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A kind of preparation method of molybdenum-doped decapolytungstate quaternary ammonium tungstate 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 high-efficiency doping, excellent activity, and novel ideas

Active Publication Date: 2021-05-04
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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  • A kind of preparation method of molybdenum-doped decapolytungstate quaternary ammonium tungstate high-efficiency photocatalyst
  • A kind of preparation method of molybdenum-doped decapolytungstate quaternary ammonium tungstate high-efficiency photocatalyst
  • A kind of preparation method of molybdenum-doped decapolytungstate quaternary ammonium tungstate high-efficiency photocatalyst

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Experimental program
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Embodiment 1

[0020] Embodiment 1: the method for preparing molybdenum-doped n-tetrabutyl decapolytungstate quaternary ammonium salt of the present invention comprises the following steps:

[0021] (1) Add 6.6g of sodium tungstate dihydrate and sodium molybdate dihydrate with a certain molar ratio (Mo:W=0.01:9.99-0.03:9.97) into water (20-50mL) at 20-50°C and stir to dissolve , the solution concentration calculated by sodium tungstate is 0.4-1.0mol / L, then slowly add 1-6mol / L hydrochloric acid dropwise to adjust the pH value to 1.5-2.5;

[0022] (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, gra...

Embodiment 2

[0026] Embodiment 2 (2-1~2-3) The method for preparing molybdenum-doped tetrabutyl decapolyammonium tungstate described in the invention includes the following steps: carry out according to the method of Example 1, the difference is that in In step (1), the molar ratio of sodium tungstate dihydrate and sodium molybdate dihydrate is 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 implementing Examples 2-1 to 2-3), the results are shown in Table 1.

[0027] Example n(Mo):n(W) Abs1 / λ＝267nm

[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.

Embodiment 3

[0029] Embodiment 3 (3-1~3-2): the method for preparing molybdenum-doped tetrabutyl decapoly ammonium tungstate salt according to the present invention comprises the following steps: carry out according to the method of embodiment 1, the difference is , the polymerization temperatures in step (2) were 60-70° C. and 90-100° C. (respectively corresponding to Examples 3-1 to 3-2), and the specific results are shown in Table 2.

[0030] Example Polymerization temperature / (℃) Abs1 / λ＝267nm

[0031] From Table 2, the optimal polymerization temperature is 70-80°C, and different temperatures have different effects on the quality of the catalyst (the R value becomes smaller).

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Abstract

The invention relates to the field of photocatalyst synthesis, and discloses a preparation method of molybdenum-doped decapolytungstic acid quaternary ammonium salt and a conversion system for organic matter selective oxidation of molecular oxygen with high-efficiency visible light catalysis based on it as a catalyst. Using sodium tungstate dihydrate and sodium molybdate dihydrate as raw materials, hydrochloric acid as an acidifying agent, a series of molybdenum-doped ammonium decammonium tungstate catalysts were synthesized by heating polymerization and then exchanging with quaternary ammonium cations. The synthesized target catalyst can efficiently catalyze the selective oxidation of cyclohexane, toluene, ethylbenzene and benzyl alcohol by molecular oxygen to synthesize corresponding oxygen-containing organic compounds in acetonitrile, especially the acetonitrile medium containing acidic water, and 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 industries such as paint, medicine, coatings, pesticides and rubber. In industry, the traditional methods of cyclohexane oxidation include cobalt salt method and boric acid method, but they need to be carried out und...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02C07C45/33C07C45/36C07C45/38C07C47/54C07C49/403C07C49/78
CPCB01J31/0239B01J35/004B01J2231/70C07C45/33C07C45/36C07C45/38C07C2601/14C07C49/403C07C47/54C07C49/78
Inventor 伏再辉杨波张超苏安群陈梦柯
Owner HUNAN NORMAL UNIVERSITY