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Hyper-branched silicon-contained aryne polymer and preparation method thereof

A technology for a polymer and a silicon aryne, which is applied in the field of preparation of the hyperbranched silicon-containing aryne polymer to achieve the effects of easy storage and excellent thermal stability

Inactive Publication Date: 2010-04-14
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The hyperbranched silicon-containing aryne polymer of the present invention is a novel hyperbranched polymer containing a Si-≡-Ar structure, and there is no relevant report in the literature

Method used

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  • Hyper-branched silicon-contained aryne polymer and preparation method thereof
  • Hyper-branched silicon-contained aryne polymer and preparation method thereof
  • Hyper-branched silicon-contained aryne polymer and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0022] Under nitrogen protection, place magnesium powder 3.3g (138mmol) / THF (80ml) in a four-necked flask, cool with a cold water bath, and add bromoethane (EtBr) 13.6g (126mmol) / THF (30ml) , and after reacting at 50°C for 2 hours, 7.56 g (60 mmol) / THF (30 ml) of diethynylbenzene was added dropwise to the cooled system, and reacted at 70°C for 2 hours. The system was cooled to room temperature, and methyltrichlorosilane (CH 3 SiCl 3 ) 3.0 g (20 mmol), and kept at 70° C. for 5 hours. The reaction was terminated with acid and extracted with toluene. After washing with water, the organic phase was taken, and the solvent was distilled off under reduced pressure to obtain a brown viscous liquid. Its infrared spectrum is as figure 1 , H NMR spectrum ( 1 H NMR) such as figure 2 , NMR carbon spectrum ( 13 C NMR) such as image 3 , NMR spectrum silicon spectrum ( 29 Si NMR) such as Figure 4 . The molecular weight is 771 and the PDI is 3.64.

Embodiment 2

[0024] Under the protection of nitrogen, place 2.5g (103mmol) of magnesium powder in a four-necked flask, use toluene and ether as a mixed solvent, cool with a cold water bath, and add 10.2g (94mmol) of EtBr to it, and then react at 40°C for 3 hours , 5.67 g (45 mmol) of diethynylbenzene was added dropwise to the cooled system, and reacted at 50° C. for 5 hours. The system was cooled to room temperature, and methyltrichlorosilane (CH 3 SiCl 3 ) 3.0 g (20 mmol), and kept at 60° C. for 4 hours. The reaction was terminated with acid and extracted with toluene. After washing with water, the organic phase was taken, and the solvent was distilled off under reduced pressure to obtain a brown viscous liquid. The molecular weight is 1130 and the PDI is 3.25.

Embodiment 3

[0026] Under nitrogen protection, magnesium powder 2.5g (103mmol) / THF (60ml) was placed in the four-necked flask, cooled with a cold water bath, and bromopentane 14.2g (94mmol) / THF (20ml) was added thereto, and then 50 After reacting at °C for 3 hours, 5.67 g (45 mmol) / THF (20 ml) of diethynylbenzene was added dropwise to the cooled system, and reacted at 40 °C for 5 hours. The system was cooled to room temperature, and methyltrichlorosilane (CH 3 SiCl 3 ) 3.29g (22mmol), and kept at 70°C for 3 hours. Terminate the reaction with acid and extract with toluene. After washing with water, take the organic phase, precipitate with methanol, filter with suction, wash and dry in vacuum to obtain a light yellow solid powder. The molecular weight is 7380 and the PDI is 2.92.

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Abstract

The invention discloses a hyper-branched silicon-contained aryne polymer and a preparation method thereof. The polymer is structurally characterized in that the polymer is a hyper-branched structure containing silicone atoms and aryne group. The preparation method of the polymer comprises the following steps: taking diethynyl-benzene, trichlorosilane or tetrachlorosilane, halohydrocarbon and magnesium powders as raw materials, and synthesizing the hyper-branched silicon-contained aryne polymer by the following three steps under the protection of inert gas: the halohydrocarbon and the magnesium powders react to generate the alkyl magnesium halide Grignard reagent firstly; the alkyl magnesium halide Grignard reagent and the diethynyl-benzene react to generate the diphenylacetylene magnesium halide Grignard reagent subsequently, and the diphenylacetylene magnesium halide Grignard reagent and the trichlorosilane or tetrachlorosilane react to generate the hyper-branched silicon-contained aryne polymer. In the invention, the process is simple, the operation is convenient, the reaction time is short, the process condition is easy to be controlled, and the post processing is simple. The prepared hyper-branched polymer is brown viscous liquid or primrose yellow powdered solid, is stable at room temperature and is easy for storage, and the condensate thereof has excellent thermal stability.

Description

technical field [0001] The invention relates to a novel hyperbranched silicon-containing aryne polymer, and also relates to a preparation method of the hyperbranched silicon-containing aryne polymer. Background technique [0002] Hyperbranched polymer is a highly branched three-dimensional spherical polymer with a large number of terminal functional groups gathered on the surface of the molecular structure. Compared with linear polymers, hyperbranched polymers have low viscosity and good solubility. Organosilicon polymers are special polymer materials with unique physical and chemical properties, and are widely used in high-tech fields such as aerospace electronic information. In recent years, organosilicon polymers in which silicon and carbon-carbon triple bonds are simultaneously introduced into the polymer molecular chain have aroused great interest. This kind of polymer has good processing performance, and under the action of high temperature or catalyst, it can be cros...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60C08G77/50
Inventor 齐会民杜磊黄发荣徐美玲刘衍兵黄云辉扈艳红周燕
Owner EAST CHINA UNIV OF SCI & TECH
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