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Supported polyoxometallate and preparation method thereof

A polyoxometalate, load-type technology, applied in chemical instruments and methods, oxidized water/sewage treatment, inorganic chemistry, etc., can solve the problems of few research reports, polyacid detachment, easy separation, etc.

Active Publication Date: 2014-06-11
宁波神筹环保设备有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] So far, the research on the degradation of pollutants by polyacid compounds has mostly focused on the research on the catalytic activity of photodegradation, and there are few research reports on the catalytic oxidation of pollutants in water by using molecular oxygen and hydrogen peroxide.
For example, the Chinese patent literature with the application number 201010137976.5 reports a method for the degradation of phenol by a micellar polyacid complex, but it is prone to separation after use
In prior art reports on silica-loaded polyoxometalates, the method is to modify silica on the surface or inner pores of amino groups, and then remove polyacids. However, polyacids are mostly distributed on the surface of silicon spheres, and, The polyacid is easy to detach from the silicon ball after it is used for many times

Method used

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Examples

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preparation example Construction

[0027] The embodiment of the present invention discloses a preparation method of supported polyoxometalate, comprising the following steps: Step a) making polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (referred to as P123) was dissolved in HCl aqueous solution, then added silicon source compound and mixed uniformly to obtain the first mixed solution; step b) adding H to the first mixed solution 5 PV 2 Mo 10 o 40 (referred to as polyacid), collect the solid after the reaction; step c) reflux the solid in ethanol, filter, and dry to obtain the loaded polyoxometalate.

[0028] The present invention utilizes H 5 PV 2 Mo 10 o 40 Its good acid catalytic effect can hydrolyze the silicon source into silicon spheres, and at the same time control the corresponding reaction conditions, so that the H 5 PV 2 Mo 10 o 40 Wrapped inside. The invention solves the problem of low efficiency of loading polyacid in the past, and the problem that polyacid i...

Embodiment 1

[0041] Weigh Na according to molar ratio 1:1.3 2 HPO 4 and (NH4)VO 4 , were respectively dissolved in boiling distilled water with a mass ratio of 1:20, and after being dissolved respectively, the above two solutions were mixed. The mixture was cooled to room temperature, acidified with concentrated sulfuric acid until the color of the solution turned red, and Na 2 MoO 4 2H 2 O and Na 2 HPO 4 W. Concentrated sulfuric acid was slowly added to the solution with vigorous stirring until the solution turned from dark red to pre-red. Rinse the precipitate with distilled water for 2 to 3 times to obtain a precipitate; place the precipitate in a mug furnace and sinter at 150-300°C for 2 to 6 hours to obtain H 5 PV 2 Mo 10 o 40 .

Embodiment 2

[0042] Embodiment 2 preparation embodiment

[0043] Dissolve 8g of P123 ultrasonically in 300mL of 2.0M HCl aqueous solution, pour it into a three-necked flask equipped with two constant-pressure dropping funnels, slowly drop 17g of TEOS from a constant-pressure dropping funnel, and place it at 40°C after dropping After hydrolysis with mechanical stirring in an oil bath for 1 hour, slowly add 5 g of KH550 into another constant pressure dropping funnel solution.

[0044] The resulting mixture solution was stirred in an oil bath at 40° C. for 30 minutes, and then 2.5 g of the H obtained from Example 1 was added. 5 PV 2 Mo 10 o 40 , the stirring was continued for 20 hours and then the stirring was stopped, the reaction solution was aged at 90° C. for 24 hours, and the obtained solid was filtered and vacuum-dried at 100° C. for 12 hours. The collected solid was heated to reflux in 95% ethanol for 20 hours, and washed to remove P123 as a template. Finally, filter, wash with wa...

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Abstract

The invention provides supported polyoxometallate and a preparation method thereof. The preparation method comprises the following steps: dissolving polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer in an HCl water solution, adding a silicon source compound, and uniformly mixing to obtain a first mixed solution; adding H5PV2Mo10O40, and after reaction, collecting solids; and carrying out a backflow reaction on the solids in ethyl alcohol, filtering, and drying to obtain the supported polyoxometallate. The supported polyoxometallate and the preparation method thereof provided by the invention have the advantages that the good acid catalysis effect of the H5PV2Mo10O40 is utilized to hydrolyze a silicon source to form a silicon ball, and meanwhile, the corresponding reaction condition is controlled, so that the H5PV2Mo10O40 is uniformly coated with a silicon dioxide silicon ball skeleton in a forming process; the problems that the former polyacid supporting efficiency is low, and polyacid is likely to separate from the silicon ball after being repeatedly used are solved, and the supported polyoxometallate is stable and effective. The invention also provides application of the supported polyoxometallate to degradation of phenol in sewage.

Description

technical field [0001] The invention relates to the technical field of sewage treatment, in particular to a preparation method and application of a loaded polyoxometalate. Background technique [0002] Phenol is a raw material or intermediate produced in industries such as papermaking, coking, oil refining, plastics, pesticides, and pharmaceutical synthesis. With the development of the economy, the untreated phenolic wastewater has caused a serious threat to the living environment of human beings. Phenolic compounds are a kind of protoplasmic poisons. All biologically active substances can produce toxicity. They can directly enter the blood circulation through contact with the skin and mucous membranes without detoxification by the liver, causing cell damage and loss of vitality; they can also invade the human body through the mouth. cause cell damage. Low-concentration phenol solution can denature protein, and high-concentration phenol solution can coagulate protein, caus...

Claims

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Application Information

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IPC IPC(8): B01J27/199C01G39/00C02F1/72C02F101/34
Inventor 魏亮翁挺吴晓伟
Owner 宁波神筹环保设备有限公司
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