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Modified thermosetting resin and preparation method thereof

A thermosetting resin and thermosetting technology, which is applied in the field of thermosetting resins, can solve the problems that the resin matrix cannot be prevented from entering the mesoporous silica channels, the incomplete closed-pore mesoporous silica is not easy to apply, and the selection of raw materials is narrow. The effect of electrical constant, high specific surface area, and wide applicability

Inactive Publication Date: 2012-08-08
SUZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the above-mentioned incompletely closed-pore mesoporous silica is not easy to apply, and there are mainly the following two problems: (1) Since this incompletely closed-pore mesoporous silica is oxidized by the active groups of some materials and the original mesoporous It is formed by the chemical action of the silanol at the opening of the silicon hole, so the size of the material used for "closed cells" determines the degree of closed cells of mesoporous silica; if the size of the material used for "closed cells" is small, it does not Completely closed mesoporous silica cannot prevent the resin matrix from entering the pores of mesoporous silica; this means that the size of the material used for "closed pores" must increase as the pore size of mesoporous silica increases, and the range of raw material selection is narrow
[0005] To sum up, it can be seen that the use of inorganic materials with pore structure to modify thermosetting resins has significant advantages, but the desired results have not yet been achieved.

Method used

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  • Modified thermosetting resin and preparation method thereof
  • Modified thermosetting resin and preparation method thereof
  • Modified thermosetting resin and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] 1. Preparation of closed-pore mesoporous silica

[0028] 1 g of mesoporous silica SBA-15 was kept at 110° C. for 2 hours to obtain dry mesoporous silica SBA-15. Add 22.7 g of anhydrous toluene to dry SBA-15, stir, and slowly add 2.15 g of dimethyldichlorosilane dropwise at 40°C. After completion of the dropwise addition, the reaction was carried out at 40° C. for 6 hours. Vacuum removal of anhydrous toluene and unreacted polychlorosilane gave a white powder, which was washed 3 times with anhydrous toluene to obtain a crude product. The crude product was dried at 55° C. for 7 hours to obtain mesoporous silica containing chlorine groups on the surface. Its infrared spectrum and scanning electron microscope (SEM) are shown in the attached figure 1 and 2 shown.

[0029] Add 1g of mesoporous silica containing chlorine groups on the surface to 68.4g of anhydrous acetone to form solution A; add 1g of octa(tetramethylammonium) silicate to 24.9g of anhydrous methanol to for...

Embodiment 2

[0036] 1. Preparation of closed-pore mesoporous silica

[0037] Closed-pore mesoporous silica was prepared according to the method of Example 1.

[0038] 2. Preparation of modified bismaleimide resin

[0039] 10g of N,N'-4,4'-diphenylmethane bismaleimide (BDM), 8.5g of diallyl bisphenol A (DBA) and 0.37g of the polyhedral sesquite prepared in Example 2 Siloxane closed-pore mesoporous silica SBA-15, stirred evenly at 140°C to obtain modified bismaleimide resin.

[0040] Vacuumize the obtained modified bismaleimide resin at 140°C for 0.5 hours, and then follow the processes of 150°C / 2h+180°C / 2h+200°C / 2h+220°C / 2h and 230°C / 4h for curing and post-processing. After natural cooling, the cured modified bismaleimide resin was obtained, which was recorded as BDM / DBA / 2pSBA-15. Its dielectric constant-frequency curve is shown in the attached Figure 4 Curve b in (BDM / DBA / 2pSBA-15).

Embodiment 3

[0052] 1. Preparation of closed-pore mesoporous silica

[0053] 1 g of mesoporous silica SBA-15 was kept at 110° C. for 2 hours to obtain dry SBA-15. Add 20 g of anhydrous toluene to dry SBA-15, stir, and slowly add 2 g of dimethyldichlorosilane dropwise at 40°C. After completion of the dropwise addition, the reaction was carried out at 40° C. for 6 hours. Vacuum removal of anhydrous toluene and unreacted polychlorosilane to obtain a white powder, which was washed twice with anhydrous toluene to obtain a crude product. The crude product was dried at 55° C. for 7 hours to obtain mesoporous silica containing chlorine groups on the surface.

[0054] Add 1g of mesoporous silica containing chlorine groups on the surface to 30g of anhydrous acetone to form solution A; add 1g of octamer(tetramethylammonium) silicate to 20g of anhydrous methanol to form solution B. Solutions A and B were mixed, and the mixture was sonicated at 40 °C for 20 min to form solution C. Solution D was fo...

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Abstract

The invention discloses a modified thermosetting resin and a preparation method thereof. 100 parts of heat curable resin and 0.1-100 parts of closed pore meso pore silicon oxide are uniformly mixed at the temperature of 30-180DEG C, and a modification thermosetting resin is obtained. The closed-pore mesoporous is prepared through the steps that: polyhedral silsesquioxane forms a coating on an external surface and apertures of meso pore silicon oxide, the closed-pore mesoporous silicon oxide is connected by Si-O key or Si-N key. The closed pore meso pore silicon oxide has a higher specific surface area comparing to the original closed-pore mesoporous silicon oxide, and simultaneously possesses more interfaces, which can avoid that the resin enters interfaces of inorganic materials, guaranteeing the modification thermosetting resin possesses a low dielectric property, and a stable performance. The preparation method for modified thermosetting resin disclosed in the invention has the characteristics of extensive applicability and simple operation.

Description

technical field [0001] The invention relates to a modified thermosetting resin and a preparation method thereof. It specifically relates to a thermosetting resin modified by closed-pore mesoporous silicon oxide. Background technique [0002] In recent years, with the rapid development of the electronic information industry, low dielectric constant materials have attracted widespread attention. Currently, an efficient way to prepare such materials is to introduce voids into the polymer, since air has a dielectric constant of only 1, thereby lowering the polymer's dielectric constant. For example, Gufan Zhao et al. achieved a dielectric constant of 1.9 by introducing voids into polyimide (see literature: Gufan Zhao, Takayuki Ishizaka,, Hitoshi Kasai, Masatoshi Hasegawa, Takeo Furukawa, Hachiro Nakanishi, and Hidetoshi Oikawa. Chemistry of Materials. 2009, 21, 419-424). However, this method of introducing voids often results in voids on the surface of the prepared material, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08L79/04C08L63/00C08K9/10C08K7/00C08K3/36
Inventor 梁国正单伟顾嫒娟袁莉
Owner SUZHOU UNIV
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