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Nanosheet containing noble metal and preparation method thereof

A nanosheet and precious metal technology, applied in the field of catalysis, can solve the problems of slow reaction rate, many by-products, complicated steps, etc., and achieve the effects of easy operation, low cost and high selectivity

Active Publication Date: 2018-07-17
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods for preparing cyclohexanone have high energy consumption, high cost, many by-products, complicated steps, slow reaction rate, large pollution, and low efficiency.

Method used

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  • Nanosheet containing noble metal and preparation method thereof
  • Nanosheet containing noble metal and preparation method thereof
  • Nanosheet containing noble metal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] H 1.07 Ti 1.73 O 4 •H 2 Preparation of nanosheets

[0025] Set the molar ratio of 2.4:0.8:10.4 to K 2 CO 3 , Li 2 CO 3 And TiO 2 After grinding uniformly, place it in a corundum crucible, calcinate at 800℃ for 2 h, cool to room temperature, grind again, and calcinate at 1000 ℃ for 20 h, repeat once; obtain layered K 0.80 Ti 1.73 Li 0.67 O 4 , Take 10 g obtained K 0.80 Ti 1.73 Li 0.67 O 4 The sample is added to 1000 ml, 1 mol / L hydrochloric acid solution and stirred, and the acid is changed every 24 h. After 4 days, it is washed with deionized water to neutrality and dried at 60 ℃, which is a layered H 1.07 Ti 1.73 O 4 •H 2 O; The above layered H 1.07 Ti 1.73 O 4 •H 2 O and TBAOH (tetrabutylammonium hydroxide) (40 wt%) solution were mixed at a molar ratio of 1:1, magnetically stirred for 15 days, centrifuged at 3000 rpm, and the unstripped layer was removed to obtain H 1.07 Ti 1.73 O 4 •H 2 O nanosheet sol, 1 mol / L hydrochloric acid was added dropwise under ultrasonic conditio...

Embodiment 2

[0029] Pd@H 1.07 Ti 1.73 O 4 •H 2 O nanosheets catalyze the hydroxylation of phenol to produce cyclohexanone under light induction.

[0030] Pd@H will be prepared 1.07 Ti 1.73 O 4 •H 2 O nanosheets are used as catalysts to achieve the hydroxylation of phenol under light induction to prepare cyclohexanone. Weigh 20 mg nanosheets and 100 mg silicotungstic acid, vacuumize to exhaust the air, add 2 mL purified water and 10 μL phenol. In H 2 Stir under conditions, then turn on the light source for photocatalytic reaction. The product is detected by gas chromatography; the light source used in the experiment is a 300 W xenon lamp; the conversion of phenol and the production of products are as follows image 3 As shown, it can be seen from the figure that when there is a catalyst, the conversion rate of aniline reaches 100% after 15 hours of light (curve a), and the yield of cyclohexanone reaches more than 99% (curve b). Or without light or with H 1.07 Ti 1.73 O 4 •H 2 Under the conditio...

Embodiment 3

[0032] M@H 1.07 Ti 1.73 O 4 •H 2 O(Au,Pd,Pt) nanosheets were prepared and used as a catalyst to photodehydrate water to produce hydrogen.

[0033] Preparation method: H 1.07 Ti 1.73 O 4 •H 2 Disperse the O nanosheets in 22 mL deionized water, and stir ultrasonically until they are evenly dispersed; under stirring, the HAuCl 4 • 4H 2 O, H 2 PtCl 6 • 6H 2 O or Pd(NO 3 ) 2 • 2H 2 The O solution was added dropwise to the solution, and 10 mL of methanol solution was added, nitrogen gas was added for 0.5 h, UV light was irradiated for 3-5 h, filtered, washed and dried to obtain M@H 1.07 Ti 1.73 O 4 •H 2 The loading amount of M in O(M=Au,Pd,Pt) is converted according to the optimal amount of 1wt%. From Figure 4 It can be seen that the synthesized catalyst has a strong SPR characteristic absorption peak.

[0034] Precious metals that will be prepared @H 1.07 Ti 1.73 O 4 •H 2 O(Au, Pt) nanosheets are catalysts for photolysis of water to produce hydrogen. Add 80 mg of catalyst to 72 mL of wa...

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Abstract

The invention discloses a nano-plate with precious metal and application of the nano-plate, and belongs to the field of catalytic material preparation.The M@H1.07Ti1.73O4 H2O nano-plate is used as a carrier, and metal nano-particles of Au, Pd, Pt and the like are loaded on nano-composite materials formed by the surfaces of the ultrathin H1.07Ti1.73O4 H2O nano-plate with monomolecular layers by the aid of a photodeposition reduction method.The nano-plate and the application have the advantages that the nano-composite materials are high in efficiency in the aspect of photocatalytic water splitting hydrogen production; the nano-composite materials can be used as photocatalysts for preparing cyclohexanone by means of phenol hydroxylation under a photoinduction condition, and accordingly problems of high energy consumption and cost, low selectivity and the like when cyclohexanone is prepared by means of phenol hydrogenation at high temperatures under high pressures can be solved; the nano-plates is simple in process, high in selectivity and low in energy consumption and cost, is environmentally friendly and has huge application potential, and actual production requirements can be met.

Description

Technical field [0001] The present invention belongs to the field of catalysis technology, and specifically relates to a precious metal @H 1.07 Ti 1.73 O 4 •H 2 O nanosheets and their applications. Background technique [0002] Cyclohexanone is an important organic chemical product with high solubility and low volatility. It can be used as a special solvent and an ideal solvent for polymers such as nitrocellulose and cellulose. It is also an important organic chemical raw material. It is the main intermediate for the preparation of nylon, caprolactam and adipic acid. With the development of social modernization, the use of cyclohexanone continues to expand. Especially as a high-grade organic solvent, it is widely used in coatings, inks, adhesives and other industries, forming a larger commodity market. At present, the methods commonly used to produce cyclohexanone include phenol hydrogenation, cyclohexene hydration and cyclohexane oxidation. However, these methods for preparing...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44B01J23/52C07C45/51C07C49/403C01B3/04
CPCB01J23/44B01J23/52B01J35/004B01J35/0073B01J35/023B01J37/345C01B3/042C01B2203/107C01B2203/1082C07C45/512C07C49/403Y02E60/36
Inventor 吴棱宋玉洁熊锦华刘玉豪罗水广梁诗景
Owner FUZHOU UNIV
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