CN116178954B - Bismaleimide resin composite material for carbon fiber prepreg tape and preparation method thereof - Google Patents
Bismaleimide resin composite material for carbon fiber prepreg tape and preparation method thereof Download PDFInfo
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
- C08J5/241—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using inorganic fibres
- C08J5/243—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using inorganic fibres using carbon fibres
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- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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Abstract
The invention belongs to the field of resin-based composite materials, and particularly relates to a bismaleimide resin composite material for a carbon fiber prepreg tape and a preparation method thereof. The composite material comprises the following components in parts by mass: 35-60 parts of o-diallyl bisphenol A,30-60 parts of bismaleimide resin, 1-3 parts of accelerator and 0.05-1.5 parts of graphene. The o-diallyl bisphenol A can enable the bismaleimide resin to have good viscosity, is favorable for the prepreg tape to have better shock resistance after curing, the interaction of the accelerator and the bismaleimide resin can reduce the curing temperature of the resin, and the interaction of the graphene and the bismaleimide resin can improve the overall corrosion resistance and wear resistance.
Description
Technical Field
The invention belongs to the field of resin-based composite materials, and particularly relates to a bismaleimide resin composite material for a carbon fiber prepreg tape and a preparation method thereof.
Background
The bismaleimide resin matrix composite material has excellent mechanical strength and high temperature resistance, is widely applied in the aerospace field, has much lower weight than metal, and is a lightweight material in the aerospace field. The bismaleimide resin prepreg tape is an important intermediate product of aerospace parts, however, the bismaleimide resin is poor in impact resistance after being cured, toughening modification is often needed, but even if the bismaleimide resin system is subjected to toughening modification, the viscosity and the film forming property are poor, the prepreg tape is not beneficial to manufacturing, the process production can be carried out only by heating to a higher temperature (usually more than 90 ℃), the energy consumption is high, and the requirement on equipment temperature control is high. Meanwhile, the long-term use of the resin requires a certain corrosion and wear resisting effect, and the addition of conventional corrosion and wear resisting agents for achieving the effect can affect the performance of the whole system.
Disclosure of Invention
The invention provides a bismaleimide resin composite material for a carbon fiber prepreg tape and a preparation method, and the bismaleimide resin composite material is realized by the following technical scheme:
the bismaleimide resin composite material disclosed by the invention comprises the following materials in parts by weight: 35-60 parts of o-diallyl bisphenol A,30-60 parts of bismaleimide resin, 1-3 parts of accelerator and 0.05-1.5 parts of graphene.
The bismaleimide resin of the invention adopts one or more of BMI-1, BMI-3, BMI-4, BMI-6 or BMI-70 and BMI-80 of Honghu city bismaleimide material technology Co., ltd.
The accelerator is composed of one or more of organic phosphines, thiourea or imidazole compounds.
Graphene is composed of one or both of SE1231, SE1232 manufactured by the company, science and technology, sixth element, inc.
The invention also provides a preparation method of the bismaleimide resin composite material for the wet-process carbon fiber prepreg tape, which comprises the following steps:
(1) Weighing: according to the weight portions, 35 to 60 portions of the o-diallyl bisphenol A,30 to 60 portions of the bismaleimide resin, 1 to 3 portions of the accelerator and 0.05 to 1.5 portions of the graphene are weighed;
(2) Preparing a resin mixture: baking the O-diallyl bisphenol A weighed in the step (1) to a flowing state, stirring in a high-speed dispersing machine at 50-80 ℃, adding the accelerator and the graphene during the stirring, and fully and uniformly mixing for 15-30min;
(3) Blending and discharging: transferring the mixture obtained in step (2) into a reaction kettle, gradually adding bismaleimide resin into the reaction kettle after the temperature is raised to 80-100 ℃, heating and stirring for 30-60min at the temperature in the range, and discharging after fully and uniformly mixing.
The bismaleimide resin composite material prepared by the invention is used for preparing a carbon fiber prepreg tape, and the specific application method is as follows:
and continuously dipping and winding the carbon fiber belt by using a mixed solution of bismaleimide resin and methylene dichloride, and standing at room temperature (10-40 ℃) for more than 6 hours to obtain the carbon fiber prepreg belt.
The mass ratio of the bismaleimide resin to the dichloromethane is 1:2; the winding speed is 3-6 m/min.
The beneficial effects of the invention are as follows:
in the invention, the o-diallyl bisphenol A can ensure that the bismaleimide resin has good viscosity, and the cross-linking copolymerization reaction with the bismaleimide resin can ensure that the cured product has good shock resistance besides high strength, and the addition amount of the o-diallyl bisphenol A can effectively improve the fluidity of the bismaleimide resin at a lower temperature, so that the use at the lower temperature is convenient; the accelerator can form a copolymer with the bismaleimide resin in the curing reaction process, so that the curing temperature is effectively reduced, the curing time is shortened, the curing production efficiency is effectively improved, the crosslinking density is increased, the influence of the accelerator on the glass transition temperature and brittleness of the bismaleimide resin can be reduced due to the lower proportion of the accelerator, the performance of the bismaleimide resin on high temperature resistance and impact resistance is facilitated, the glass transition temperature Tg (DMA) after curing can reach more than 230 ℃, and the thermal decomposition Temperature (TGA) is 5 percent
400 ℃ or above; the active functional groups in the graphene and the bismaleimide resin are subjected to in-situ polymerization in the manufacturing process and are uniformly adhered to the bismaleimide resin, so that the corrosion resistance and the wear resistance of the cured workpiece are greatly improved outside the good mechanical properties, and the problem of non-uniform performance of the workpiece caused by graphene sedimentation is solved. The mixed material is mixed with dichloromethane to regulate the viscosity of the bismaleimide system, so that the bismaleimide system has more proper fluidity, the prepreg tape can be produced at a lower temperature (10-40 ℃) such as normal temperature, the volatility of the dichloromethane is extremely high, and the influence on the post-production products of the finished prepreg tape can be reduced.
Compared with a common bismaleimide resin system, the bismaleimide resin composite material prepared by the invention has higher impact resistance, and the problem that the bismaleimide resin is brittle after solidification is effectively solved; the lower curing temperature can reduce the curing cost and improve the curing production efficiency; because of the better corrosion and wear resistance, the product can not use special corrosion or wear resistance measures.
The prepreg tape prepared by the invention can be used for weaving, winding, laying silk, laying tape and other processes of sample pieces because of similar fiber shapes, meets the process requirements of different products, and can be stored for a long time at normal temperature without problems of gummosis, sedimentation, embrittlement and the like when used for a long time.
Drawings
Fig. 1 is a winding picture of a prepreg tape prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
The bismaleimide resin composite material for the prepreg tape consists of the following raw materials in parts by weight:
o-diallyl bisphenol A:40 parts, BMI-1:15 parts of KI-70:15 parts of diethyl thiourea: 1 part of graphene SE1231:0.1 part.
Baking the weighed O-diallyl bisphenol A to a flowing state, stirring in a high-speed dispersing machine at 80 ℃, adding an accelerator diethyl thiourea and graphene during the stirring, and fully and uniformly mixing for 30min; then transferring the mixture into a reaction kettle, gradually adding the bismaleimide resin into the reaction kettle after the temperature is raised to 100 ℃, heating and stirring for 30min at the temperature in the range, and discharging after fully and uniformly mixing.
Example 2
The bismaleimide resin composite material for the prepreg tape consists of the following raw materials in parts by weight:
o-diallyl bisphenol A:60 parts of BMI-1:20 parts, BMI-4:15 parts of KI-80:25 parts of triphenylphosphine: 3 parts of graphene SE1232:1 part.
Baking the weighed O-diallyl bisphenol A to a flowing state, stirring in a high-speed dispersing machine at 50 ℃, adding accelerator triphenylphosphine and graphene during the stirring, and fully and uniformly mixing for 15min; transferring the mixture into a reaction kettle, gradually adding the bismaleimide resin into the reaction kettle after the temperature is raised to 100 ℃, heating and stirring for 60min at the temperature in the range, and discharging after fully and uniformly mixing.
Example 3
The invention relates to a bismaleimide resin composite material for prepreg tape, which is composed of the following raw materials in parts by weight:
o-diallyl bisphenol A:50 parts of BMI-3:10 parts of BMI-6:15 parts of KI-70:20 parts of methylimidazole: 1.5 parts of graphene SE1231:0.5 parts, SE1232:0.5 part.
Baking the weighed O-diallyl bisphenol A to a flowing state, stirring in a high-speed dispersing machine at 50 ℃, adding an accelerator methylimidazole and graphene during the stirring, and fully and uniformly mixing for 30min; transferring the mixture into a reaction kettle, gradually adding the bismaleimide resin into the reaction kettle after the temperature is raised to 90 ℃, heating and stirring for 45min at the temperature in the range, and discharging after fully and uniformly mixing.
Example 4
The bismaleimide resin composite material for the prepreg tape consists of the following raw materials in parts by weight:
o-diallyl bisphenol A:35 parts, BMI-1:20 parts, BMI-4:15 parts of KI-80:25 parts of triphenylphosphine: 3 parts of graphene SE1232:1 part.
Baking the weighed O-diallyl bisphenol A to a flowing state, stirring in a high-speed dispersing machine at 50 ℃, adding accelerator triphenylphosphine and graphene during the stirring, and fully and uniformly mixing for 15min; transferring the mixture into a reaction kettle, gradually adding the bismaleimide resin into the reaction kettle after the temperature is raised to 100 ℃, heating and stirring for 60min at the temperature in the range, and discharging after fully and uniformly mixing.
Example 5
The bismaleimide resin composite material for the prepreg tape consists of the following raw materials in parts by weight:
o-diallyl bisphenol A:60 parts of BMI-1:20 parts, BMI-4:15 parts of KI-80:25 parts of triphenylphosphine: 3 parts of graphene SE1232:0.05 part.
Baking the weighed O-diallyl bisphenol A to a flowing state, stirring in a high-speed dispersing machine at 50 ℃, adding accelerator triphenylphosphine and graphene during the stirring, and fully and uniformly mixing for 15min; transferring the mixture into a reaction kettle, gradually adding the bismaleimide resin into the reaction kettle after the temperature is raised to 100 ℃, heating and stirring for 60min at the temperature in the range, and discharging after fully and uniformly mixing.
Example 6
The bismaleimide resin composite material for the prepreg tape consists of the following raw materials in parts by weight:
o-diallyl bisphenol A:60 parts of BMI-1:20 parts, BMI-4:15 parts of KI-80:25 parts of triphenylphosphine: 3 parts of graphene SE1232:1.5 parts.
Baking the weighed O-diallyl bisphenol A to a flowing state, stirring in a high-speed dispersing machine at 50 ℃, adding accelerator triphenylphosphine and graphene during the stirring, and fully and uniformly mixing for 15min; transferring the mixture into a reaction kettle, gradually adding the bismaleimide resin into the reaction kettle after the temperature is raised to 100 ℃, heating and stirring for 60min at the temperature in the range, and discharging after fully and uniformly mixing.
Comparative example 1
The bismaleimide resin composite material for the prepreg tape consists of the following raw materials in parts by weight:
o-diallyl bisphenol A:60 parts of BMI-1:20 parts, BMI-4:15 parts of KI-80:25 parts of triphenylphosphine: 3 parts of molybdenum disulfide: 3 parts.
Baking the weighed O-diallyl bisphenol A to a flowing state, stirring in a high-speed dispersing machine at 50 ℃, adding accelerator triphenylphosphine and molybdenum disulfide during the stirring, and fully and uniformly mixing for 15min; transferring the mixture into a reaction kettle, gradually adding the bismaleimide resin into the reaction kettle after the temperature is raised to 100 ℃, heating and stirring for 60min at the temperature in the range, and discharging after fully and uniformly mixing.
Comparative example 2
The bismaleimide resin composite material for the prepreg tape consists of the following raw materials in parts by weight:
o-diallyl bisphenol A:60 parts of BMI-1:20 parts, BMI-4:15 parts of KI-80:25 parts of triphenylphosphine: 3 parts of polytetrafluoroethylene powder: 3 parts.
Baking the weighed O-diallyl bisphenol A to a flowing state, stirring in a high-speed dispersing machine at 50 ℃, adding accelerator triphenylphosphine and polytetrafluoroethylene powder during the stirring, and fully and uniformly mixing for 15min; transferring the mixture into a reaction kettle, gradually adding the bismaleimide resin into the reaction kettle after the temperature is raised to 100 ℃, heating and stirring for 60min at the temperature in the range, and discharging after fully and uniformly mixing.
The results of the main performance test of the resin system of the above example are shown in Table 1.
TABLE 1
In examples 1 to 3 above, the abrasion index of the cast article was improved by 35% or more as compared with the conventional bismaleimide resin, and the corrosion resistance under the salt spray condition was improved by about 3 times.
The composite material prepared in example 2 of the present invention was combined with dichloromethane 1 at room temperature (10-40 ℃): the viscosity of the 2-proportion mixing is about 500-600 cps, the viscosity is very suitable for prepreg tape production, meanwhile, the mixed liquid and carbon fiber have good impregnating effect and film forming property (the resin is uniformly distributed on the fiber tape, the resin is not agglomerated and falls off after being placed for a long time, as shown in figure 1), and the viscosity is moderate, thereby being suitable for manufacturing a downstream product process.
Example 4 after the amount of O-diallyl bisphenol A was reduced (less than 40 parts), the viscosity increased, and the production of prepreg tape could not be performed due to the higher viscosity when used at normal temperature; after the addition amount of graphene is reduced (less than 0.1 part) in example 5, the abrasion index and the corrosion resistance are obviously reduced; example 6 showed no increase in abrasion index and corrosion resistance after increasing the amount of graphene added (more than 1 part).
In comparative example 1, graphene is replaced, molybdenum disulfide is used, the addition amount is 3 parts, the abrasion index is only increased by about 13%, and no improvement in corrosion resistance is realized; comparative example 2 replaced graphene, and the addition amount was 3 parts by using polytetrafluoroethylene powder, and the salt spray test was close to the graphene level, but the abrasion resistance was still increased by only about 19%.
Based on the above comparison, the addition amounts of the respective functional materials are most suitable in the range of the present invention and in the material selection aspect of example 1, example 2, and example 3.
Claims (6)
1. The bismaleimide resin composite material is characterized by comprising the following components in parts by weight: 35-60 parts of o-diallyl bisphenol A,30-60 parts of bismaleimide resin, 1-3 parts of accelerator and 0.05-1.5 parts of graphene;
the bismaleimide resin is selected from one or more of BMI-1, BMI-3, BMI-4, BMI-6, BMI-70 and BMI-80;
the graphene is selected from one or two of SE1231 and SE 1232.
2. The bismaleimide resin composite according to claim 1 wherein the accelerator is composed of one or more of organic phosphines, thioureas or imidazoles.
3. A method for preparing the bismaleimide resin composite according to claim 1 wherein the steps of the preparation method are as follows:
(1) Weighing: weighing the O-diallyl bisphenol A, the bismaleimide resin, the accelerator and the graphene according to parts by weight;
(2) Preparing a resin mixture: baking the O-diallyl bisphenol A weighed in the step (1) to a flowing state, stirring in a high-speed dispersing machine at 50-80 ℃, adding the accelerator and the graphene during the stirring, and fully and uniformly mixing for 15-30min;
(3) Blending and discharging: transferring the mixture obtained in step (2) into a reaction kettle, gradually adding bismaleimide resin into the reaction kettle after the temperature is raised to 80-100 ℃, heating and stirring for 30-60min at the temperature in the range, and discharging after fully and uniformly mixing.
4. A carbon fiber prepreg tape prepared using the bismaleimide resin according to claim 1.
5. A method of preparing a prepreg tape according to claim 4, wherein the method of preparing comprises: and continuously dipping and winding the carbon fiber belt by using a mixed liquid of bismaleimide resin and methylene dichloride, and standing at room temperature for more than 6 hours to obtain the carbon fiber prepreg belt.
6. The method for preparing a carbon fiber prepreg tape according to claim 5, wherein the mass ratio of the bismaleimide resin to the methylene chloride is 1:2; the winding speed is 3-6 m/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102796375A (en) * | 2012-08-09 | 2012-11-28 | 西北工业大学 | Hyperbranched polysiloxane grafted graphene/bismaleimide composite material and preparation method thereof |
| CN107298858A (en) * | 2017-07-12 | 2017-10-27 | 中国航发北京航空材料研究院 | A kind of graphene oxide toughening model+composition and preparation method thereof |
| CN109206905A (en) * | 2018-08-29 | 2019-01-15 | 中航复合材料有限责任公司 | A kind of graphene bismaleimide resin composite material and preparation method thereof |
| CN114685990A (en) * | 2020-12-31 | 2022-07-01 | 洛阳尖端技术研究院 | Modified graphene/bismaleimide resin and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102796375A (en) * | 2012-08-09 | 2012-11-28 | 西北工业大学 | Hyperbranched polysiloxane grafted graphene/bismaleimide composite material and preparation method thereof |
| CN107298858A (en) * | 2017-07-12 | 2017-10-27 | 中国航发北京航空材料研究院 | A kind of graphene oxide toughening model+composition and preparation method thereof |
| CN109206905A (en) * | 2018-08-29 | 2019-01-15 | 中航复合材料有限责任公司 | A kind of graphene bismaleimide resin composite material and preparation method thereof |
| CN114685990A (en) * | 2020-12-31 | 2022-07-01 | 洛阳尖端技术研究院 | Modified graphene/bismaleimide resin and preparation method thereof |
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