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Magnetic silicon-lithium catalyst as well as preparation method and application thereof

A lithium catalyst and catalyst technology, applied in the field of chemical materials, can solve the problems of insufficient green economy, high cost, and large environmental pollution, and achieve the effects of good reaction activity and selectivity, less loss of active components, and high catalytic activity.

Active Publication Date: 2021-01-26
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing synthesis methods are generally in high temperature and strong acidic or alkaline environment, and many of them use halogenation as a common raw material. The synthesis method is not green and economical enough, and the environmental pollution is relatively large and the cost is relatively high.

Method used

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  • Magnetic silicon-lithium catalyst as well as preparation method and application thereof
  • Magnetic silicon-lithium catalyst as well as preparation method and application thereof
  • Magnetic silicon-lithium catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The preparation of embodiment 1 magnetic silicon lithium catalyst

[0042] Weigh 4.0g magnetic Fe 3 o 4 Put into 160mL ethanol-water mixture (ethanol / water=7 / 1), ultrasonically disperse for 30min, add 10mL tetraethyl orthosilicate and 10mL ammonia water to the mixture, stir mechanically for 20h; filter with suction, wash with deionized water 3 times , and then washed the precipitate with absolute ethanol for 3 times, and dried in vacuum at 100°C for 24 hours to obtain Fe 3 o 4 @SiO 2 ; Add 0.8g lithium chloride, 1.5g Fe in the flask 3 o 4 @SiO 2 React with 20mL methanol at 75°C for 12h at reflux. After the reaction, cool to room temperature, remove excess methanol by rotary evaporation, filter with suction, wash the precipitate with absolute ethanol 3 times, and vacuum dry at 90°C for 24h to obtain the silicon lithium catalyst.

[0043] figure 1 The SEM image of the prepared magnetic silicon-lithium catalyst shows that the surface morphology of the silicon-lithi...

Embodiment 2

[0044] The preparation of embodiment 2 magnetic silicon lithium catalysts

[0045] Weigh 4.0g magnetic Fe 3 o 4 Put into 160mL ethanol-water mixture (ethanol / water=7 / 1), ultrasonically disperse for 30min, add 10mL tetraethyl orthosilicate and 10mL ammonia water to the mixture, stir mechanically for 20h; filter with suction, wash with deionized water 3 times , and then washed the precipitate with absolute ethanol for 3 times, and dried in vacuum at 100°C for 24 hours to obtain Fe 3 o 4 @SiO 2 ; Add 0.9g lithium chloride, 1.8g Fe in the flask 3 o 4 @SiO 2 React with 75mL of methanol at 50°C for 72h at reflux. After the reaction, cool to room temperature, remove excess methanol by rotary evaporation, filter with suction, wash the precipitate with absolute ethanol 6 times, and dry in vacuum at 80°C for 72h to obtain the silicon-lithium catalyst. The preparation of embodiment 3 magnetic silicon lithium catalysts

Embodiment 3

[0046] Weigh 4.0g magnetic Fe 3 o 4 Put into 160mL ethanol-water mixture (ethanol / water=7 / 1), ultrasonically disperse for 30min, add 10mL tetraethyl orthosilicate and 10mL ammonia water to the mixture, stir mechanically for 20h; filter with suction, wash with deionized water 3 times , and then washed the precipitate with absolute ethanol for 3 times, and dried in vacuum at 100°C for 24 hours to obtain Fe 3 o 4 @SiO 2 ; Add 1.0g lithium chloride, 2.0g Fe in the flask 3 o 4 @SiO 2 and 55mL methanol, reflux at 110°C for 72h, after the reaction, cool to room temperature, remove excess methanol by rotary evaporation, filter with suction, wash the precipitate with absolute ethanol 3 times, and vacuum dry at 90°C for 24h to obtain the silicon-lithium catalyst.

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Abstract

The invention discloses a magnetic silicon-lithium catalyst as well as a preparation method and application thereof, and belongs to the field of chemical materials. The preparation method comprises the following steps: designing and synthesizing a magnetic Fe3O4@ SiO2 composite carrier, mixing lithium chloride, Fe3O4@ SiO2 and methanol, carrying out reflux reaction at 50-130 DEG C for 2-72 hours,performing cooling, carrying out rotary evaporation to remove excessive methanol after the reaction is finished, carrying out suction filtration, washing, and drying to obtain the silicon-lithium catalyst. The prepared magnetic silicon-lithium catalyst can be used in the synthesis of benzoquinone compounds, the chemical selectivity of the product is very high and can reach 100%, and the yield is over 90%; the catalyst can be recycled by an external magnet, the loss of active components is less, and the cost is saved. In addition, the catalyst provided by the invention can also be used for catalyzing bisphenol F synthesis, and has high reaction activity and selectivity.

Description

technical field [0001] The invention relates to a magnetic silicon-lithium catalyst and a preparation method and application thereof, belonging to the field of chemical materials. Background technique [0002] Quinone compounds include benzoquinone, naphthoquinone, phenanthraquinones, anthraquinone and their derivatives. Most quinone compounds have phenolic or hydroxyl groups. Some phenolic compounds, such as polyphenols and tannins, are easily oxidized into quinones, such as anthraquinone, which are often accompanied by tannins. Quinone compounds widely exist in the plant kingdom, and their pharmacological activities have also attracted much attention. Among them, benzoquinone compounds and their unique chemical properties have attracted wide attention. Most benzoquinones in nature exist in plants, and the main benzoquinones in plants are p-benzoquinone and its derivatives. Such benzoquinone compounds have special effects such as antibacterial and insect repellent. How...

Claims

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Application Information

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IPC IPC(8): B01J23/745B01J23/78B01J32/00B01J37/02C07C37/20C07C39/16C07C315/00C07C317/24
CPCB01J23/745B01J23/78B01J23/002B01J37/0201C07C37/20C07C315/00C07C2601/16B01J35/33C07C39/16C07C317/24Y02P20/584
Inventor 王大伟朱观鑫夏晓峰吴强倪才华
Owner JIANGNAN UNIV
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