Preparation methods of benzocyclobutene functionalized cage type polysilsesquioxane (POSS) and resins of benzocyclobutene functionalized cage type polysilsesquioxane

[0050] Example 1:

[0051] Benzocyclobutene functionalized cage polysilsesquioxane is characterized in that the compound has the chemical structural formula shown in (IV):

[0052]

[0053] Where:

[0054]

[0055] 0 1 <8, R+R 1 = 8.

[0056] Example 2:

[0057] The preparation method of cage type [1,1-dimethyl,1-(4'-benzocyclobutenyl)silylethyl]vinylsilsesquioxane (abbreviated as BCB-POSS), the steps are: dry Add 6.33g cage octaethylene silsesquioxane (OVPOSS) to the anaerobic bottle equipped with a magnetic stirrer. Blow nitrogen for 10 minutes to remove the oxygen in the system. Add [4-(1,1- (Dimethyl-1-hydrogen))silylbenzocyclobutene (4-DMHSBCB for short) 16.2g, (catalyst) H with a molar concentration of 0.025M 2 PtCl 6 100 μL of the tetrahydrofuran solution and 50 mL of toluene, the mixture was reacted at 80° C. for 72 hours under a nitrogen atmosphere, and thin-layer chromatography monitored whether the reaction of the reaction raw material OVPOSS was complete. After the reaction, cool the reacted material to room temperature, add ethanol 5 times the mass of the reacted material, precipitate, and filter; add 5 times the mass of the reacted material to the solid obtained after filtration, precipitate and filter; Then add ethanol 5 times the mass of the reacted material to the solid obtained after the reaction, precipitate, and filter; the solid obtained after filtration (ie, the precipitate) is placed in a vacuum drying oven at a pressure of -0.09~-0.095MPa and a temperature of 80 After drying for 20 hours at ℃, a paste product is obtained, namely the prepared cage-type [1,1-dimethyl,1-(4'-benzocyclobutenyl)silylethyl]vinylsilsesquioxane ( Referred to as BCB-POSS), the yield is 85%.

[0058] The structure is characterized as follows: infrared spectrum IR (KBr coating film, cm-1): 3058, 3019, 2962, 2227, 1595, 1462, 1400, 1295, 1253, 1092, 1021, 881, 799.4, 633; 1 H NMR(600MHz, CDCl 3 )δ:0.33-0.41(6H,-SiCH 3 ),0.69-1.11(4H,-SiCH 2 -), 3.27(4H, -CH 2 -),5.7-6.1(n,-SiC 2 H 5 ), 7.12-7.45 (3H, -ArH).

[0059] Example 3:

[0060] The preparation method of cage type [1,1-dimethyl,1-(4'-benzocyclobutenyl)silylethyl]vinylsilsesquioxane (abbreviated as BCB-POSS), the steps are: dry Add 6.33g cage octaethylene silsesquioxane (OVPOSS for short) into an anaerobic bottle equipped with a magnetic stirrer. Blow nitrogen for 30 minutes to remove oxygen in the system. Add [4-(1,1- (Dimethyl-1-hydrogen)]silyl benzocyclobutene (4-DMHSBCB for short) 24.3g, (catalyst) H with a molar concentration of 0.025M 2 PtCl 6 200 μL of the tetrahydrofuran solution and 60 mL of toluene, the mixture was reacted at 85° C. for 60 hours under a nitrogen atmosphere, and the reaction material OVPOSS was monitored by thin layer chromatography to see if the reaction was complete. After the reaction, cool the reacted material to room temperature, add ethanol of 10 times the mass of the reacted material, precipitate, and filter; add ethanol to the solid obtained after filtration with 10 times the mass of the reacted material, precipitate and filter; Then add ethanol 10 times the mass of the reacted material to the solid obtained after the reaction, precipitate and filter; the solid obtained after filtration (ie, the precipitate) is placed in a vacuum drying oven at a pressure of -0.09~-0.095MPa and a temperature of 90 After drying for 12 hours at ℃, a paste product is obtained, namely the prepared cage-type [1,1-dimethyl,1-(4'-benzocyclobutenyl)silylethyl]vinylsilsesquioxane ( Referred to as BCB-POSS), the yield is 88%.

[0061] The structure is characterized as follows: infrared spectrum IR (KBr coating film, cm-1): 3058, 3019, 2962, 2227, 1595, 1462, 1400, 1295, 1253, 1092, 1021, 881, 799.4, 633; 1 H NMR(600MHz, CDCl 3 )δ:0.33-0.41(6H,-SiCH 3 ),0.69-1.11(4H,-SiCH 2 -), 3.27(4H, -CH 2 -),5.7-6.1(n,-SiC 2 H 5 ), 7.12-7.45 (3H, -ArH).