CN108929519A - A kind of basalt fiber composite material and preparation method thereof - Google Patents
A kind of basalt fiber composite material and preparation method thereof Download PDFInfo
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- CN108929519A CN108929519A CN201710388822.5A CN201710388822A CN108929519A CN 108929519 A CN108929519 A CN 108929519A CN 201710388822 A CN201710388822 A CN 201710388822A CN 108929519 A CN108929519 A CN 108929519A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
- C08G59/32—Epoxy compounds containing three or more epoxy groups
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/12—Unsaturated polyimide precursors
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/05—Polymer mixtures characterised by other features containing polymer components which can react with one another
Abstract
The present invention provides a kind of basalt fiber composite material and preparation method thereof, this method includes：Epoxy resin and cyanate ester resin are stirred according to the ratio, toughener is added, adds curing catalysts, is stirred, forms Toughening Epoxy Resin cyanate ester resin；Prepreg is made in Toughening Epoxy Resin cyanate ester resin and basalt fibre；And laying, solidification, obtain basalt fiber composite material.The mechanical property and heat resistance of the basalt composite material of preparation greatly enhance, and reduce costs, and can be widely applied to the fields such as industry, building, automobile, aviation.
Description
Technical field
The present invention relates to Material Fields, more particularly, to a kind of basalt fiber composite material and preparation method thereof.
Background technique
Cyanate ester resin (CE) is the novel high-performance resin containing two or more cyanate functional groups (- OCN),
It can satisfy aerospace field structure/function with excellent properties such as high heat resistance, low dielectric constant and dielectric losses
The requirement of energy composite material, is a kind of high performance matrix resin.
But presently, there are epoxy resin/cyanate composite material system in mainly with common bisphenol A type epoxy resin
It is reacted with cyanate ester resin, and the heat resistance of bisphenol A type epoxy resin is significantly lower than the heat resistance of cyanate ester resin, therefore can be sacrificial
The heat resistance of domestic animal cyanate ester resin.
Meanwhile the reinforcement in existing composite material is mainly carbon fiber and glass fibre, carbon fiber has very high
Specific strength, but it is at high cost, it is mainly used in war industry field；Glass fibre is at low cost, equal in war industry and civil field
It is widely used, but glass fibre non-refractory, when temperature is higher than 400 DEG C, loss of strength is serious, retains almost without intensity.
Summary of the invention
The present invention is greater than 3 Toughening Epoxy Resin cyanate ester resin using degree of functionality, effectively maintains resin system
Heat resistance；In addition, reinforcement uses high performance basalt fibre, which is a kind of environment-protection fiber, and mechanical strength is high, source
It is abundant, there is excellent chemical stability, and heat-resist, using temperature up to 650 DEG C, is combined with high performance resin
Composite material further improve the composite materials property and heat resistance, and in preparation process using hot melt prepare
Prepreg, high production efficiency, quality are stable and at low cost.
The present invention provides a kind of preparation methods of basalt fiber composite material, include the following steps：
Epoxy resin and cyanate ester resin are stirred according to the ratio, toughener is added, adds curing catalysts, is stirred
Mixing, vacuum outgas form Toughening Epoxy Resin cyanate ester resin；By Toughening Epoxy Resin cyanate ester resin with it is profound
Prepreg is made in military rock fiber；And laying, solidification, obtain basalt fiber composite material.
In the above preparation method, the mass ratio of epoxy resin and cyanate ester resin is 6~8:2~4.
In the above preparation method, the mass ratio of epoxy resin and cyanate ester resin is 7:3.
In the above preparation method, epoxy resin is four glycidyl amine of diaminodiphenylmethane, four glycidyl methylenes
Diphenylamines or epoxidation m-xylene diamine.
In the above preparation method, cyanate ester resin is bisphenol A cyanate ester resin, bis-phenol M type cyanate ester resin, bis-phenol
E type cyanate ester resin or bisphenol-f type cyanate ester resin.
In the above preparation method, epoxy resin and cyanate ester resin 80~100 DEG C at a temperature of be stirred to mixed
It closes uniform.
In the above preparation method, toughener is the one or more of polyether sulfone, polyetherimide, polysulfones and polyether-ketone.
In the above preparation method, the quality of toughener is the 25~35% of epoxy resin and cyanate ester resin gross mass.
In the above preparation method, curing catalysts be manganese octoate, cupric octoate, zinc octoate, sad chromium it is one or more.
In the above preparation method, the quality of curing catalysts be epoxy resin and cyanate ester resin gross mass 0.8~
1.2%.
In the above preparation method, by hot melt by Toughening Epoxy Resin cyanate ester resin and basalt fibre system
At prepreg.
In the above preparation method, basalt fibre is basalt one-way fabric.
In the above preparation method, cured pressure is 1~2MPa；Cured temperature is 100~150 DEG C；When cured
Between be 1~3h.
The present invention also provides a kind of basalt fiber composite materials prepared according to method made above.
The basalt fibre of the Toughening Epoxy Resin cyanate ester resin of the method preparation provided through the invention is compound
Material, by the selection to epoxy resin type and the epoxy resin and cyanate ester resin quality proportioning, and it is toughener, solid
Change the addition of catalyst, so that-OCN the functional group in cyanate ester resin sufficiently reacts with functional groups more in epoxy resin,
It is mixed again by high-temperature stirring, effectively increases the heat resistance of composite material, the epoxy resin roughening for having obtained function admirable changes
The cyanate ester resin of property, and by compound with high mechanical properties and heat-resist basalt fibre, further had
The composite material of excellent mechanical property and high heat resistance, meanwhile, preparation process is simple, and material source is abundant, can effectively drop
Low cost.
Detailed description of the invention
Fig. 1 is the preparation flow schematic diagram of basalt fiber composite material.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit in any way
The present invention.
The present invention selects degree of functionality to be greater than 3 Toughening Epoxy Resin cyanate ester resin, while selecting high performance profound
Military rock fiber is reinforcement, has obtained the basalt composite material with high mechanical property and heat resistance by hot melt, is had
Steps are as follows for body：
It is 6~8 by mass ratio:2~4 epoxy resin and cyanate ester resin 80~100 DEG C at a temperature of be stirred
To being uniformly mixed, the toughener of 25~35% (percentages for accounting for epoxy resin Yu cyanate ester resin gross mass) is added, stirring is mixed
It is bonded to uniformly mixed, vacuum outgas to bubble-free；Wherein, epoxy resin is four glycidyl amine of diaminodiphenylmethane, Fourth Ring
Oxygen propyl group methylene dianiline or epoxidation m-xylene diamine；Cyanate ester resin is bisphenol A cyanate ester resin, bis-phenol M type cyanic acid
Ester resin, bisphenol E-type cyanate resin or bisphenol-f type cyanate ester resin；Toughener be polyether sulfone, polyetherimide, polysulfones and
Polyether-ketone it is one or more.
The curing catalysts of 0.8~1.2% (percentage for accounting for epoxy resin Yu cyanate ester resin gross mass), stirring is added
It mixes to being uniformly mixed, vacuum outgas to bubble-free forms Toughening Epoxy Resin cyanate ester resin；By normal in this field
Prepreg is made in Toughening Epoxy Resin cyanate ester resin and basalt fibre by hot melt；Wherein, curing catalysts
For manganese octoate, cupric octoate, zinc octoate, sad chromium it is one or more.
Laying, under the pressure of 1~2MPa, 100~150 DEG C of 1~3h of solidification obtain basalt fiber composite material.
Embodiment one
It is 6 by mass ratio:2 four glycidyl amine of diaminodiphenylmethane and bisphenol A cyanate ester resin is at 90 DEG C
At a temperature of be stirred to be uniformly mixed, be added 30% (percentage for accounting for epoxy resin Yu cyanate ester resin gross mass) polyethers
Sulfone is stirred to uniformly mixed, vacuum outgas to bubble-free；
The manganese octoate of 1% (percentage for accounting for epoxy resin Yu cyanate ester resin gross mass) is added, is stirred to mixing
Uniformly, vacuum outgas forms Toughening Epoxy Resin cyanate ester resin to bubble-free；By hot melt by epoxy resin roughening
Prepreg is made in modified cyanic acid ester resin and basalt fibre；
Laying, under the pressure of 1MPa, 150 DEG C of solidification 3h obtain basalt fiber composite material.
Embodiment two
It is 8 by mass ratio:3 four glycidyl methylene dianilines and bis-phenol M type cyanate ester resin 80 DEG C at a temperature of
It is stirred to being uniformly mixed, the polyetherimide of 25% (percentage for accounting for epoxy resin Yu cyanate ester resin gross mass) is added
Amine is stirred to uniformly mixed, vacuum outgas to bubble-free；
The cupric octoate of 0.8% (percentage for accounting for epoxy resin Yu cyanate ester resin gross mass) is added, is stirred to mixed
It closes uniformly, vacuum outgas to bubble-free forms Toughening Epoxy Resin cyanate ester resin；Epoxy resin is increased by hot melt
Prepreg is made in tough modified cyanic acid ester resin and basalt fibre；
Laying, under the pressure of 2MPa, 100 DEG C of solidification 1h obtain basalt fiber composite material.
Embodiment three
It is 7 by mass ratio:4 four glycidyl amine of diaminodiphenylmethane and bisphenol E-type cyanate resin is at 100 DEG C
At a temperature of be stirred to be uniformly mixed, be added 35% (percentage for accounting for epoxy resin Yu cyanate ester resin gross mass) gather
Sulfone is stirred to uniformly mixed, vacuum outgas to bubble-free；
The zinc octoate of 0.9% (percentage for accounting for epoxy resin Yu cyanate ester resin gross mass) is added, is stirred to mixed
It closes uniformly, vacuum outgas to bubble-free forms Toughening Epoxy Resin cyanate ester resin；Epoxy resin is increased by hot melt
Prepreg is made in tough modified cyanic acid ester resin and basalt fibre；
Laying, under the pressure of 1.5MPa, 125 DEG C of solidification 2h obtain basalt fiber composite material.
Example IV
It is 7 by mass ratio:3 four glycidyl amine of diaminodiphenylmethane and bisphenol-f type cyanate ester resin is at 95 DEG C
At a temperature of be stirred to be uniformly mixed, be added 29% (percentage for accounting for epoxy resin Yu cyanate ester resin gross mass) polyethers
Ketone is stirred to uniformly mixed, vacuum outgas to bubble-free；
The sad chromium of 1.2% (percentage for accounting for epoxy resin Yu cyanate ester resin gross mass) is added, is stirred to mixed
It closes uniformly, vacuum outgas to bubble-free forms Toughening Epoxy Resin cyanate ester resin；Epoxy resin is increased by hot melt
Prepreg is made in tough modified cyanic acid ester resin and basalt fibre；
Laying, under the pressure of 2MPa, 100 DEG C of solidification 1.5h obtain basalt fiber composite material.
Embodiment five
It is 7 by mass ratio:3 epoxidation m-xylene diamine and bisphenol A cyanate ester resin 90 DEG C at a temperature of stir
It mixes to being uniformly mixed, the polyether sulfone of 30% (percentage for accounting for epoxy resin Yu cyanate ester resin gross mass) is added, stirring is mixed
It is bonded to uniformly mixed, vacuum outgas to bubble-free；
The manganese octoate of 1.1% (percentage for accounting for epoxy resin Yu cyanate ester resin gross mass) is added, is stirred to mixed
It closes uniformly, vacuum outgas to bubble-free forms Toughening Epoxy Resin cyanate ester resin；Epoxy resin is increased by hot melt
Prepreg is made in tough modified cyanic acid ester resin and basalt fibre；
Laying, under the pressure of 1MPa, 150 DEG C of solidification 3h obtain basalt fiber composite material.
Embodiment six
It is 7 by mass ratio:3 four glycidyl amine of diaminodiphenylmethane and bisphenol A cyanate ester resin is at 85 DEG C
At a temperature of be stirred to be uniformly mixed, be added 30% (percentage for accounting for epoxy resin Yu cyanate ester resin gross mass) polyethers
Sulfone is stirred to uniformly mixed, vacuum outgas to bubble-free；
The manganese octoate of 1% (percentage for accounting for epoxy resin Yu cyanate ester resin gross mass) is added, is stirred to mixing
Uniformly, vacuum outgas forms Toughening Epoxy Resin cyanate ester resin to bubble-free；By hot melt by epoxy resin roughening
Prepreg is made in modified cyanic acid ester resin and basalt fibre；
Laying, under the pressure of 1.5MPa, 130 DEG C of solidification 2h obtain basalt fiber composite material.
It is stirred above using SHR-10 high-speed mixer, revolving speed is 800~900r/min.
Impact strength, compressive strength use method commonly used in the art, use CMT5105 electronic universal cupping machine
Measurement；Glass transition temperature is measured using differential scanning calorimetry (DSC) commonly used in the art.
The batten of 30mm*30mm*4mm is cut into after the basalt composite material of embodiment one to six is cooled to room temperature,
Its impact strength, compressive strength and glass transition temperature are tested, test result see the table below 1：
Table 1, test result
Seen from table 1, the present invention is greater than 3 Toughening Epoxy Resin cyanate ester resin using degree of functionality, passes through selection
The quality proportioning of epoxy resin type and the epoxy resin and cyanate ester resin, and the addition of toughener, curing catalysts,
So that-OCN the functional group in cyanate ester resin and more functional group reactions in epoxy resin, then mixed by high-temperature stirring,
The heat resistance of the cyanate ester resin of Toughening Epoxy Resin is improved, so that the glass transition temperature Tg of the composite material is most
Up to 650 DEG C, and the basalt fibre due to having used mechanical property good, and resin film is infiltrated into enhancing using hot melt
Material basalt fibre, so that the impact resistance and toughness of composite material greatly enhance, impact strength is up to 475.41kJ/
m2, compressive strength is up to 331MPa.Therefore, the basalt fiber composite material of the method preparation provided through the invention has
High mechanical property and heat resistance, and it is at low cost, it can be widely applied to the fields such as industry, building, automobile, aviation.
It will be understood by those skilled in the art that above embodiments are only exemplary embodiments, without departing substantially from spirit of the invention
In the case where range, a variety of variations can be carried out, replaced and changed.
Claims (14)
1. a kind of preparation method of basalt fiber composite material, which is characterized in that include the following steps：
Epoxy resin and cyanate ester resin are stirred according to the ratio, toughener is added, adds curing catalysts, stirring is mixed
It closes, forms Toughening Epoxy Resin cyanate ester resin；
Prepreg is made in the Toughening Epoxy Resin cyanate ester resin and basalt fibre；And
Laying, solidification obtain the basalt fiber composite material.
2. preparation method according to claim 1, which is characterized in that the matter of the epoxy resin and the cyanate ester resin
Amount is than being 6~8:2~4.
3. preparation method according to claim 2, which is characterized in that the matter of the epoxy resin and the cyanate ester resin
Amount is than being 7:3.
4. preparation method according to claim 1, which is characterized in that the epoxy resin is the contracting of diaminodiphenylmethane four
Water glyceramine, four glycidyl methylene dianilines or epoxidation m-xylene diamine.
5. preparation method according to claim 1, which is characterized in that the cyanate ester resin is bisphenol A cyanate ester tree
Rouge, bis-phenol M type cyanate ester resin, bisphenol E-type cyanate resin or bisphenol-f type cyanate ester resin.
6. preparation method according to claim 1, which is characterized in that the epoxy resin and the cyanate ester resin are 80
It is stirred at a temperature of~100 DEG C to uniformly mixed.
7. preparation method according to claim 1, which is characterized in that the toughener is polyether sulfone, polyetherimide, gathers
Sulfone and polyether-ketone it is one or more.
8. preparation method according to claim 7, which is characterized in that the quality of the toughener be the epoxy resin and
The 25~35% of the cyanate ester resin gross mass.
9. preparation method according to claim 1, which is characterized in that the curing catalysts are manganese octoate, cupric octoate, pungent
Sour zinc, sad chromium it is one or more.
10. preparation method according to claim 9, which is characterized in that the quality of the curing catalysts is the epoxy
The 0.8~1.2% of resin and the cyanate ester resin gross mass.
11. preparation method according to claim 1, which is characterized in that changed the epoxy resin roughening by hot melt
Property cyanate ester resin and the basalt fibre prepreg is made.
12. preparation method according to claim 11, which is characterized in that the basalt fibre is that basalt is unidirectionally knitted
Object.
13. preparation method according to claim 1, which is characterized in that the cured pressure is 1~2MPa；It is described solid
The temperature of change is 100~150 DEG C；The cured time is 1~3h.
14. a kind of basalt fiber composite material of preparation method preparation according to claim 1 to 13.
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| CN201710388822.5A CN108929519A (en) | 2017-05-24 | 2017-05-24 | A kind of basalt fiber composite material and preparation method thereof |
| PCT/CN2018/083676 WO2018214680A1 (en) | 2017-05-24 | 2018-04-19 | Basalt fiber composite material and preparation method therefor |
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| CN201710388822.5A CN108929519A (en) | 2017-05-24 | 2017-05-24 | A kind of basalt fiber composite material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110357785A (en) * | 2019-07-26 | 2019-10-22 | 阳姓桦 | A kind of preparation method of cyanate ester resin plasticizer |
| CN112111150A (en) * | 2020-08-20 | 2020-12-22 | 陕西省建筑科学研究院有限公司 | La-BF/BADCy composite material and preparation method thereof |
| CN113320239A (en) * | 2021-06-15 | 2021-08-31 | 武汉中科先进技术研究院有限公司 | Basalt fiber reinforced wear-resistant composite material and preparation method thereof |
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