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Oxazine and alkyne compound modified silicon-containing aryne resin and preparing method thereof

A silicon aryne and compound technology, which is applied in the field of modified silicon-containing aryne resin, modified silicon-containing aryne resin and its preparation, can solve the problems of unsatisfactory fiber adhesion, low high temperature resistance, and high resin viscosity. , to achieve excellent mechanical properties and heat resistance, low viscosity of molten resin, and low softening point

Inactive Publication Date: 2012-07-11
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In summary, although the existing silicon-containing aryne resins have excellent characteristics, the brittleness of the resin is still relatively large after curing, and the bonding with the fiber sex is not ideal
Huang Farong and others modified silicon-containing aryne resins with arylethynyl benzoxazine compounds, and obtained a modified silicon-containing aryne resin with good high temperature resistance and mechanical properties (Chinese patent ZL 200710044519.X) , however, the high viscosity of the resin is not conducive to processing
Therefore, the silicon-containing aryne resin was modified with propargyl ether compounds to obtain a modified silicon-containing aryne resin with good process and mechanical properties (Chinese patent ZL 200910047842.1), but its high temperature resistance is lower than that of Silicon-containing aryne resin modified by arylethynyl benzoxazine compounds

Method used

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  • Oxazine and alkyne compound modified silicon-containing aryne resin and preparing method thereof
  • Oxazine and alkyne compound modified silicon-containing aryne resin and preparing method thereof
  • Oxazine and alkyne compound modified silicon-containing aryne resin and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] The preparation of bisphenol A ethynyl benzoxazine and bisphenol A dipropargyl ether modified dimethyl type silicon-containing aryne resin (BAP-DABPA-PSAM-20) comprises the following steps:

[0058] (1) Preparation of dimethyl-type silicon-containing aryne resin (PSAM)

[0059] Add 6.00g (0.25 mol) of treated magnesium powder and 50mL of tetrahydrofuran (THF) into a 250mL four-neck flask equipped with a stirring, constant pressure funnel and spherical condenser, and then slowly add ethyl bromide dropwise through the constant pressure funnel. A mixed solution of 21.60 g (0.20 mol) of alkane and 50 mL of THF; the dropwise addition was completed within 1.5 hours, and then refluxed for 1.5 hours to obtain a gray-black ethyl Grignard reagent;

[0060] A mixed solution of 11.35 g (0.09 mol) of diethynylbenzene and 50 mL of THF was added dropwise under cooling in an ice-water bath, the reaction mixture gradually changed from gray-black to gray-white, and the dropwise addition ...

Embodiment 2

[0077] The preparation of bisphenol A ethynyl benzoxazine and bisphenol A dipropargyl ether modified dimethyl type silicon-containing aryne resin (BAP-DABPA-PSAM-25) comprises the following steps:

[0078] Steps (1), (2), and (3) are the same as in Example 1.

[0079] (4) Preparation of bisphenol A ethynyl benzoxazine and bisphenol A dipropargyl ether modified dimethyl silicon-containing aryne resin (BAP-DABPA-PSAM-25)

[0080] Add 2.0g (10 parts by weight) of BAP, 3.0g (15 parts by weight) of DABPA, and 15.0g (75 parts by weight) of PSAM into a reactor equipped with a stirrer, a thermometer and a reflux condenser, and pass an inert gas, Slowly raise the temperature to 120°C, start stirring, and continue stirring for 3.0 hours after the reactants are melted and homogeneous, and a reddish-brown viscous resin is obtained.

[0081] The reddish-brown viscous resin has a resin viscosity of less than 0.4 Pa·s in the range of 120-200° C., and at a temperature higher than 200° C., th...

Embodiment 3

[0084]The preparation of bisphenol A ethynyl benzoxazine and bisphenol A dipropargyl ether modified dimethyl silicon-containing aryne resin (BAP-DABPA-PSAM-50) comprises the following steps:

[0085] Steps (1), (2), and (3) are the same as in Example 1.

[0086] (4) Preparation of bisphenol A ethynyl benzoxazine and bisphenol A dipropargyl ether modified dimethyl silicon-containing aryne resin (BAP-DABPA-PSAM-50)

[0087] Add 5.0g (25 parts by weight) of BAP, 5.0g (25 parts by weight) of DABPA, and 10.0g (50 parts by weight) of PSAM into a reactor with a stirrer, a thermometer and a reflux condenser, and pass an inert gas, Slowly raise the temperature to 140°C, start stirring, and continue stirring for 4.0 hours after the reactants are melted and homogeneous, and a reddish-brown viscous resin is obtained.

[0088] The reddish-brown viscous resin has a resin viscosity of less than 0.4 Pa·s in the range of 120-210° C., and at a temperature higher than 210° C., the resin viscosi...

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Abstract

The invention relates to modified silicon-containing aryne resin. A preparing method of the modified silicon-containing aryne resin includes the following steps: (1) preparing silicon-containing aryne polymer, (2) preparing benzoxazine compound, (3) preparing propargyl ether compound, and (4) preparing the modified silicon-containing aryne resin, mixing 50-90 parts by weight of the silicon-containing aryne polymer obtained through the step (1), 5-25 parts by weight of the benzoxazine compound obtained through the step (2) and 5-25 parts by weight of the propargyl ether compound obtained through the step (3), and leading the mixture to be stirred for reacting in a reactor comprising a stirrer, a thermometer and a reflux condensing pipe with inert gases to obtain the modified silicon-containing aryne resin. The oxazine and alkyne compound modified silicon-containing aryne resin and the preparing method of the modified silicon-containing aryne resin have the advantages that the modified silicon-containing aryne resin can be dissolved in many common solvents, is low in softening point and melting resin viscosity, and can generate solidifying reaction under heat, irradiation and even light effect. Resin condensates are good in heat resistance and can be well bonded with reinforcing fiber, and compound materials of the modified silicon-containing aryne resin have good mechanical performance and heat resistance.

Description

technical field [0001] The invention relates to a modified silicon-containing aryne resin and a preparation method thereof in the technical field of chemistry and chemical engineering, in particular to a silicon-containing aryne polymer, a benzoxazine compound and a propargyl ether compound Copolymerized modified silicon-containing aryne resin. Background technique [0002] Silicon-containing aryne resin is a new type of polyacetylene resin, which has a highly cross-linked structure after curing. It not only has excellent heat resistance and ablation resistance, but also has excellent processability, mechanical properties and high-temperature ceramicization. performance etc. [0003] The report of the silicon-containing aryne resin of existing multiple structure so far, as: the people such as Luneva utilizes acetylene Grignard reagent and alkyl, the reaction of aryl silicon halide to prepare silicon-containing acetylenic resin (L.K.Luneva, A.M.Sladkov, and V.V. Korshak, Vy...

Claims

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Application Information

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IPC IPC(8): C08G61/12
Inventor 黄发荣杜磊周燕邓诗峰汤乐旻田鑫
Owner EAST CHINA UNIV OF SCI & TECH
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