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Solid carbon base keggin type phosphomolybdic heteropoly acid catalyst and application thereof

A technology of phosphomolybdenum heteropoly acid and solid carbon, which is applied in the field of catalysis, can solve the problems of increasing equipment energy consumption and cost, restricting industrialization process, and high structural stability, and achieves easy recycling, improved kinetic performance, and good stability Effect

Inactive Publication Date: 2019-12-03
WENGFU (GRP) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Keggin-type heteropolyacids have higher homogeneous catalytic efficiency, but the catalyst needs to be separated and recovered after the reaction, which will increase equipment energy consumption and cost, thus limiting its wider industrialization process
The industrial application of Keggin-type heteropolyacids can be expanded by using carriers to form heterogeneous reaction catalysts. However, Keggin-type heteropolyacids are easily soluble in water, and the force between them and the carrier is small due to their high structural stability. Easy to lose during the reaction

Method used

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  • Solid carbon base keggin type phosphomolybdic heteropoly acid catalyst and application thereof
  • Solid carbon base keggin type phosphomolybdic heteropoly acid catalyst and application thereof
  • Solid carbon base keggin type phosphomolybdic heteropoly acid catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Catalyst preparation:

[0022] Put 1.000g of activated carbon and 5mL of 4,4-sulfonyl benzilacetic acid solution in a dilute acid solution with a pH of 3 prepared by sulfuric acid, add 0.2g of keggin type phosphomolybdenum heteropolyacid, 1ml of 2-alkyl imidazoline, room temperature Stir under magnetic force for 24 hours, then vibrate ultrasonically for 1 hour, transfer to a hydrothermal reaction kettle, use a temperature-programmed oven to raise the reaction temperature from room temperature to 150°C within 1 hour, keep the temperature for 48 hours, and then cool down to room temperature naturally. Rinse several times with ultrapure water and ethanol respectively, filter, and dry for 12 hours to obtain samples for later 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 100mL volumetric flask, and adjust the volume to 0.01mol / L iodine solu...

Embodiment 2

[0039] Catalyst preparation:

[0040] Put 1.000g of activated carbon and 5ml of 4,4-sulfonyl tolueneacetic acid solution in a dilute acid solution with a pH of 3 prepared by sulfuric acid, add 0.2g of Keggin type phosphomolybdenum heteropoly acid, 1ml of 2-alkyl imidazoline, 0.04 g ferrous sulfate, stirred magnetically 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. 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.

[0041] Catalyst evaluation:

[0042] 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 io...

Embodiment example 3

[0046] Catalyst preparation:

[0047] Put 1.000g of activated carbon and 5ml of 4,4-sulfonyl tolueneacetic acid solution in a dilute acid solution with a pH of 3 prepared by sulfuric acid, add 0.2g of Keggin type phosphomolybdenum heteropolyacid, 1ml of 2-alkylimidazoline, 0.0456g of zinc sulfate, stirred magnetically 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. 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.

[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 volume to 0.01mol / L iodine solution, take 10mL of iod...

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Abstract

The invention discloses a solid carbon base keggin type phosphomolybdic heteropoly acid catalyst and application thereof. The preparation steps are as follows: a carbon porous material and a carboxylfunctional group coupling agent are added into a dilute acid solution with the pH being 3-4, magnetic stirring is conducted at the room temperature for 12-24 h, Keggin type phosphomolybdic heteropolyacid, an inorganic metal salt and a surfactant are added, ultrasonic vibration is conducted for 0.5-1 h, a mixture is transferred into a hydrothermal reactor, a temperature programming dryer is used,the reaction temperature is raised from the room temperature to 150-180 DEG C in 0.5-1 h, the temperature is maintained for 48-72 h, and then decreased to the room temperature naturally, washing withultrapure water and ethanol for multiple times is conducted, filtration is conducted, and drying is conducted for 10-12 h. The solid carbon base keggin type phosphomolybdic heteropoly acid catalyst can efficiently catalyze hydrogen peroxide to oxidize iodine ions to form an iodine simple substance under heterogeneous conditions, reaction conditions are mild, the hydrogen peroxide utilization rateis high, environmental friendliness, no pollution and no peroxidation are achieved, thermal stability is good, and the catalyst can be reused 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 preparation and application method of a solid carbon-based keggin type phosphomolybdenum heteropolyacid catalyst for iodine recovery. Background technique [0002] Iodine resources are one of the scarce resources in the world, and have a wide range of uses in medicine, agriculture, dyes, metallurgy, synthetic rubber, national defense and cutting-edge technology. China is a country seriously deficient in iodine. According to statistics, the annual demand for iodine in my country is as high as 4014 tons, while the total production capacity of iodine in the whole country is only about 670 tons, which is far from meeting the demand of the market, and most of it is imported from abroad. Since there are no special iodine resources, my country's iodine is mainly obtained from seaweed, phosphate rock, various natural brines and other resources, but the concentration of iodine in it...

Claims

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Application Information

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IPC IPC(8): B01J31/18C01B7/14C02F9/04C02F101/12
CPCB01J27/19C01B7/14C02F1/722C02F1/725C02F1/66C02F2101/12
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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