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Solid silica-based Anderson type molybdenum-containing heteropoly acid catalyst and application thereof

A heteropolyacid and solid silicon technology, applied in the field of catalysis, can solve the problems of no significant increase in oxidation rate, low catalytic efficiency, and high cost, and achieve the effects of reducing iodine recovery costs, increasing oxidation rate, and easy recovery

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

However, the catalytic efficiency of the currently used catalysts is relatively low, the recovery is poor, and the cost is high
For example, Chen Xiaohu et al. used sulfuric acid as a catalyst to catalyze the recovery of iodine oxidation, but the oxidation rate did not increase significantly.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Catalyst preparation:

[0023] Put 1.000g of diatomaceous earth and 5ml of N-[3-(trimethoxysilyl)propyl]ethylenediamine solution in a dilute acid solution with a pH of 3 prepared by sulfuric acid, and add 0.2g of Anderson-type zinc molybdenum Heteropoly acid, 1ml octadecyl dimethyl hydroxyethyl ammonium nitrate, 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 reduced within 1 hour by using a temperature-programmed oven. Raise 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.

[0024] Catalyst evaluation:

[0025] (1) The catalyst embodiment:

[0026] Dissolve 1.6667g of potassium iodide in an appropriate amount of deionized water, transfer it to a 100mL volumetric flas...

Embodiment 2

[0041] Catalyst preparation:

[0042] Put 1.000g of diatomaceous earth and 5ml of N-[3-(trimethoxysilyl)propyl]ethylenediamine solution in a dilute acid solution with a pH of 3 prepared by sulfuric acid, and add 0.2g of Anderson-type iron molybdenum Polyacid, 1ml octadecyl dimethyl hydroxyethyl ammonium nitrate, 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 changed within 1 hour by using a temperature-programmed oven. The room 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.

[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 t...

Embodiment example 3

[0046] Catalyst preparation:

[0047] Place 1.000g of bentonite and 5ml of N-[3-(trimethoxysilyl)propyl]ethylenediamine solution in a dilute acid solution with a pH of 3 prepared by sulfuric acid, and add 0.2g of Anderson type zinc molybdenum heteropolyacid , 1ml of octadecyl dimethyl hydroxyethyl ammonium nitrate, 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 increase the reaction temperature from room temperature within 1 hour Raise 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.

[0048] Catalyst evaluation:

[0049] Cycle times ( / time) Catalytic reaction rate (mol L -1 ·s -1 )

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PUM

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Abstract

The invention discloses a solid silica-based Anderson type molybdenum-containing heteropoly acid catalyst and application thereof. The catalyst comprises the following steps of adding a silica porousmaterial and an amino functional group coupling agent into a dilute acid solution with pH of 3-4, stirring with magnetic at the room temperature for 12-24 h, adding Anderson type molybdenum-containingheteropoly acid and a surfactant, vibrating with ultrasonic for 0.5-1h, transferring the solution into a hydrothermal reactor, using an oven with programmed heating, raising the reaction temperaturefrom the room temperature to 150-180 DEG C within 0.1-1 h, maintaining the temperature for 48-72 h, then cooling the reaction temperature naturally to the room temperature, washing several times withultrapure water and ethanol respectively, and filtering and drying for 10-12 h. The catalyst can effectively catalyze hydrogen peroxide to oxidize iodide ion under heterogeneous conditions to produceiodine elemental, a reaction condition is mild, the utilization rate of hydrogen peroxide is high, environmentally friendly and pollution-free are achieved, peroxidation does not exist, thermal stability is good, and the catalyst can be reused for many 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 method and application of a solid silicon-based Anderson type molybdenum-containing heteropolyacid catalyst. Background technique [0002] Iodine is an important chemical raw material, which is widely used in cutting-edge technologies such as medicine, agriculture, dyes, metallurgy, synthetic rubber, and national defense technology. With the continuous expansion of the application field of iodine resources, the global demand for iodine is also becoming stronger. At present, the main sources of iodine in the world are saltpeter, seaweed, underground brine and marine sedimentary phosphate rock. The common feature of these iodine sources is that the iodine equivalent is very low, resulting in a slow rate of oxidation of iodine ions into iodine element, low extraction rate and high production cost. Although iodine can be recovered by ion exchange, precipitation, e...

Claims

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Application Information

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IPC IPC(8): B01J23/28B01J23/881B01J27/188C01B7/14C01B7/16C02F9/04C02F101/12
CPCB01J23/28B01J23/881B01J23/002B01J27/188C01B7/14C01B7/16C02F1/722C02F1/725C02F1/66C02F2101/12
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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