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Preparation method for molybdenum-doped quaternary ammonium decatungstate high-efficiency photocatalyst

A decamerized tungstic acid and photocatalyst technology, applied in the preparation of organic compounds, carbon-based compounds, chemical instruments and methods, etc., to achieve the effects of high-efficiency doping, novel ideas, and excellent activity

Active Publication Date: 2018-12-14
HUNAN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few reports on the metal doping of quaternary ammonium salts of isopolyacids

Method used

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  • Preparation method for molybdenum-doped quaternary ammonium decatungstate high-efficiency photocatalyst
  • Preparation method for molybdenum-doped quaternary ammonium decatungstate high-efficiency photocatalyst
  • Preparation method for molybdenum-doped quaternary ammonium decatungstate high-efficiency photocatalyst

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Experimental program
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Effect test

Embodiment 1

[0019] Embodiment 1: the method for preparing molybdenum-doped n-tetrabutyl decapolytungstate quaternary ammonium salt of the present invention comprises the following steps:

[0020] (1) Add 6.6g of sodium tungstate dihydrate and sodium molybdate dihydrate in a certain molar ratio (Mo:W=0.01:9.99-0.03:9.97) to 20-50 o Stir and dissolve C in water (20-50mL), the solution concentration calculated by sodium tungstate is 0.4-1.0 mol / L, then slowly add 1-6 mol / L hydrochloric acid dropwise to adjust the pH value to 1.5-2.5;

[0021] (2) Heat the solution obtained in step (1) to 70-80°C for polymerization reaction under stirring, and polymerize for 15-20 minutes, during which time 1-6mol / L hydrochloric acid is used to adjust the pH value to 1.5-2.5. Then add n-tetrabutyl chloride or ammonium bromide salt solution with a concentration of 2-6mol / L (the molar weight is 0.5-1.5 times the molar weight of sodium tungstate), carry out ion exchange reaction at 80-100°C for 15-30min, gradual...

Embodiment 2

[0025] Example 2 (2-1~2-3) The method for preparing molybdenum-doped tetrabutyl decapolyammonium tungstate described in the invention includes the following steps: proceed according to the method of Example 1, the difference is that in The molar ratios of sodium tungstate dihydrate and sodium molybdate dihydrate in step (1) are respectively 0.005:9.995-0.008:9.992, 0.04:9.96-0.06:9.94, 0.07:9.93-0.1:9.9 (corresponding to implementation Example 2-1~2-3), the results are shown in Table 1.

[0026] Table 1

[0027]

[0028] It can be seen from Table 1 that the R value of decapolyammonium tungstate doped with a small amount of molybdenum is equivalent to that of decapolyammonium tungstate without molybdenum, indicating that the doping of a small amount of molybdenum hardly affects the structure of decapolytungstic acid.

[0029] Example 3 (3-1~3-2): The method for preparing molybdenum-doped tetrabutyldecammonium tungstate salt according to the present invention includes the fo...

Embodiment 5

[0037]Example 5 (5-1~5-2): The method for preparing molybdenum-doped tetrabutyldecammonium tungstate salt according to the present invention includes the following steps: proceed according to the method of Example 1, the difference is , the pH values ​​adjusted in step (2) were 1.5-2.0, 2.1-2.5 (respectively corresponding to Examples 5-1~5-2), and the specific results are shown in Table 4.

[0038] Table 4

[0039]

[0040] It can be seen from Table 4 that when the pH value is lower than 2.0, the prepared catalyst R is smaller, and when the pH value is 2.1-2.5, the quality is still inferior to that of the catalyst prepared when the pH value is 2.0-2.1.

[0041] Example 6 (6-1~6-3): According to the preparation method of Example 1, the difference is that in step (2) 1-6mol / L tetramethyl, tetraethyl Base, tetrapropyl chloride or ammonium bromide salt solution to obtain molybdenum-doped tetramethyl, tetraethyl, tetrapropyl ammonium decapolytungstate. The specific results are...

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Abstract

The invention relates to the field of photocatalyst synthesis, and discloses a preparation method for a molybdenum-doped quaternary ammonium decatungstate high-efficiency photocatalyst and a transformation system for efficiently catalyzing molecular oxygen to oxidize an organic matter selectively in visible light based on the molybdenum-doped quaternary ammonium decatungstate high-efficiency photocatalyst serving as a catalyst. A series of molybdenum-doped quaternary ammonium decatungstate high-efficiency photocatalysts are synthesized by heating and polymerizing by taking dehydrate sodium tungstate and dehydrate sodium molybdate as raw materials and taking hydrochloric acid as an acidifying agent, and performing exchange by using quaternary ammonium cations. The synthesized target catalyst can efficiently catalyze molecular oxygen to oxidize cyclohexane, methylbenzene, ethylbenzene and benzyl alcohol to synthesize corresponding oxygen-containing organic matters in acetonitrile, particularly, in an acidic water-containing acetonitrile medium, under the irradiation of visible light.

Description

technical field [0001] The invention relates to the field of photocatalyst synthesis, and discloses a molybdenum-doped decamerium tungstate quaternary ammonium salt high-efficiency photocatalyst preparation method and a high-efficiency visible light-catalyzed molecular oxygen selective oxidation organic matter conversion system based on the catalyst. Background technique [0002] Selective oxidation of organic matter is a very important transformation reaction, because its oxygen-containing products have been widely used in industry as bulk chemical raw materials and key intermediates. For example, cyclohexanone and cyclohexanol (commonly known as KA oil) synthesized by selective oxidation of cyclohexane are important chemical intermediates, and are also used in paint, medicine, coating, pesticide and rubber industries. In industry, the traditional methods of cyclohexane oxidation include cobalt salt method and boric acid method, but they need to be carried out under harsh c...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07C45/33C07C45/36C07C45/38C07C47/54C07C49/403C07C49/78
CPCC07C45/33C07C45/36C07C45/38B01J31/0239C07C2601/14B01J2231/70B01J35/39C07C49/403C07C47/54C07C49/78
Inventor 伏再辉杨波张超苏安群陈梦柯
Owner HUNAN NORMAL UNIVERSITY
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