JPH0471103B2 - - Google Patents

Description

[Detailed description of the invention]

[Technical Field of the Invention] The present invention relates to a resin composition having excellent heat resistance and mechanical strength. [Technical background of the invention and its problems] Various resins made of polycyanoaryl ether are known (Japanese Unexamined Patent Application Publication No. 1983-1999).
14270 and JP-A-59-206433), it is used in a wide range of applications because it has excellent heat resistance and mechanical strength. However, in recent years, as the scope of use of such resins has further expanded, it is often the case that even higher heat resistance and mechanical strength are required than in the past. Therefore, there is a strong demand for the development of resin materials with even better heat resistance and mechanical strength. [Object of the Invention] In response to such conventional demands, the present invention aims to provide a resin composition containing polycyanoaryl ether as a resin skeleton and having excellent heat resistance and mechanical strength. [Summary of the invention] The resin composition of the present invention has the following formula: The reduced viscosity [ηsp/C] at 60°C of a solvent with a concentration of 0.2 g/dl using p-chlorophenol as a solvent is 0.8 dl/g.
The above crystalline polycyanoaryl ether and the crystalline polycyanoaryl ether have 5 to 5 to
It is characterized by consisting of 60% by weight of fibrous reinforcing material. Further, such crystalline polycyanoaryl ether can be prepared using, for example, p-chlorophenol as a solvent.
In order to improve heat resistance, it is preferable to have a degree of polymerization such that the reduced viscosity [ηsp/c] at 60° C. of a solution with a concentration of 0.2 g/dl is 0.8 dl/g or more. Examples of the fibrous reinforcing material to be added to the crystalline polycyanoaryl ether resin include carbon fibers, lath fibers, alumina fibers, and aromatic polyamide fibers, with carbon fibers and lath fibers being particularly preferred. Further, the carbon fiber may be any of acrylonitrile type, pitch type, and cellulose type. Furthermore, these fibrous reinforcements
Either continuous fibers or discontinuous fibers may be used. For example, it is preferable to use roving, chopped fibers, or milled fibers. The resin composition of the present invention can be obtained by blending the above-mentioned fibrous reinforcing material with the above-mentioned crystalline polycyanoaryl ether. The blending amount of the fibrous reinforcing material is 5 to 60% by weight of the entire resin composition. If the amount of fibrous reinforcing material is less than 5% by weight, sufficient heat resistance and mechanical strength improvement effects cannot be obtained, while if it exceeds 60% by weight, the crystalline polycyanoaryl ether will It has the disadvantage of not being properly distributed in the interstices. Preferably 10-40% by weight
It is. In producing this resin composition, the fibrous reinforcing material may be blended with the crystalline polycyanoaryl ether in the above-mentioned amount and then melt-kneaded. The temperature at this time is 350-410℃, preferably
The temperature is 370 to 400°C, and the kneading time is 1 to 10 minutes, preferably 2 to 5 minutes. [Embodiments of the Invention] Example 1 (1) Production of crystalline polycyanoaryl ether In a separable flask with an internal volume of 5 equipped with a stirring device, a rectification device, and an argon gas blowing tube, 2.
6-dichlorobenzonitrile 344.02g (2.0mol)
and 317.2g of 2,7-dihydroxynaphthalene
(1.98 mol) and 330 g (2.4 mol) of potassium carbonate, as well as sulfolane, 2.5 mol and 1 mol of toluene as solvents, and the reaction was carried out with stirring at 160°C for 2 hours while blowing argon gas and for 2 hours at 200°C. Ta. The water produced during the reaction was constantly distilled off along with the toluene. After the reaction was completed, the product was cooled to room temperature and poured into methanol, the precipitated polymer was collected and pulverized in a Warning blender, and then washed with hot water 2 and water 2, respectively, to produce the following. 515 g (yield: 100%) of crystalline polycyanoaryl ether represented by formula () was obtained. When this polymer was dissolved in p-chlorophenol to a concentration of 0.g/dl, the reduced viscosity [ηsp/c] at 60°C was 0.95 dl/g. In addition, when we investigated the thermal properties of this polymer, we found that the glass transition temperature was 214℃, and the thermal decomposition onset temperature was 214℃.
It was 499℃. Furthermore, this polymer was insoluble in common solvents and had excellent flame retardancy. (2) Production of resin composition To the crystalline polycyanoaryl ether powder obtained in (1) above, carbon fiber (Toray Co., Ltd.: Trading Card), its content is
The mixture was blended to 10% by weight using a Henschel mixer, and then this mixture was
The mixture was kneaded and extruded using a mm extruder at a cylinder temperature of 370 to 400°C to form pellets. Then, using an injection molding machine, the cylinder temperature is 370 to 400.
A test piece was molded from this pellet at a mold temperature of 140°C. After annealing the obtained test piece at 200°C for 2 hours, a tensile test and measurement of heat distortion temperature were performed. In addition, the heat distortion temperature is
The tensile test was carried out using a thermal strain measuring instrument manufactured by Toyo Seiki, while an Autograph IS- manufactured by Shimadzu Corporation was used for the tensile test.
5000 and a tensile speed of 1 mm/min, the breaking strength, breaking elongation, and elastic modulus were measured. The above measurement results are shown in the table. Examples 2 to 3 Test pieces were prepared and tested in the same manner as in Example 1, except that the amounts of the fibrous reinforcing material were 20% by weight and 30% by weight, respectively. The results are shown in the table. Examples 4 to 6 Test pieces were prepared in the same manner as in Example 1, except that glass fibers with an average length of 3 mm (manufactured by Asahi Fiberglass Co., Ltd.) were used instead of carbon fibers as the fibrous reinforcement material. Each test was conducted. Incidentally, the amount of glass fiber blended was 10, 20 and 30% by weight, respectively. The results obtained are shown in the table. Reference Example Test pieces were prepared in the same manner as in Example 1, except that no fibrous reinforcing material was added, and various tests were conducted. The results obtained are shown in the table.

[Table] [Effects of the Invention] As is clear from the above description, the resin composition of the present invention contains a crystalline polycyanoaryl ether resin having a specific structure and an appropriate amount of fibrous reinforcing material. It has much higher heat resistance and mechanical strength than other products, making it suitable for electronic and electrical equipment,
It is extremely useful in fields that require excellent heat resistance and mechanical strength, such as materials for various machines.

Claims (1)

[Claims] Primary formula: The reduced viscosity [ηsp/C] at 60°C of a solvent with a concentration of 0.2 g/dl using p-chlorophenol as a solvent is 0.8 dl/g.
A resin composition comprising the above crystalline polycyanoaryl ether and a fibrous reinforcing material blended with the crystalline polycyanoaryl ether in an amount of 5 to 60% by weight. 2. The resin composition according to claim 1, wherein the fibrous reinforcing material is carbon fiber or glass fiber.