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Catalyst for biphenyl preparation as well as preparation method and application thereof

A technology of catalyst and biphenyl, which is applied in the field of catalysts for the preparation of biphenyl and its preparation, can solve the problems of limited application, difficulty in modifying the neutral skeleton structure, and low yield, and achieve high catalytic efficiency, high utilization rate of precious metals, and preparation The effect of simple process

Active Publication Date: 2020-04-28
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2014, Corma et al. first reported the use of supported Au catalysts in O 2 The system catalyzes the oxidative coupling reaction of benzene to biphenyl, and various inert substrates such as benzene, toluene, chlorobenzene, etc. can be selectively converted into corresponding biaryls, but the actual product yield is less than 2%.
However, most of the reported covalently bonded POSS porous polymers are neutral framework structures that are difficult to modify, and their applications are limited to general gas adsorption.

Method used

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  • Catalyst for biphenyl preparation as well as preparation method and application thereof
  • Catalyst for biphenyl preparation as well as preparation method and application thereof
  • Catalyst for biphenyl preparation as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 200 mL of anhydrous methanol and 6 mL of concentrated hydrochloric acid into a 250 mL round bottom flask, and slowly add 20 g of chloromethyltriethoxysilane while stirring at room temperature. The above solution was heated and sealed in a water bath at 40°C for two weeks. After the reaction, the solvent was removed by rotary evaporation and dried in vacuo to finally obtain a white crystal product, namely ClMePOSS, with a yield of 90%.

[0032] 0.6 g of ClMePOSS and 0.4 g of trimidazolylbenzene were dissolved in 10 mL of THF, and then the solution was placed in a Teflon-lined stainless steel reactor and reacted statically in an oven at 100 °C for 48 h. After the reaction, the resulting gel-like monolithic solid was cut into small pieces and stirred in an ethanol solvent for 2 hours, and then the dispersed ionic colloidal suspension solution was suction-filtered, thoroughly washed with ethanol, THF, and water, and vacuum-dried. Finally, a light brown solid product is...

Embodiment 2

[0038] Add 100 mL of anhydrous methanol and 4 mL of concentrated hydrochloric acid into a 250 mL round bottom flask, and slowly add 10 g of chloromethyltriethoxysilane under stirring at room temperature. The above solution was heated and sealed in a water bath at 40°C for two weeks. After the reaction, the solvent was removed by rotary evaporation and dried in vacuo to finally obtain a white crystal product, namely ClMePOSS, with a yield of 90%.

[0039] 0.3 g of ClMePOSS and 0.4 g of 1,2-diimidazolethane were dissolved in 10 mL of THF, and then the solution was placed in a Teflon-lined stainless steel reactor and reacted statically in an oven at 100 °C for 48 h. After the reaction, the resulting gel-like monolithic solid was cut into small pieces and stirred in an ethanol solvent for 2 hours, and then the well-dispersed ionic colloidal suspension solution was suction-filtered, thoroughly washed with ethanol, THF, and water, and vacuum-dried. , and finally obtain a light brow...

Embodiment 3

[0045] Put 1.5mmol benzene, 0.02gAu@PCIF-1, 5mL acetic acid, and 0.02g trifluoroacetic acid in a closed high-pressure reactor and mix evenly. Oxygen is introduced into the reactor, and the pressure of the reaction system in the reactor is 8 atm. Maintain the temperature of the reactor At 120° C., oxidative coupling reaction was carried out for 10 h to obtain biphenyl, the yield of biphenyl was 3.4%, the conversion rate of benzene was 3.5%, and the selectivity of biphenyl was 95.0%.

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Abstract

The invention discloses a catalyst for biphenyl preparation and a preparation method and application thereof, and belongs to the technical field of chemical catalysis. The catalyst comprises nanogoldAu and an imidazolyl porous ion frame PCIF loaded with nanogold. The method comprises the following steps: putting benzene, a catalyst, a solvent and an additive into a closed reaction kettle, uniformly mixing, introducing oxygen into the reaction kettle, keeping the pressure of the reaction system in the kettle within the range of 8-20 atm, keeping the temperature of the reaction kettle within the range of 100-180 DEG C, and carrying out an oxidative coupling reaction to obtain biphenyl. The catalyst that is Au@PCIF has the advantages of rich ion sites, high nano-gold dispersity, high catalytic efficiency, a simple preparation process, stability, difficulty in decomposition, easiness in separation from a liquid phase, high precious metal utilization rate and the like, has high selectivityand conversion rate in biphenyl preparation, and has high industrial application value.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysis, and in particular relates to a catalyst for biphenyl preparation, a preparation method and application thereof. Background technique [0002] With the rapid development of petrochemical, fine chemical and electronic chemical industry, biphenyl has gradually occupied an important position in pharmaceutical chemical industry, electronic chemical industry and other industries. In recent years, with the increasing demand for pharmaceutical products and liquid crystal products, the demand for biphenyl has increased significantly year by year. However, the domestic production of biphenyl is much smaller than the domestic demand for biphenyl, and most of the biphenyl needs to be imported. [0003] At present, the industrial preparation methods of biphenyl mainly include the chemical synthesis of biphenyl by pyrolysis of benzene and the traditional coupling method. These preparation methods ...

Claims

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Application Information

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IPC IPC(8): B01J31/06C07C2/84C07C15/14
CPCB01J31/06C07C2/84B01J2231/4205B01J2231/70C07C2531/06B01J35/394B01J35/393C07C15/14
Inventor 刘阳庆孙静雯姚康许琦
Owner YANCHENG INST OF TECH
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