Series-parallel synthesis method of polyborosilazane

A technology of polyborosilazane and parallel connection, which is applied in the field of organosilicon polymer materials, can solve the problems of unsuitability for large-scale production and low synthesis yield, and achieve small changes in liquid phase volume, few by-products, and high production efficiency. Improved effect

Active Publication Date: 2019-07-30
NAT UNIV OF DEFENSE TECH
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Problems solved by technology

[0004] The invention provides a serial-parallel synthesis method of polyborosilazane, which is used to overcome defects such as low synthesis yield and unsuitability for large-scale production in the prior art, realize high-yield synthesis and be suitable for large-scale production

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preparation example Construction

[0023] The present invention proposes a series-parallel synthesis method of polyborosilazane. For the synthesis process, see figure 1 The method for synthesizing polyborosilazane by using several parallel monomer synthesis kettles, pre-polymerization kettles, and polymerization kettles in series includes the following steps:

[0024] S1: Mix chlorosilane solution, boron trichloride solution and nitrogen-containing reagent in proportion to obtain mixed raw materials;

[0025] In the step S1, the molar ratio of the chlorosilane solution to the boron trichloride solution in the mixed raw material is (1:2) to (2:1), and the amount of the nitrogen-containing reagent is chlorosilane solution to trichloride 2 to 4 times the amount of the total substance of the boron solution;

[0026] The solute of the chlorosilane solution is SiR 1 Cl 3 or SiR 1 R 2 Cl 2 , R 1 and R 2 It can be methyl, phenyl, vinyl or hydrogen, and the solvent is n-hexane, cyclohexane or toluene; the molar ...

Embodiment 1

[0048] This embodiment provides a method for synthesizing polyborosilazane in series and parallel. The method for synthesizing polyborosilazane is a method in which three parallel monomer synthesis tanks, a pre-polymerization tank, and a polymerization tank are connected in series to synthesize polyborosilazane. ,

[0049] Include the following steps:

[0050] S1: Dichloromethylsilane solution (5mol / L, 16L), boron trichloride solution (5mol / L, 8L) and hexamethyldisilazane (240mol ) are mixed to obtain mixed raw materials; three parts are prepared;

[0051] S2: Add the three mixed raw materials obtained in step S1 into three parallel monomer synthesis tanks (100 L) cooled to -20°C at a rate of 100 mL / min, and then raise the temperature of the three parallel monomer synthesis tanks to 100°C;

[0052] S3: Transfer the products in the three parallel monomer synthesis tanks to a pre-polymerization tank (100 L) heated to 120°C for pre-polymerization;

[0053] S31: Transfer the p...

Embodiment 2

[0065] This embodiment provides a method for synthesizing polyborosilazane in series and parallel. The method for synthesizing polyborosilazane is a method in which three parallel monomer synthesis tanks, a pre-polymerization tank, and a polymerization tank are connected in series to synthesize polyborosilazane. ,

[0066] Include the following steps:

[0067] S1: Dichloromethylsilane solution (2mol / L, 30L), boron trichloride solution (2mol / L, 30L) and HN[Si(CH 3 ) 2 (CH 2 =CH 2 )] 2 (360mol) mix, obtain mixed raw material; Prepare three parts;

[0068] S2: Add the three mixed raw materials obtained in step S1 into three parallel monomer synthesis tanks (200 L) cooled to -50°C at a rate of 500 mL / min, and then raise the temperature of the three parallel monomer synthesis tanks to 100°C;

[0069] S3: Transfer the products in the three parallel monomer synthesis tanks to a pre-polymerization tank (200L) heated to 150°C for pre-polymerization;

[0070] S31: Transfer the p...

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Abstract

The invention discloses a series-parallel synthesis method of polyborosilazane. The series-parallel synthesis method is a method for synthesizing the polyborosilazane through serial connection by using a plurality of monomer synthesis kettles, pre-polymerization kettles and polymerization kettles which are connected in parallel. The method includes the steps that raw materials are prepared and mixed, monomers are synthesized, and pre-polymerization, polymerization, collection and cooling are carried out to obtain a polyborosilazane product. Compared with the prior art, the series-parallel synthesis method of the polyborosilazane greatly improves the production efficiency through step-by-step continuous reaction, and is suitable for large-scale production.

Description

technical field [0001] The invention relates to the technical field of organosilicon polymer materials, in particular to a series-parallel synthesis method of polyborosilazane. Background technique [0002] Polyborosilazane is an organic polymer containing Si, B, N, C, H and other elements, which can be used to prepare various forms of ceramic materials, such as SiBCN ceramic fiber, SiBN ceramic fiber, SiBCN ceramic matrix composite material , can also be used to modify other carbon materials or be modified by metal elements to prepare nanocomposites. It is an elemental organic polymer that has been widely studied in the past two decades. It is used as a precursor of thermal structural ceramic materials and structural-functional integration materials. It has a broad application space. [0003] Co-ammonolysis polymerization directly through chlorosilane and chloroborane is a reliable method for synthesizing polyborosilazane. The process route of this method is simple and rel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/62
CPCC08G77/62
Inventor 邵长伟王军王浩王兵
Owner NAT UNIV OF DEFENSE TECH
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