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Method for electrochemically preparing boron-containing polysilane

A polysilane, electrochemical technology, applied in electrolytic components, electrolytic process, electrolytic organic production, etc., can solve the problems of high synthesis cost, low ceramic yield, high raw material price, etc., and achieve high ceramic conversion rate and mild reaction conditions. , the effect of low price of raw materials

Active Publication Date: 2021-08-10
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the ceramic yield of this method is low, the price of raw materials is high, and the synthesis cost is high (Zhu Yihua, Wang Hao, Shao Changwei. Synthesis and characterization of SiC ceramic precursors with high boron content[J]. Chemical Journal of Chinese Universities, 2013, 34( 10): 2415-2420)

Method used

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  • Method for electrochemically preparing boron-containing polysilane
  • Method for electrochemically preparing boron-containing polysilane
  • Method for electrochemically preparing boron-containing polysilane

Examples

Experimental program
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Embodiment 1

[0028] In this example, see figure 1 , using an electrochemical reaction setup, including N 2 Gas cylinder 1, drying tower as molecular sieve 2, calcium chloride drying tower 3, ultrasonic equipment 4, magnesium electrode 5, rubber stopper 6, ventilation pipe 7, stirring rod 8, motor 9, feeding pipe 10, thermometer 11 and electrodes wire. Utilize the rubber stopper 6 to seal the electrochemical reaction bottle, the ventilation pipe 7, the stirring rod 8, the feed pipe 10, the thermometer 11, and the electrode wire are respectively installed and set through the rubber stopper 6, and the motor 9 is used to drive the 8 pairs of stirring rods The solution in the electrochemical reaction bottle is stirred, and the ultrasonic device 4 ultrasonically stirs the solution in the electrochemical reaction bottle, and the magnesium electrode 5 is immersed in the solution in the electrochemical reaction bottle made of metal magnesium, and the vent tube 7 is made of N 2 Cylinder 1 as gas s...

Embodiment 2

[0039] This embodiment is basically the same as Embodiment 1, especially in that:

[0040] In this embodiment, using the electrochemical reaction device of this embodiment, a method for electrochemically preparing boron-containing polysilane, using trihalosilane, allyl chloride, and sodium borohydride as raw materials, wherein trihalosilane, allyl The molar ratio of base chloride to sodium borohydride is 3:1:1, tetrahydrofuran is used as solvent, lithium perchlorate is used as electrolyte, metal magnesium material is used as electrode, and it is obtained by electrochemical reaction under a periodically reversing DC electric field. Boron-containing polysilane comprises the steps of:

[0041] a. Add 0.15 mol propyltrichlorosilane and 0.05 mol allyl chloride into the electrochemical reverse bottle equipped with vent tube and stirring rod 8, and add sodium dehydration to the electrochemical reverse bottle at the same time, and distill to obtain the 66 °C fraction Treated 130ml te...

Embodiment 3

[0048] This embodiment is basically the same as the previous embodiment, and the special features are:

[0049] In this embodiment, using the electrochemical reaction device of this embodiment, a method for electrochemically preparing boron-containing polysilane, using trihalosilane, allyl chloride, and sodium borohydride as raw materials, wherein trihalosilane, allyl The molar ratio of base chloride to sodium borohydride is 3:1:1, tetrahydrofuran is used as solvent, lithium perchlorate is used as electrolyte, metal magnesium material is used as electrode, and it is obtained by electrochemical reaction under a periodically reversing DC electric field. Boron-containing polysilane comprises the steps of:

[0050] a. Add 0.15mol of phenyltrichlorosilane and 0.05mol of allyl chloride into the electrochemical inversion bottle equipped with vent tube and stirring rod 8, at the same time, add sodium dehydration to the electrochemical inversion bottle, and distill the 66°C fraction T...

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Abstract

The invention discloses a method for electrochemically preparing boron-containing polysilane, which belongs to the field of inorganic non-metallic materials. Under the condition of room temperature and inert gas protection, trihalosilane, allyl chloride and sodium borohydride are used as raw materials, anhydrous tetrahydrofuran is used as solvent, lithium perchlorate is used as electrolyte, and metal magnesium blocks are used as electrodes. The electrochemical reaction is carried out under the field to obtain boron-containing polysilane. The reaction conditions of the method are mild, safe and controllable, the raw material price is low, and the prepared precursor has a high ceramic conversion rate, which can be used to prepare silicon carbide-boron carbide or silicon-boron-carbon-nitrogen high-temperature ceramics, and is used in the preparation of high-performance high-temperature ceramics The field of materials has broad application prospects.

Description

technical field [0001] The invention relates to a method for preparing a silicon polymer, in particular to a method for preparing a high polymer containing silicon and boron atoms in a skeleton, which is applied to the technical fields of polymer materials and ceramic precursor materials. Background technique [0002] Boron-containing polysilane is a kind of high polymer containing silicon and boron atoms in the skeleton. As a ceramic precursor, silicon carbide-boron carbide can be prepared by high-temperature pyrolysis under an inert atmosphere, or silicon-boron carbon can be prepared by high-temperature treatment under a nitrogen atmosphere. Nitrogen ceramic material. Compared with boron-based or silicon-based ceramics with a simple composition, after the precursor polymer containing both B and Si elements is cracked, a high-temperature ceramic material with a multi-component composition and excellent structural stability can be obtained, which can be used in aerospace and...

Claims

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Application Information

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IPC IPC(8): C08G77/06C08G79/08C25B3/29C25B3/09C25B3/11
CPCC25B3/29
Inventor 甄强谢佳姮陈来
Owner SHANGHAI UNIV
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