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Method for synthesizing ceramic precursor polycarbosilane

A technology of ceramic precursor and polycarbosilane, applied in the direction of silicon organic compounds, etc., can solve the problems of low product purity, difficult to be suitable for the production and preparation of high-performance ceramic materials, etc., and achieves low alkali metal content, easy control of product structure, and high product quality. The effect of the structure is easy to control

Active Publication Date: 2012-07-25
苏州赛力菲陶纤有限公司
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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for synthesizing ceramic precursor polycarbosilane, which solves the problems in the prior art that the purity of the product obtained by the synthesis method of ceramic precursor polycarbosilane is not high, and it is difficult to be suitable for the production and preparation of high-performance ceramic materials.

Method used

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  • Method for synthesizing ceramic precursor polycarbosilane
  • Method for synthesizing ceramic precursor polycarbosilane
  • Method for synthesizing ceramic precursor polycarbosilane

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Embodiment 1

[0046] The synthesis of embodiment 1 polycarbosilane

[0047] Dimethyldichlorosilane and metal sodium are polycondensed in xylene to obtain polydimethylpolysilane, which is neutralized by methanol and washed with water and dried to obtain a white solid powder; the white solid powder is cracked at 300°C to form a ring Silane-based liquid substances. figure 1 Infrared spectrum of cyclosilane.

[0048] Add 120-160 kg of CPS engineering reagents into a 300-liter rearrangement polymerization reactor with an external heating ring-opening cracking system, fill it with pure nitrogen, heat it to 300-350°C, and turn on the external heating device 300°C, strictly control the liquid reflux rate, and then fill the nitrogen system, rearrange the polymerization kettle, gradually (heating rate 0.1°C / min) to 380-470°C, and keep warm for 10-50 hours.

[0049] Stop heating, after being cooled to a certain temperature (200~250 ℃), obtain viscous tan liquid, the tan liquid is by tan liquid: xyle...

Embodiment 2

[0054] The synthesis of embodiment 2 polycarbosilane

[0055] Cyclosilane raw materials were purchased from Zhangjiagang Laibao Silicone Products R&D Center, and other raw materials were conventional reagents.

[0056] In the engineering test of adding 150 kg of CPS to a 300-liter rearrangement polymerization reactor with an external heating and ring-opening cracking system, after filling with pure nitrogen, after heating to 300-350 °C, open the external heating device 300 ~350°C, strictly control the liquid reflux rate, then fill the nitrogen system, rearrange the polymerization kettle, gradually (heating rate 0.1°C / min) to 350-500°C, and keep warm for 10-50 hours. Stop heating, after cooling to a certain temperature (100~250 ℃), obtain viscous tan polycarbosilane (PCS), it is dissolved in xylene (PCS: xylene (weight ratio)=1: 4~5 ) after fully dissolving, filter, remove the solvent in the distillation kettle, and keep warm at a vacuum degree (0.04-0.1MPa) of 200-300°C. Aft...

Embodiment 3

[0057] Synthesis and performance comparison test of embodiment 3 comparative example polycarbosilane

[0058] COMPARATIVE EXAMPLE In the 300-liter reactor of Example 1, 80-100 kg of powdery PDMS were thrown in, and polycarbosilane was prepared directly according to the conditions commonly used in the prior art.

[0059] Performance test method: wherein melting point test method: microscope melting point apparatus; Molecular weight determination and distribution: GPC, solvent; Infrared spectrum measurement: in Hitachi (Hitachi) 285 grid type infrared spectrometer, KBr tablet method; Na+ determination: by Shanghai Testing center; TGA analysis with Rigaku micro-thermometer, at 10°C / min, N 2 Atmosphere, 900°C.

[0060] Under the same above-mentioned reaction conditions and in the same purification treatment process, the polycarbosilane obtained, except that the PCS melting point is slightly higher, other structures are equivalent to Example 1, but Na in the PCS molecule + The co...

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Abstract

The invention discloses a method for synthesizing ceramic precursor polycarbosilane. The method is characterized by comprising the following steps of: cracking cyclosilane serving as a raw material at the temperature of between 350 and 500 DEG C under the protection of an inert gas or nitrogen; and then performing molecular rearrangement to form the polycarbosilane (PCS). In the method, the structure of the whole reaction temperature product is easy to control; the alkali metal content of the product PCS is low; and the test is performed under normal pressure, without high-pressure equipment or adding a catalyst, so the equipment is simple and practicable.

Description

technical field [0001] The invention belongs to the technical field of synthesis of high-performance ceramic materials, and in particular relates to a method for synthesizing a ceramic precursor polycarbosilane. Background technique [0002] High-performance ceramic materials have extremely high temperature resistance, oxidation resistance, wear resistance and anti-corrosion properties. It is a high-tech new material that is incomparable to general metal materials and polymer materials. It has a wide range of applications in various fields. For high-performance ceramic materials (such as ceramic fiber, ceramic block, ceramic matrix composite material coating powder, etc.), countries have given special attention to the foundation and application and engineering, especially in information, national defense, modern transportation and It is placed in an important position in the energy industry. [0003] Due to the high melting point and high hardness of ceramics, it is general...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/60C07F7/21C04B35/565
Inventor 张卫中田秀梅吕斌
Owner 苏州赛力菲陶纤有限公司
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