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An m-ti hydrotalcite-based closed boron cluster mb x h x Preparation method and application of nanometer precious metal

A closed-type, hydrotalcite-based technology, which is applied in the field of preparation of M-Ti hydrotalcite-based closed-type boron cluster MBxHx nanoscale noble metals, can solve the problems of difficult catalyst recovery, high reaction temperature, and unfriendly environment, and achieve reuse High rate, high conversion rate, good environmental effect

Active Publication Date: 2022-07-05
WUHAN UNIV
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

In addition to being able to be extracted from petroleum components, phenol is mainly derived from organic synthesis. The commonly used synthetic methods in industry include the three-step method of cumene, and the hydrolysis of bromobenzene in alkaline water. The process is complex, unfriendly to the environment, and costly. Higher disadvantages greatly limit its development. At present, the one-step oxidation of benzene to obtain phenol has gradually become a research hotspot, but there are also disadvantages such as high reaction temperature and difficult recovery of catalysts.

Method used

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  • An m-ti hydrotalcite-based closed boron cluster mb <sub>x</sub> h <sub>x</sub> Preparation method and application of nanometer precious metal
  • An m-ti hydrotalcite-based closed boron cluster mb <sub>x</sub> h <sub>x</sub> Preparation method and application of nanometer precious metal
  • An m-ti hydrotalcite-based closed boron cluster mb <sub>x</sub> h <sub>x</sub> Preparation method and application of nanometer precious metal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Dissolve 4.0003g of urea in 100mL of water, and add 0.2003g of TiCl dropwise simultaneously 4 and 1.0011g closed boron cluster MgB 12 H 12 solution;

[0029] (2) Continue stirring for 3h under nitrogen protection, age in a hydrothermal kettle for 24h at 140°C, filter, wash and dry to obtain 2.8429g Mg-Ti hydrotalcite-based closed boron cluster MgB 12 H 12 ,like figure 1 As shown, the Mg-Ti hydrotalcite-based closed boron cluster MgB prepared in this example 12 H 12 The infrared spectrum of , the successful combination of hydrotalcite and boron clusters can be seen by Fourier transform infrared spectroscopy (FT-IR);

[0030] (3) 2.8001Mg-Ti hydrotalcite-based closed boron cluster MgB 12 H 12 Disperse in 50 mL of water, add 0.0558 g of sodium chloroaurate, stir and react for 5 min at 20 °C under a 365 nm UV lamp, filter to obtain a precipitate, repeatedly wash with ethanol and water, and dry at room temperature to obtain 2.8357 g of Mg-Ti hydrotalcite-based co...

Embodiment 2

[0033] (1) Dissolve 3.7416g of urea in 100mL of water, and add 0.2481g of TiCl dropwise simultaneously 4 and 1.2469g closed boron cluster CoB 12 H 12 solution;

[0034] (2) Continue stirring for 1 h under nitrogen protection, age in a hydrothermal kettle for 48 h at 120 °C, filter, wash and dry to obtain 3.2094 g Co-Ti hydrotalcite-based closed boron cluster CoB 12 H 12 ;

[0035] (3) 3.2001g Co-Ti hydrotalcite-based closed boron cluster CoB 12 H 12 Disperse in 50mL of water, add 0.0798g of sodium chloropalladate, stir and react for 10min at 35°C under a 400nm UV lamp, filter to obtain a precipitate, repeatedly wash with ethanol and water, and dry at room temperature to obtain 3.2518g of Co-Ti hydrotalcite base compound. boron cluster CoB 12 H 12 Nano-palladium catalyst;

[0036] (4) Dissolve 4.0102g of benzene in 10mL of acetonitrile, add 0.2004g of Co-Ti hydrotalcite-based closed boron cluster CoB 12 H 12 The nano-palladium catalyst and 3.9746g of 30% hydrogen per...

Embodiment 3

[0038] (1) Dissolve 2.8614g NaOH in 100mL water, and add 0.1910g butyl phthalate and 0.7628g closed boron cluster MgB dropwise at the same time. 10 H 10 solution;

[0039] (2) Continue stirring for 2h under nitrogen protection, age in a hydrothermal kettle for 72h at 80°C, filter, wash and dry to obtain 2.1778g Mg-Ti hydrotalcite-based closed boron cluster MgB 10 H 10 ;

[0040] (3) 2.0005g Mg-Ti hydrotalcite-based closed boron cluster MgB 10 H 10 Disperse in 50 mL of water, add 0.0399 g of sodium chloroplatinate, stir and react for 10 min at 40 °C under a 200 nm UV lamp, filter to obtain a precipitate, repeatedly wash with ethanol and water, and dry at room temperature to obtain 2.0341 g of Mg-Ti hydrotalcite-based compound. boron cluster MgB 10 H 10 Nano platinum catalyst;

[0041] (4) Dissolve 1.9989g benzene in 10mL acetonitrile, add 0.1975g Mg-Ti hydrotalcite-based closed boron cluster MgB 10 H 10 Nano-platinum catalyst and 2.9891g of 30% hydrogen peroxide were ...

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Abstract

The invention relates to the technical field of hydrotalcite material supported catalysts, in particular to an M-Ti hydrotalcite-based closed boron cluster MB x H x The preparation method and application of nano-scale precious metal, the specific steps are as follows: dissolving alkali in water, adding dropwise soluble titanium salt and closed boron cluster MB respectively at the same time x H x The solution was continuously stirred under nitrogen protection until the reaction was complete, and then aged to obtain M-Ti hydrotalcite-based closed boron clusters MB x H x ; M-Ti hydrotalcite-based closed boron cluster MB x H x Disperse in water, add soluble salt of precious metal, stir and react under ultraviolet light irradiation at 20-50°C, filter to obtain precipitate, wash and dry to obtain the M-Ti hydrotalcite-based closed boron cluster MB x H x Nanoscale precious metals. The invention utilizes the reducibility of closed boron clusters, in-situ supports nano-precious metal particles on the surface of hydrotalcite, and the precious metal is wrapped by boron clusters, which is more stable and not easy to fall off.

Description

technical field [0001] The invention relates to the technical field of hydrotalcite material supported catalysts, in particular to an M-Ti hydrotalcite-based closed boron cluster MB x H x Preparation method and application of nanometer precious metal. Background technique [0002] Hydrotalcite is a layered inorganic material of double metal oxyhydroxide, which has interlayer ion exchangeability and controllability of size distribution, and has a wide range of roles in catalysis, adsorption, degradation, medicine, sterilization, etc. According to different metal combinations, hydrotalcites have different effects. Among them, Ti-containing hydrotalcites have good photocatalytic activity. The reason is that the band gap of Ti is wide, and electron transitions can be excited under the excitation of ultraviolet light. At the same time, according to the water The ion exchangeability of talc can also introduce different anions, which has a certain synergistic effect on photocatal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/52B01J23/89B01J23/50B01J23/72B01J23/60B01J23/44B01J23/68C07C37/60C07C39/04C07C39/08C07C37/58
CPCB01J23/66B01J23/52B01J23/8913B01J23/42B01J23/58B01J23/892B01J23/688B01J23/72B01J23/8906B01J23/60B01J23/8926B01J23/44C07C37/60C07C37/58C07C39/04C07C39/08Y02P20/52
Inventor 张海波邓雪帆周晓海
Owner WUHAN UNIV
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