CN1230570A - Short staple-containing composite polyimide material and its preparation and use - Google Patents
Short staple-containing composite polyimide material and its preparation and use Download PDFInfo
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- CN1230570A CN1230570A CN 98101237 CN98101237A CN1230570A CN 1230570 A CN1230570 A CN 1230570A CN 98101237 CN98101237 CN 98101237 CN 98101237 A CN98101237 A CN 98101237A CN 1230570 A CN1230570 A CN 1230570A
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- staple fibre
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Abstract
The composite polyimide material contains short staple 5-60 pts. wt and polyimide resin 40-95 pts. wt., and is prepared by using methanol or ethanol as solvent and through wet mixing, drying, crushing and heating to cure. It may be used as heat resisting, wear resisting, radiation resisting and insulating material in aeronautics, astronautics and civil use.
Description
And its production and use
The present invention relates to a kind of composite polyimide material, particularly design a kind of staple fibre enhanced PMR type polyimide amine matrix material.
1994, people such as R.H.Pater (SAMPE, J1994,30 (5), 29) reported the application of continuous fibre enhanced composite polyimide material in aerospace industry, this material has the specific tenacity height, the specific modulus height, radiation hardness, a series of properties such as high temperature resistant, it is the first-selected kind of aerospace advanced material, but this continuous fibre enhanced material is owing to be subjected to the following restriction of itself performance, and processing characteristics is bad, and it is big to prepare volume with complicated technologies such as autoclaves, structure component simple in structure, limited the range of application of this material greatly, the way that overcomes this shortcoming at present is earlier matrix material to be made bar, then, and through being machined into the component of desired shape, not only waste starting material, improved cost, and after the mechanical workout, the mechanical property of material is damaged.
The objective of the invention is to overcome the shortcoming of the composite polyimide material poor processability of continuous fibre enhanced, obtained the good staple fibre enhanced PMR type composite polyimide material of processing characteristics, but with this material once shaped complex structure, the high temperature resistant component that volume is changeable, improve raw material availability, kept the mechanical property of material.
Staple fibre enhanced PMR type thermosetting polyimide composite material of the present invention comprises following component and content:
The preferable weight part of component weight part
Staple fibre 5-60 15-50
Polyimide resin 40-95 50-85
Staple fibre of the present invention comprises that length exists.0.01-20mm carbon fiber, graphite fibre, glass fibre, the whisker of the various trades mark.
PMR polyimide type resin of the present invention is meant:
R
2：CO
The preparation method of staple fibre enhanced PMR type composite polyimide material of the present invention is characterized in that following these steps to carrying out:
(1) have in the container of stirring, water distilling apparatus and noble gas protection at glass there-necked flask or other,
Put into the 5-60 weight part, the staple fibre of preferred 15-40 weight part adds 40-95 then
Weight part, the ethanol or the first of the PMR polyimide type resin of preferred 60-85 weight part
Alcoholic solution high-speed stirring 10-30 minute, fully floods fiber and resin
(2) under the protection of whipped state and nitrogen or argon gas, with well heater electrically heated, water-bath or oil
Bathe heating means with extremely boiling of mixture heating up, ethanol or methyl alcohol are steamed, make mixing
Ethanol content accounts for the 5-20% of mixture total weight amount in the thing;
(3) said mixture is poured into while hot in big mouthful of container such as watch-glass, furnace pot or the porcelain dish, put into (vacuum) baking oven, dried by the fire 1-4 hour down at 70-120 ℃; (4) temperature is increased to 100-180 ℃, dried by the fire 1-4 hour; (5) temperature is increased to 180-240 ℃, dried by the fire 1-4 hour; (6) prepreg that obtains is crushed to the 60-200 order, obtains the molding powder.(7) (vacuum) vulcanizing press is warming up to 150-300 ℃, in an amount of accurately weighing
Stating the molding powder adds in the metal die; (8) mould is put into that (vacuum 0 vulcanizing press keeps in touch pressure, with 1-10 ℃/minute
The temperature rise rate of clock is raised to 260-310 ℃, is forced into 1-10MPa, with 1-10 ℃ liter
Temperature speed high price mould is warmed up to 300-360 ℃, and heat-insulation pressure keeping solidified after 1-8 hour,
Make mould be cooled to 25-200 ℃ naturally; (9) drip molding is placed in 300-370 ℃ the aging pipe or baking oven, it is little that thermal ageing is handled 2-10
The time, obtain profiled member.
Staple fibre enhanced PMR type heat curing-type composite polyimide material prepreg processing flowability of the present invention is good, its melt flow index [was pressed the GB3682-83 standard test between 1.0-4.0g/ minute, the 5.00kg that wherein loads, mouthful mould internal diameter 1.18mm].Can be with the baroque component of this material once shaped, technology is simple, saves material, and gained component outward appearance is highly polished, and interior porosity is low.
Staple fibre enhanced PMR type heat curing-type composite polyimide material of the present invention has the basic physicals shown in the table 1:
Table 1, staple fibre strengthen the basic physicals of composite polyimide material
| Tensile strength (MPa) | ????23℃ | ????90-150 |
| ????250℃ | ????60-100 | |
| Flexural strength (MPa) | ????23℃ | ????100-200 |
| ????250℃ | ????70-140 | |
| Shock strength (kJ/M 2) | ????10-20 | |
| Heat-drawn wire (℃) | ????250-450 | |
| Relative density | ????1.2-1.7 | |
The application of staple fibre enhanced PMR type composite polyimide material of the present invention is meant the heatproof of aerospace and civil area, wear-resisting, radioprotective, insulating material.
Embodiment provided by the invention is as follows: embodiment 1, be that the T-300 carbon fiber of 5mm adds and to have in the glass there-necked flask of whipping appts and protection of inert gas device and water distilling apparatus with 5 gram mean lengths; adding the 190g solid content is the 50%PMR resin solution; vigorous stirring 20 minutes; use the heating in water bath there-necked flask then; under nitrogen protection, ethanol is steamed, up to put in order out the ethanol volume to about the 75ml till.Mixture in the there-necked flask is poured in the porcelain tray while hot, and the stand lamellar is put into 100 ℃ thermal cycling wind baking oven, dries by the fire 3 hours, and cooling is crushed to 80 orders with material prepreg, obtains the prepreg of fibre content 5%.Embodiment 2, be that the glass fibre of 5mm replaces the T-300 carbon fiber with mean length, other can make short glass fiber enhanced PMR type heat curing-type composite polyimide material prepreg with embodiment 1.Embodiment 3, replace the T-300 carbon fiber with whisker, other can make whisker enhanced PMR type thermosetting polyimide composite material prepreg with embodiment 1.Embodiment 4, carbon fiber weight is become 60g, add the 80g solid content and be 50% PMR resin solution other with embodiment 1, promptly obtain the PMR type thermosetting polyimide composite material prepreg of fibre content 60%.Embodiment 5, carbon fiber weight is become 30g, add the 140g solid content and be 50% PMR type thermoset polyimide resin solution, other promptly obtains the PMR type thermosetting polyimide composite material prepreg of carbon fiber content 30 with embodiment 1.Embodiment 6, take by weighing the material prepreg molding powder that obtains among the 12.0g embodiment 1, put into the metal die of 25mm, vulcanizing press is warming up to 200 ℃, put into mould, executing contact presses, be warmed up to 260 ℃, after the pressurization, die temperature is risen to 320 ℃, and heat-insulation pressure keeping solidifies and stopped heating in 2 hours, keep-ups pressure, make die temperature reduce to 200 ℃ naturally, die sinking, promptly obtaining thickness is 4mm, diameter 25mm, ganoid short carbon fiber enhanced PMR type thermosetting polyimide composite material disk.The tensile strength of this material is 98MPa, and flexural strength is 130MPa, and shock strength is 14KJ/M
2, heat-drawn wire is 380 ℃, relative density is 1.53.
Claims (7)
1. a composite polyimide material that contains staple fibre is characterized in that described matrix material comprises following group
Part and content (weight part):
The component weight part
Staple fibre 5-60
Thermoset polyimide resin 40-95
Described staple fibre is that length is carbon fiber, graphite fibre, glass fibre and/or the whisker of 0.01-20mm.
Described polyimide resin is the following PMR type thermoset polyimide resin of structural formula:
R1:CH2 in the formula
R2：CO
2. a kind of composite polyimide material that contains staple fibre according to claim 1 is characterized in that described multiple
Condensation material comprises following component and content (weight part):
The component weight part
Staple fibre 15-50
Polyimide resin 50-85
3, a kind of composite polyimide material that contains staple fibre according to claim 1 is characterized in that described staple fibre is that length is carbon fiber, graphite fibre, glass fibre and/or the whisker of 0..1-20mm.
4. a kind of preparation method who contains the composite polyimide material of staple fibre according to claim 1 is characterized in that
Step is carried out in the following order:
(1) in the container of protection of inert gas, add 5-60 weight part staple fibre, add the ethanol or the methanol solution of the PMR polyimide type resin of 40-95 weight part again,
(2) solvent in the said mixture is steamed,
(3) 70-120 ℃ of baking 1-4 hour, continuing was warming up to 100-180 ℃ again, dries by the fire 180-240 1-4 hour
℃, dry by the fire after 1-4 hour, through being ground into the molding powder,
(4) at 260-310 ℃, 1-10MPa curing reaction 1-8 hour.
5. a kind of preparation method who contains the composite polyimide material of staple fibre according to claim 3, its spy
Levy and be that described short fibre content is the 15-50 weight part.
6. a kind of preparation method who contains the composite polyimide material of staple fibre according to claim 3, its spy
Levy and be that described staple fibre is carbon fiber, graphite fibre, glass fibre and/or whisker.
7. a kind of purposes that contains the composite polyimide material of staple fibre according to claim 1, its feature exists
Material in the heatproof that is used for aerospace or civilian industry, wear-resisting, radioprotective or insulation aspect.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98101237A CN1082068C (en) | 1998-04-01 | 1998-04-01 | Short staple-containing composite polyimide material and its preparation and use |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98101237A CN1082068C (en) | 1998-04-01 | 1998-04-01 | Short staple-containing composite polyimide material and its preparation and use |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1230570A true CN1230570A (en) | 1999-10-06 |
| CN1082068C CN1082068C (en) | 2002-04-03 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98101237A Expired - Lifetime CN1082068C (en) | 1998-04-01 | 1998-04-01 | Short staple-containing composite polyimide material and its preparation and use |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100341942C (en) * | 2005-12-29 | 2007-10-10 | 上海交通大学 | Method for preparing poly(p-phenylene benzobisoxazole)/polyimide composite material |
| CN100462403C (en) * | 2006-07-24 | 2009-02-18 | 海洋化工研究院 | Blend of polyimide polymer and its use as high temperature resisting dipping glue |
| CN104403313A (en) * | 2014-11-18 | 2015-03-11 | 上海聿衡新材料科技有限公司 | Polyimide composite material and preparation method thereof |
| CN105255178A (en) * | 2015-10-12 | 2016-01-20 | 苏州亿馨源光电科技有限公司 | Impact-resistant composite insulating material and preparing method thereof |
| CN108239399A (en) * | 2018-01-29 | 2018-07-03 | 铜陵四通环境科技有限公司 | A kind of preparation method of high temperature resistant glass fibre reinforced plastic |
| CN108299825A (en) * | 2018-03-23 | 2018-07-20 | 航天特种材料及工艺技术研究所 | Compound electromagnetic wave transparent material of fire resistant resin base and preparation method thereof when a kind of long |
| CN109337367A (en) * | 2018-10-19 | 2019-02-15 | 浙江仁丰科技有限公司 | A kind of preparation method of the high-temperature insulation material of the heating sheet of new-energy automobile power battery shell |
| CN112694749A (en) * | 2020-12-28 | 2021-04-23 | 长春长光宇航复合材料有限公司 | non-PMR type polyimide carbon fiber prepreg, composite material and preparation method thereof |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52105959A (en) * | 1976-03-02 | 1977-09-06 | Nippon Piston Ring Co Ltd | Rubbing part material |
| JPS5989824A (en) * | 1982-11-12 | 1984-05-24 | Toray Ind Inc | Composite for sliding member |
| JPS6116964A (en) * | 1984-07-02 | 1986-01-24 | Toray Ind Inc | Carbon fiber-reinforced heat-resistant resin composition |
| JP2540513B2 (en) * | 1986-03-07 | 1996-10-02 | 三井東圧化学株式会社 | Resin composition with excellent plating characteristics |
| JPS62263253A (en) * | 1986-05-09 | 1987-11-16 | Showa Denko Kk | Resin composition |
| JP2946510B2 (en) * | 1987-09-04 | 1999-09-06 | 東レ株式会社 | Polyimide resin composition |
| JPH0481461A (en) * | 1990-07-25 | 1992-03-16 | Toray Ind Inc | Polyimide resin composition |
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1998
- 1998-04-01 CN CN98101237A patent/CN1082068C/en not_active Expired - Lifetime
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100341942C (en) * | 2005-12-29 | 2007-10-10 | 上海交通大学 | Method for preparing poly(p-phenylene benzobisoxazole)/polyimide composite material |
| CN100462403C (en) * | 2006-07-24 | 2009-02-18 | 海洋化工研究院 | Blend of polyimide polymer and its use as high temperature resisting dipping glue |
| CN104403313A (en) * | 2014-11-18 | 2015-03-11 | 上海聿衡新材料科技有限公司 | Polyimide composite material and preparation method thereof |
| CN105255178A (en) * | 2015-10-12 | 2016-01-20 | 苏州亿馨源光电科技有限公司 | Impact-resistant composite insulating material and preparing method thereof |
| CN108239399A (en) * | 2018-01-29 | 2018-07-03 | 铜陵四通环境科技有限公司 | A kind of preparation method of high temperature resistant glass fibre reinforced plastic |
| CN108299825A (en) * | 2018-03-23 | 2018-07-20 | 航天特种材料及工艺技术研究所 | Compound electromagnetic wave transparent material of fire resistant resin base and preparation method thereof when a kind of long |
| CN109337367A (en) * | 2018-10-19 | 2019-02-15 | 浙江仁丰科技有限公司 | A kind of preparation method of the high-temperature insulation material of the heating sheet of new-energy automobile power battery shell |
| CN112694749A (en) * | 2020-12-28 | 2021-04-23 | 长春长光宇航复合材料有限公司 | non-PMR type polyimide carbon fiber prepreg, composite material and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1082068C (en) | 2002-04-03 |
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