CN1255426A - Polyarylether mitrilesulfone fibre cloth reinforced compound material and its making method - Google Patents
Polyarylether mitrilesulfone fibre cloth reinforced compound material and its making method Download PDFInfo
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- CN1255426A CN1255426A CN 98121878 CN98121878A CN1255426A CN 1255426 A CN1255426 A CN 1255426A CN 98121878 CN98121878 CN 98121878 CN 98121878 A CN98121878 A CN 98121878A CN 1255426 A CN1255426 A CN 1255426A
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Abstract
A polyarylether nitrilesulfone fibre cloth reinforced compound material is prepared through dipping the reinforcing material in resin solution twice to obtain the pre-dipped material with high resin content, and hot pressing at temp higher than softening point of basic resin. Said basic resin is polyarylether nitrile sulfone or polyarylether sulfone. sed solvent is strong polar non-protonic solvent. Used precipitant is the solvent in which polyarylether nitrilesulfone or polyarylether sulfone can not be dissolved. Said reinforcing fibre cloth is carbon fibre cloth and non-alkali glass fibre cloth. Said compound material has higher mechanical strength and high-temp. resistance.
Description
The present invention relates to a kind of polyarylether mitrilesulfone fibre cloth reinforced compound material and manufacture method thereof, belong to the reinforced composite field of special engineering plastics.
Polyaryl ether-nitrile-sulfone and polyether sulphone are the aromatic ring polymer with special molecular structure, they contain the oxygen-ether linkage of rigidity, stable on heating phenylene, sulfuryl and hear resistance, flexibility on molecular backbone, wherein polyaryl ether-nitrile-sulfone also contains the itrile group side group of strong polarity.Be a class set high heat distortion temperature, high impact and good processing and forming special engineering plastics.Long-term serviceability temperature is 180 ℃, and its combination property and polytetrafluoroethylene (PTFE) and polyimides are approaching, and processing characteristics is than the latter much better [plastics industry, 1989, (5), 23].Thermoplastic special engineering plastics is made the fiber cloth reinforced composite, and one of conventional method is the powdered resin material to be sprinkling upon carry out lamination on the fiber cloth, and this method is unfavorable for large-scale production obviously.Two of conventional method is to adopt cement-dipping method, is about to the fiber cloth impregnating resin solution, impregnation, oven dry again after the dry out solvent then, and repeated multiple times like this had not only been wasted solvent but also contaminated environment, also was difficult to obtain the fiber cloth prepreg of satisfied high resin content simultaneously.
A kind of polyarylether mitrilesulfone fibre cloth reinforced compound material and the manufacture method thereof that provide at the deficiencies in the prior art is provided, be characterized in polyaryl ether-nitrile-sulfone or polyether sulphone be dissolved in and make resin solution in the solvent, adopt dipping precipitating technology to make prepreg again, be about to resin solution impregnation of carbon fibers cloth or glass fabric, taking out the back immerses in the precipitating agent, obtain the fiber cloth prepreg through curing, and then with the superimposed compression moulding of prepreg, thereby the carbon cloth or the glass fabric reinforced composite materials of acquisition polyaryl ether-nitrile-sulfone or polyether sulphone.Simultaneously waste product or tailing with dissolution with solvents after, resin can be reclaimed usefulness again, thereby make this composite and do not waste matrix resin.
Purpose of the present invention is realized that by following technical measures wherein said initiation material umber is parts by weight.
The initiation material formula constituent of polyarylether mitrilesulfone fibre cloth reinforced compound material is:
25～75 parts of polyaryl ether-nitrile-sulfones (or polyether sulphone)
25～75 parts of carbon cloths (or glass fabric)
80～800 parts of solvents (N-dimethylacetylamide, dimethyl sulfoxide (DMSO) and/or N-N-methyl-2-2-pyrrolidone N-are at least a for available N, dinethylformamide, N)
2000～5000 parts of precipitating agent (available methyl alcohol, ethanol, acetone, toluene, benzene and/or water are at least a)
The manufacture method of polyaryl ether-nitrile-sulfone (or polyether sulphone) fiber cloth reinforced composite:
(1) preparation of resin solution
Polyaryl ether-nitrile-sulfone in the above-mentioned prescription (or polyether sulphone) is added in the dissolution equipment, add the solvent of formula ratio, start stirring, be warming up to 100～200 ℃ of dissolvings 0.5～1 hour, be cooled to below 50 ℃, filter with filter cloth and obtain uniform resin solution.
(2) the dipping precipitation method prepares prepreg
Flooded above-mentioned resin solution 5～10 minutes with carbon fiber or glass fabric, taking out the back immersed in the precipitating agent 5 minutes, resin gets final product precipitating on fiber cloth, it is cured 10 minutes in 160～200 ℃ baking oven after, take out and press the preceding method impregnating resin solution again, immerse then in the precipitating agent, the last processing under 160～200 ℃ temperature obtained prepreg in 15 minutes.
(3) preparation of reinforced composite
Above-mentioned polyaryl ether-nitrile-sulfone (or polyether sulphone) fiber cloth prepreg is superimposed between template, then template is put into 300～340 ℃ pressure forming machine, after executing contact pressure and keeping 30 minutes, looking the gummosis situation progressively exerts pressure, final pressure is 6.9MPa, behind the pressure-maintaining and heat-preservation 30 minutes, pressurize is cooled to room temperature, and release is taken out the carbon cloth or the glass fabric that obtain polyaryl ether-nitrile-sulfone (or polyether sulphone) and strengthened laminar composite.
The polyaryl ether-nitrile-sulfone that the present invention makes (or polyether sulphone) carbon cloth or glass fabric composite outward appearance are respectively black and light grey glossiness laminate.Resin content can be regulated as required.Resin in waste product and the tailing has reproducibility.Laminate has higher mechanical strength.The polyaryl ether-nitrile-sulfone that carbon cloth strengthens, the bending strength of polyether sulphone laminate are respectively 626.0MPa (resin content is 41.2%) and 535.3MPa (resin content is 44.1%), the polyaryl ether-nitrile-sulfone that glass fabric strengthens, the bending strength of polyether sulphone laminate are respectively 293.9MPa (resin content is 54.0%) and 273.9MPa (resin content is 38.5%), such composite can be used for aerospace field, or is used as insulating materials etc.
The present invention has following advantage:
1. in the process of making polyaryl ether-nitrile-sulfone (or polyether sulphone) fiber cloth reinforced composite, adopt dipping precipitating technology, can meet the requirements of resin content after making prepreg through twice impregnation.
2. in the manufacture process of such composite, the recyclable usefulness again of solvent and precipitating agent, free from environmental pollution.
3. the tailing that is produced in such composite material manufacturing process, recyclable resin such as waste product is used again.
4. such compound enforcement easy to manufacture is easy to promote, and long-term serviceability temperature is 180 ℃, can be used for aerospace field or is used as electrically insulating material.Have remarkable economic efficiency and social benefit.
Embodiment
Below by embodiment the present invention is specifically described; be necessary to be pointed out that at this following examples only are used for further specifying of the present invention; can not be interpreted as limiting the scope of the invention, these those skilled in the art can make some nonessential improvement and adjustment to the present invention according to foregoing.This technology is applicable to the preparation of the fiber cloth reinforced composite of the thermoplastic engineering plastic with solubility simultaneously.
1. with 50 gram polyaryl ether-nitrile-sulfones (Sichuan Union University development), 200ml N, dinethylformamide adds in the 500ml there-necked flask of belt stirrer, condenser, thermometer, stirring is started in heating, is warming up to 100～150 ℃ of dissolvings 0.5～1 hour, be cooled to below 50 ℃, filter with filter cloth, obtain solids content and be about 18% resin solution, viscosity is (to be coated with 4 in 43.1 seconds
#Cup, 28 ℃).With the thick alkali-free glass cloth of handling through KH-550 of 20 15 * 15cm 0.1mm of resin solution dipping 5～10 minutes, taking out glass cloth behind the impregnation immersed in the ethanol 5 minutes, resin is that precipitating is on glass cloth, it was cured in 160 ℃ baking oven 10 minutes, take out and press the preceding method impregnating resin solution, and then immerse in the precipitating agent, the last processing in 160 ℃ baking oven obtained prepreg in 15 minutes, the resin content of prepreg is 48.27% behind twice impregnation, volatile content is 0.04% (160 ℃, 2 hours).The polyaryl ether-nitrile-sulfone glass fabric prepreg that is obtained is superimposed between template, then template is put into 300～340 ℃ pressure forming machine, after executing contact pressure and keeping 30 minutes, look the gummosis situation and progressively exert pressure, final pressure is 6.9MPa, and pressure-maintaining and heat-preservation is after 30 minutes, pressurize is cooled to room temperature, release is taken out, and obtains the polyaryl ether-nitrile-sulfone glass fabric and strengthens laminar composite, and its normality bending strength is 293.9MPa.
2. with 50 gram polyaryl ether-nitrile-sulfones, 200ml N, dinethylformamide add in the equipment identical with embodiment 1, with identical method, make resin solution under identical condition, and viscosity is (to be coated with 4 in 44.7 seconds
#Cup, 27 ℃), 10 15 * 15cm 0.24mm are thick with the resin solution dipping, and face content is 195g/m
2T-300 carbon cloth after 5～10 minutes, take out to immerse in the water 5 minutes, resin is that precipitating is on carbon cloth, it was cured in 160 ℃ baking oven 10 minutes, take out and press the preceding method impregnating resin solution, immerse then in the water, the last processing in 160 ℃ baking oven obtained polyaryl ether-nitrile-sulfone carbon cloth prepreg in 15 minutes.The resin content of prepreg is 45.40% behind twice dipping, volatile content is 0.04% (160 ℃, 2 hours), the prepreg of gained through method in identical condition under the compression moulding identical with embodiment 1, is obtained the polyaryl ether-nitrile-sulfone carbon cloth and strengthens laminar composite.Its normality bending strength is 626.0MPa.
3. with 45 gram polyether sulphones (Jilin University's productions), 200ml N in the identical equipment of dinethylformamide adding and embodiment 1, makes resin solution with identical method under identical condition, and viscosity is (to be coated with 4 in 47.9 seconds
#Cup, 28 ℃), be the precipitating agent then with methyl alcohol and adopt the method identical to make the glass fabric prepreg with embodiment 1, the resin content of prepreg is 46.80%, volatile content is 0.04% (160 ℃, 2 hours).The polyether sulphone glass fabric prepreg that obtained through the method compression moulding identical with embodiment 1, is obtained the polyether sulphone glass fabric and strengthens laminar composite, and its normality bending strength is 273.9MPa.
4. with 45 gram polyether sulphones, 200ml N, dinethylformamide adds in the equipment identical with embodiment 1, makes resin solution with identical method under identical condition, and viscosity is (to be coated with 4 in 46.3 seconds
#Cup, 28 ℃).Be the precipitating agent then with water and adopt the method identical to make the carbon cloth prepreg with embodiment 2, the resin content of prepreg is 43.9%, volatile content is 0.04% (160 ℃, 2 hours), with the polyether sulphone carbon cloth prepreg that obtained through the method identical with embodiment 1 in identical condition compression moulding, obtain the polyether sulphone carbon cloth and strengthen laminar composite, its normality bending strength is 535.3MPa.
Claims (6)
1. polyarylether mitrilesulfone fibre cloth reinforced compound material is characterized in that this composite initiation material formula constituent (by weight) is:
25～75 parts of polyaryl ether-nitrile-sulfones
25～75 parts of carbon cloths
80～800 parts of solvents
2000～5000 parts of precipitating agent
2. according to the described polyaryl ether-nitrile-sulfone fiber reinforcement of claim 1 degree composite, it is characterized in that the used polyaryl ether-nitrile-sulfone of this reinforced composite can replace with polyether sulphone.
3. according to the described polyarylether mitrilesulfone fibre cloth reinforced compound material of claim 1, it is characterized in that the used carbon cloth useable glass fiber cloth of this reinforced composite replaces.
4. according to the described polyarylether mitrilesulfone fibre cloth reinforced compound material of claim 1, it is characterized in that the used solvent of this reinforced composite is N, dinethylformamide, N, the N-dimethylacetylamide, dimethyl sulfoxide (DMSO) and/or N-N-methyl-2-2-pyrrolidone N-are at least a.
5. according to the described polyarylether mitrilesulfone fibre cloth reinforced compound material of claim 1, it is characterized in that the used precipitating agent of this reinforced composite is that methyl alcohol, ethanol, acetone, toluene, benzene and/or water are at least a.
6. according to the manufacture method of the described polyarylether mitrilesulfone fibre cloth reinforced compound material of claim 1, it is characterized in that:
(1) preparation of resin solution
Polyaryl ether-nitrile-sulfone in the above-mentioned prescription or polyether sulphone are added in the dissolution equipment, add the solvent of formula ratio, start stirring, be warming up to 100～200 ℃ of dissolvings 0.5～1 hour, be cooled to below 50 ℃, filter with filter cloth and obtain uniform resin solution,
(2) the dipping precipitation method prepares prepreg
Flooded above-mentioned resin solution 5～10 minutes with carbon cloth or glass fabric, taking out the back immersed in the precipitating agent 5 minutes, the resin precipitating is on fiber cloth, after in 160～200 ℃ baking oven, curing 10 minutes, take out and press the preceding method impregnating resin solution again, immerse then in the precipitating agent, the last processing under 160～200 ℃ temperature obtained prepreg in 15 minutes
(3) preparation of reinforced composite
Above-mentioned polyaryl ether-nitrile-sulfone or polyether sulphone fiber cloth prepreg is superimposed between template, then template is put into the pressure forming machine that hot plate has been warming up to 300～340 ℃, after executing contact pressure and keeping 30 minutes, looking the gummosis situation progressively exerts pressure, final pressure is 6.9MPa, behind the pressure-maintaining and heat-preservation 30 minutes, pressurize is cooled to room temperature, and release is taken out the carbon cloth or the glass fabric that obtain polyaryl ether-nitrile-sulfone or polyether sulphone and strengthened laminar composite.
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| CN 98121878 CN1255426A (en) | 1998-12-01 | 1998-12-01 | Polyarylether mitrilesulfone fibre cloth reinforced compound material and its making method |
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| CN 98121878 CN1255426A (en) | 1998-12-01 | 1998-12-01 | Polyarylether mitrilesulfone fibre cloth reinforced compound material and its making method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913276A (en) * | 2010-07-07 | 2010-12-15 | 电子科技大学 | Poly(arylene ether nitrile) resin and fiber fabric laminated composite material and preparation method thereof |
| CN101712795B (en) * | 2009-11-27 | 2011-09-14 | 四川飞亚新材料有限公司 | Poly-arylene ether nitrile composite material, poly-arylene ether nitrile material and preparation method thereof |
| CN102632535A (en) * | 2012-04-10 | 2012-08-15 | 江南大学 | Preparation method of aldehyde-free artificial board |
| CN106626582A (en) * | 2016-10-08 | 2017-05-10 | 青岛海信电器股份有限公司 | Carbon fiber composite material, preparation method and electronic equipment enclosure |
| CN107901451A (en) * | 2017-11-14 | 2018-04-13 | 电子科技大学 | A kind of technology of preparing of high-temperature resistant resin base copper-clad plate |
| CN111334024A (en) * | 2020-04-17 | 2020-06-26 | 中国科学院长春应用化学研究所 | Continuous carbon fiber reinforced polyaryletherketone composite material prepreg tape and preparation method thereof |
| CN113789054A (en) * | 2021-07-28 | 2021-12-14 | 大连疆宇新材料科技有限公司 | Preparation method of high-temperature-resistant poly (arylene ether nitrile ketone) bismaleimide composite material |
| CN114131785A (en) * | 2021-11-24 | 2022-03-04 | 山东非金属材料研究所 | Preparation method of high-temperature-resistant thermoplastic composite material unidirectional prepreg tape |
-
1998
- 1998-12-01 CN CN 98121878 patent/CN1255426A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101712795B (en) * | 2009-11-27 | 2011-09-14 | 四川飞亚新材料有限公司 | Poly-arylene ether nitrile composite material, poly-arylene ether nitrile material and preparation method thereof |
| CN101913276A (en) * | 2010-07-07 | 2010-12-15 | 电子科技大学 | Poly(arylene ether nitrile) resin and fiber fabric laminated composite material and preparation method thereof |
| CN102632535A (en) * | 2012-04-10 | 2012-08-15 | 江南大学 | Preparation method of aldehyde-free artificial board |
| CN106626582A (en) * | 2016-10-08 | 2017-05-10 | 青岛海信电器股份有限公司 | Carbon fiber composite material, preparation method and electronic equipment enclosure |
| CN107901451A (en) * | 2017-11-14 | 2018-04-13 | 电子科技大学 | A kind of technology of preparing of high-temperature resistant resin base copper-clad plate |
| CN111334024A (en) * | 2020-04-17 | 2020-06-26 | 中国科学院长春应用化学研究所 | Continuous carbon fiber reinforced polyaryletherketone composite material prepreg tape and preparation method thereof |
| CN113789054A (en) * | 2021-07-28 | 2021-12-14 | 大连疆宇新材料科技有限公司 | Preparation method of high-temperature-resistant poly (arylene ether nitrile ketone) bismaleimide composite material |
| CN113789054B (en) * | 2021-07-28 | 2023-11-07 | 大连疆宇新材料科技有限公司 | Preparation method of high-temperature-resistant polyarylether nitrile ketone bismaleimide composite material |
| CN114131785A (en) * | 2021-11-24 | 2022-03-04 | 山东非金属材料研究所 | Preparation method of high-temperature-resistant thermoplastic composite material unidirectional prepreg tape |
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