High-ceramic-yield polycarbosilane preparation method
A technology of polycarbosilane and ceramics, which is applied in the field of silicon carbide precursor preparation, can solve the problems of low ceramic yield, and achieve the effects of increasing ceramic yield, good application prospects, and mild reaction conditions
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Embodiment 1
[0021] Get the polycarbosilane (PCS) of 20g and be dissolved in the tetrahydrofuran (THF) of 30g, add in the 100ml flask after dissolving completely, add acrylonitrile 2g, under nitrogen protection, add rhodium-containing compound hydrosilylation type catalyst 0.001g, then The temperature of the reaction system was raised to 60° C. for 5 h. Finally, THF was removed by vacuum distillation to obtain cyano-containing polycarbosilane PCS-CN01.
[0022] figure 1 is the FTIR spectrogram of the PCS-CNO1 prepared above. 2240cm in the picture -1 There is an obvious -C≡N peak at 2100cm -1 Si-H at 1245cm -1 The intensity ratio of Si-CH3 at Si-CH3 is 0.88, while that of the original PCS, that is, the unmodified PCS before the reaction is 0.94, indicating that the cyano group was introduced into the PCS molecule.
[0023] figure 2 It is the thermogravimetric (TG) curve figure of the above-mentioned PCS-CNO1 and unmodified PCS under nitrogen atmosphere. It can be seen that the ceram...
Embodiment 2
[0025] Get 20g of the same polycarbosilane (PCS) as Example 1 and dissolve it in 30g of xylene, add it to a 100ml flask after dissolving completely, add 3g of acrylonitrile, and under nitrogen protection, add 0.2 azobisisobutyronitrile catalyst g, and then the reaction system was heated to 65° C. for 8 h. Finally, xylene was removed by vacuum distillation to obtain cyano-containing polycarbosilane PCS-CN02.
[0026] Same as Example 1, according to the FTIR spectrum of the PCS-CN02 prepared above, it can be drawn that the cyano group is introduced into the PCS molecule.
[0027] Same as Example 1, the PCS-CN02 and unmodified PCS prepared above were subjected to thermogravimetric (TG) analysis under a nitrogen atmosphere, and the ceramic yield of PCS-CN02 was 75%, which was greatly increased compared with PCS.
Embodiment 3
[0029] Get 25g of aluminum-containing polycarbosilane (PACS) and dissolve it in 30g of xylene, add it into a 100ml flask after dissolving completely, add 2g of methacrylonitrile, under nitrogen protection, add 0.2g of azobisisobutyronitrile catalyst, Then the reaction system was heated to 70°C for 5 h. Finally, xylene was removed by vacuum distillation to obtain cyano-containing polyaluminocarbosilane PACS-CN03.
[0030] Same as Example 1, according to the FTIR spectrum of the PACS-CN03 prepared above, it can be concluded that the cyano group is introduced into the PCS molecule.
[0031] Same as Example 1, the above-mentioned PACS-CN03 and unmodified PACS were subjected to thermogravimetric (TG) analysis under a nitrogen atmosphere, and the ceramic yields of PACS and PACS-CN03 were respectively 55% and 78%, Compared with PACS, the ceramic yield of PACS-CN03 is greatly increased.
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