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Bisphenol benzoxazine modified silicon-contained aryne resin and preparation method thereof

A technology of benzoxazine and silicon aryne, which is applied in the field of modified silicon-containing aryne resin and its preparation, can solve problems such as high brittleness, poor mechanical properties of composite materials, and unsatisfactory fiber adhesion, and achieve processing Good performance, low production cost, excellent physical and mechanical properties and high temperature resistance

Active Publication Date: 2012-08-29
EAST CHINA UNIV OF SCI & TECH
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

For example, Korshak et al. used disodium-substituted p-diethynylbenzene and alkyl silicon halides to prepare silicon-containing alkyne resins through polycondensation (V. V. Korshak, A. M. Sladkov, and L. K. Luneva. Izv. Akad. Nauk SSSR, Otd. Khim . Nauk, 1962, 728.); Itoh et al. used the dehydrocoupling method and the Grignard reagent method to synthesize the silicon-containing aryne resin——MSP resin ((a). M. Itoh, M. Mitsuzuka, et al ., Macromolecules, 1994, 27: 7917~7919. (b). M. Itoh, K. Inoue, et al., Macromolecules, 1997, 30 (4): 694.), has excellent thermal properties after curing, but Due to the brittleness of the material and the shrinkage during curing, the mechanical properties of the composite are poor; Buvat et al. synthesized a phenylacetylene-terminated silicon-containing aryne resin (BLJ resin) (Buvat P, Jousse F, Delnaud L, et al . International SAMPE Symposium and Exhibition, 2000, 46: 134~144.); Huang Farong et al. also prepared silicon-containing aryne resins with various structures ((a). Wang F, Zhang J, et al. Polymer Bulletin, 2006, 56: 19-26. (b). J. Zhang, J. Huang, et al. Express Polymer Letters, 2007, 1(12): 831~836. (c) CN1709928.)
[0004] To sum up, although the existing silicon-containing aryne resins have their own characteristics, their brittleness after curing is relatively high, and the adhesion to fibers is not ideal

Method used

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  • Bisphenol benzoxazine modified silicon-contained aryne resin and preparation method thereof
  • Bisphenol benzoxazine modified silicon-contained aryne resin and preparation method thereof
  • Bisphenol benzoxazine modified silicon-contained aryne resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Example 1: Bisphenol A benzoxazine modified silicon-containing aryne resin (BA-a / PSA-30) and its preparation.

[0044] 1. Synthesis of bisphenol A benzoxazine (BA-a), whose structural formula is as follows Figure 7 shown.

[0045] Add 45.6 g (0.2 mol) of stoichiometric bisphenol A, 24.0 g (0.8 mol) of paraformaldehyde and 37.2 g (0.4 mol) of aniline into a 250 mL three-necked flask equipped with a stirring device, a nitrogen pouring tube and a condenser . Heat to 100°C under stirring, react for 20 min, after the reaction, dissolve the product in toluene (chloroform or ether), wash with 3 mol / L sodium hydroxide solution three times, then wash with deionized water until neutral, separate The organic layer was dried by adding anhydrous sodium sulfate, and finally the solvent was distilled off to obtain a light yellow solid with a yield of 70-75%. FTIR characteristic peak: 1496 cm -1 (1,2,4-trisubstituted benzene ring skeleton), 1228 cm -1 (C-O-C), 1162 cm -1 (C-N-C)...

Embodiment 2

[0051] Example 2: Hexafluorobisphenol A benzoxazine modified silicon-containing aryne resin (BAF-a / PSA-30) and its preparation.

[0052] 1. Synthesis of hexafluorobisphenol A benzoxazine (BAF-a), whose structural formula is as follows Figure 8 shown.

[0053] Into a 250 mL three-neck flask equipped with a stirring device, a nitrogen pouring tube and a condenser tube, 67.2 g (0.2 mol) of hexafluorobisphenol A, 24.0 g (0.8 mol) of paraformaldehyde and 37.2 g (0.4 mol). Heat to 100°C under stirring, react for 20 min, after the reaction, dissolve the product in toluene (chloroform or ether), wash with 3 mol / L sodium hydroxide solution three times, then wash with deionized water until neutral, separate The organic layer was dried by adding anhydrous sodium sulfate, and finally the solvent was distilled off to obtain a yellow solid with a yield of 70-75%. FTIR characteristic peak: 1500 cm -1 (1,2,4-trisubstituted benzene ring skeleton), 1244 cm -1 (C-O-C), 1129 cm -1 (C-N-C),...

Embodiment 3

[0057] Example 3: Diphenyl ether type benzoxazine modified silicon-containing aryne resin (BO-a / PSA-30) and its preparation.

[0058] 1. Synthesis of diphenyl ether-type benzoxazine (BO-a), whose structural formula is as follows Figure 9 shown.

[0059] Into a 250 mL three-neck flask equipped with a stirring device, a nitrogen pouring tube and a condenser, add stoichiometric 40.4 g (0.2 mol) of 4,4'-dihydroxydiphenyl ether, 24.0 g (0.8 mol) of paraformaldehyde and Aniline 37.2 g (0.4 mol). Heat to 100°C under stirring, react for 20 min, after the reaction, dissolve the product in toluene (chloroform or ether), wash with 3 mol / L sodium hydroxide solution three times, then wash with deionized water until neutral, separate The organic layer was dried by adding anhydrous sodium sulfate, and finally the solvent was distilled off to obtain a reddish-brown solid with a yield of 70-75%. FTIR characteristic peak: 1489 cm -1 (1,2,4-trisubstituted benzene ring skeleton), 1220 cm -1...

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Abstract

The invention discloses bisphenol benzoxazine modified silicon-contained aryne resin and a preparation method thereof. The preparation method comprises the following step: 50 to 95 percent (by mass) of silicon-contained aryne resin and 5 to 50 percent (by mass) of bisphenol benzoxazine resin are put into a reactor and stirred for 10 to 60 minutes at 100 to 120 DEG C to prepare the bisphenol benzoxazine modified silicon-contained aryne resin. The resin can synchronously form cured resin with a simultaneous interpenetrating network (SIN) structure through thermal polymerization. The bisphenol benzoxazine modified silicon-contained aryne resin prepared by the preparation method is high-performance resin with excellent high-temperature resistance and mechanical property and favorable adhesive property with fiber, and can be widely applied to the fields of spaceflight, aviation, electronics and the like.

Description

technical field [0001] The invention relates to a modified silicon-containing aryne resin and a preparation method thereof, in particular to a bisphenol-type benzoxazine-modified silicon-containing aryne resin and a preparation method thereof. Background technique [0002] Silicon-containing aryne resin is a new type of heat-resistant resin developed and used in recent years. No solvent is used in the molding process, and no small molecules escape during the curing process. It can be molded at normal or low pressure, and has excellent electrical properties and High-temperature ceramic performance (that is, a stable ceramic structure can be formed in this type of polymer at high temperature, such as SiC or / and SiO 2 wait). [0003] So far, silicon-containing aryne resins with various structures have been reported. For example, Korshak et al. used disodium-substituted p-diethynylbenzene and alkyl silicon halides to prepare silicon-containing alkyne resins through polycondens...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G61/12
Inventor 黄发荣杜磊周燕高宇郦骏飞
Owner EAST CHINA UNIV OF SCI & TECH
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