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A kind of supported polyoxometalate catalyst and its preparation and application

A polyoxometalate, supported technology, applied in the direction of physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, non-metallic elements, etc., can solve high investment and operating costs, corrosion storage and transportation Safety, treatment cost increase and other issues, to achieve the effect of low operating cost, lower nitrogen oxide content, and simple preparation method

Active Publication Date: 2015-12-09
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wet denitrification has not been widely used due to problems such as high operating costs, huge equipment, and secondary pollution.
The catalytic conversion method in the dry method has always been the focus of people's research. The catalytic conversion method mainly includes the catalytic reduction method and the catalytic decomposition method. Among them, the ammonia selective catalytic reduction method has been successfully applied in the pollution control of fixed nitrogen oxide pollution sources. This method can convert nitric oxide into nitrogen in a gas with high oxygen content, but this method has high investment and operating costs, large ammonia consumption, hidden dangers of secondary pollution caused by ammonia leakage, pipeline corrosion and storage transport safety issues
In addition, in the process of this method, the useful ammonia gas is changed into useless nitrogen gas, and this side reaction directly leads to the increase of the treatment cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Synthesis of supported polyoxometalate adsorption catalyst

[0025] 0.965gMoO 3 Dissolve in 5ml distilled water. Add a solution prepared by dissolving 1.0g KOH in 500ml distilled water into the above solution, stir at room temperature and add HClO dropwise 4 Keep the mixture acidic at pH=4.5. Take 0.55gGd(NO 3 ) 3 ·6H 2 O was dissolved in 10ml of distilled water, and slowly added to the aforementioned mixture at room temperature under stirring. At the same time, add HClO dropwise to the mixture 4 Keep pH=3.5. At room temperature, keep stirring for 48h, filter, wash with water, and air-dry at room temperature for 48h to obtain a yellow powder that is [H 20 Gd 2 Mo 8 o 37 ]·8H 2 O. Take 0.04gSiO 2 Carrier is placed in a small beaker, add 0.01g [H 20 Gd 2 Mo 8 o 37 ]·8H 2 The prepared concentration of O was 0.01g / L aqueous solution, and after stirring at room temperature for 48h, evaporated to dryness in a water bath at 65°C, the prepared load...

Embodiment 2

[0026] Example 2: Simulating Nitric Oxide-Containing Gas

[0027] Take 0.01g load (mass percentage) 5% [H20 Gd 2 Mo 8 o 37 ]·8H 2 O / SiO 2 It is fixed on the reactor, and the reaction temperature is controlled by a temperature program controller to 100°C. The gas used is 99.99% (volume fraction) of nitric oxide, and high-purity nitrogen is used as the carrier gas, and the gas mass flow meter is used to accurately control the gas. Flow rate 0.25L / min, using TH-990S flue gas analyzer to detect NO / NO 2 concentration. After reacting for 35 minutes, the supported polyoxometalates adsorbed NO to saturation, then the carrier gas was switched to high-purity helium, and the nitrogen oxides were decomposed and desorbed by programming the temperature from 150°C to 450°C. GC-MS was used to detect the nitrogen components in the decomposition products. Nitrogen gas began to be generated at about 1 min after the temperature was raised, and the nitrogen content reached a peak at 4.5 min,...

Embodiment 3

[0028] Example 3: Simulating Nitric Oxide-Containing Gas

[0029] Take 0.025g load (mass percentage) 15% [H 20 Eu 2 Mo 8 o 37 ]·8H 2 O / SiO 2 It is fixed on the reactor, and the reaction temperature is controlled by a temperature program controller to 200°C. The gas used is 99.99% (volume fraction) of nitric oxide, and high-purity nitrogen is used as the carrier gas, and the gas mass flow meter is used to precisely control the gas. Flow rate 0.4L / min, using TH-990S flue gas analyzer to detect NO / NO 2 concentration. After reacting for 50 minutes, the supported polyoxometalates adsorbed NO to saturation, then the carrier gas was switched to high-purity helium, and the nitrogen oxides were decomposed and desorbed by programming the temperature from 150°C to 450°C. GC-MS was used to detect the nitrogen components in the decomposition products. Nitrogen gas began to be generated at about 1 min after the temperature was raised, and the nitrogen content reached a peak at 5 min,...

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PUM

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Abstract

The invention relates to a supported polyoxometallate catalyst, and preparation and application thereof. The preparation of the supported polyoxometallate catalyst comprises the steps of dissolving 0.1-2.5 g of MoO3 in 5-25 ml of distilled water; dissolving 1.0-3.0 g of KOH in 500-1000 ml of distilled water to prepare a solution; adding the KOH solution into the MoO3 solution, and dropwise adding HClO4 to enable the pH to be 3.5-5.5; dissolving 1.0-2.5 g of Eu(NO3)3 or Gd(NO3)3 in 10-50 ml of distilled water and adding into the mixed solution; dropwise adding HClO4 to keep the pH at 3.0-5.0; filtering, washing and drying for 12-48 hours to obtain yellow powder; dissolving 0.001-0.05 g of yellow powder in 50-1000 ml of distilled water and adding 0.01-5 g of SiO2, and evaporating in water bath at 45-85 DEG C, thereby obtaining the catalyst. The catalyst is simple to prepare, high in denitration efficiency, easy to recycle and reuse and free of pollution to pipelines and environments.

Description

Technical field: [0001] The invention relates to a polyoxometalate catalyst with silicon dioxide as a carrier and its preparation and application. Background technique: [0002] Nitrogen oxides in the atmosphere mainly include nitric oxide and nitrogen dioxide, which mainly come from the combustion of fossil fuels and incineration of plants, as well as the transformation of nitrogen-containing compounds in farmland soil and animal excrement. [0003] At present, the removal methods of nitrogen oxides studied by people (referred to as denitrification) can be divided into wet and dry methods. Wet denitrification has not been widely used due to problems such as high operating costs, huge equipment, and secondary pollution. The catalytic conversion method in the dry method has always been the focus of people's research. The catalytic conversion method mainly includes the catalytic reduction method and the catalytic decomposition method. Among them, the ammonia selective catalyt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/10B01J31/16B01D53/86B01D53/04B01D53/56
Inventor 路洋蒲文晶路昆侯丹莉常维民刘洋慕善文周连春
Owner PETROCHINA CO LTD