The catalyst can efficiently catalyze and peroxide iodine hydroxide ions to generate iodine substances, reaction conditions are mild, the hydrogen peroxide utilization rate is high, and the catalyst is environmentally friendly, freeof contamination, free of peroxidation, good in thermal stability, capable of being used repeatedly, and easy to recycle.

Description

technical field [0001] The invention belongs to the field of catalysis, and in particular relates to a silicon-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 recovery, ...

Claims

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Application Information

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IPC IPC(8): B01J31/18B01J23/881C01B7/14
CPCB01J23/881B01J31/1805C01B7/14Y02P20/584
Inventor 郭军蔡丽丽解田史连军张丹黄利锦
Owner WENGFU (GRP) CO LTD
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