CN111808310A - Preparation method of special high-performance composite material pre-immersion liquid for aerospace - Google Patents
Preparation method of special high-performance composite material pre-immersion liquid for aerospace Download PDFInfo
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- CN111808310A CN111808310A CN202010514351.XA CN202010514351A CN111808310A CN 111808310 A CN111808310 A CN 111808310A CN 202010514351 A CN202010514351 A CN 202010514351A CN 111808310 A CN111808310 A CN 111808310A
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/18—Introducing halogen atoms or halogen-containing groups
- C08F8/20—Halogenation
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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
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
- C08J2333/26—Homopolymers or copolymers of acrylamide or methacrylamide
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/29—Compounds containing one or more carbon-to-nitrogen double bonds
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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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring
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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
- C08K7/06—Elements
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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
- C08K9/00—Use of pretreated ingredients
Abstract
The invention discloses a preparation method of a special high-performance composite material pre-immersion liquid for aerospace, and relates to the technical field of composite materials, wherein modified acrylamide-acrylic resin is prepared by the invention, can be dissolved in water to prepare emulsion, and has good adhesive property; the carbon fiber is used as a main material, a pre-immersion liquid containing the carbon fiber is obtained by adding self-made resin, nano filler, coupling agent and curing agent, the pre-immersion liquid is used for immersing basalt fiber, and a carbon fiber layer can be formed on the outer layer of the basalt fiber after high-temperature roasting, so that the using amount of the carbon fiber in the material is reduced, and the strength of the material is ensured.
Description
The technical field is as follows:
the invention relates to the technical field of composite materials, in particular to a preparation method of a special high-performance composite material pre-immersion liquid for aerospace.
Background art:
in recent years, the application of composite materials in the field of aerospace is wider and wider, and the performance requirements of the composite materials are higher and higher. The interface of the composite material reinforcement and the matrix and the dispersion of the reinforcement become the bottleneck of improving the performance of the composite material. Carbon materials such as graphene, carbon nanotubes, etc. have excellent mechanical properties and are often used as reinforcements, however, the application of graphene materials is limited by their hydrophobicity.
The carbon fiber is a high-strength and high-modulus fiber material with the carbon content of more than 95%, but most of the carbon fiber is imported and has higher price, and if the material is completely made of the carbon fiber, the processing cost of the material is increased undoubtedly. In addition, the conventional impregnation method in the field mostly adopts an organic solvent as a diluent, and has the problems of difficult solvent volatilization and processing environment pollution.
The invention content is as follows:
the invention aims to solve the technical problem of providing a preparation method of a special high-performance composite material pre-immersion liquid for aerospace.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
the preparation method of the special high-performance composite material pre-immersion liquid for aerospace comprises the following preparation steps:
(1) pretreatment of carbon fibers: placing the carbon fiber in an oven for drying, and roasting at high temperature;
(2) preparation of acrylamide-acrylate resin emulsion: dissolving acrylamide and hydroxypropyl acrylate in water to obtain a monomer aqueous solution, heating for reaction, dropwise adding an initiator aqueous solution, carrying out heat preservation reaction after dropwise adding is finished, and obtaining an acrylamide-acrylate resin emulsion after the reaction is finished;
(3) preparation of modified acrylamide-acrylic resin: dissolving bromooxime ether in methanol to obtain bromooxime ether solution, adding the bromooxime ether solution into the prepared acrylamide-acrylate resin emulsion, heating for reaction, dropwise adding an acid-binding agent aqueous solution, carrying out heat preservation reaction after dropwise adding is finished, carrying out reaction, and carrying out reduced pressure distillation to recover methanol and remove water to obtain modified acrylamide-acrylic resin;
(4) preparation of a pre-immersion liquid: and adding the pretreated carbon fibers, the prepared modified acrylamide-acrylic resin, the nano filler, the coupling agent and the curing agent into water, and mixing at a high speed to obtain a pre-immersion liquid with the solid content of 50-80%.
The mol ratio of the acrylamide to the hydroxypropyl acrylate to the bromooxime ether to the acid-binding agent is 5-30:3-10:1: 1.05-1.1.
The initiator aqueous solution is prepared by adding water into ammonium persulfate.
The acid-binding agent solution is prepared by adding water into potassium carbonate.
The mass ratio of the carbon fiber, the modified acrylamide-acrylic resin, the nano filler, the coupling agent and the curing agent is 100:50-100:5-15:1-10: 1-10.
The nano filler is one or more of nano calcium carbonate, nano silicon dioxide, nano aluminum oxide and nano titanium dioxide.
The coupling agent is a silane coupling agent. The silane coupling agent plays a role in dispersion and promotes the uniform dispersion of the inorganic filler in the resin.
The curing agent is polyisocyanate.
The method for processing the special high-performance composite material for aerospace by using the prepared pre-immersion liquid comprises the following processing processes:
(1) setting a dipping tank, and pouring a pre-dipping solution into the dipping tank;
(2) enabling the basalt fibers to pass through a dipping tank at a constant speed, and removing redundant pre-dipping liquid through a rubber scraping roller after dipping;
(3) enabling the soaked basalt fibers to pass through a heat flow drying channel, roasting at high temperature, and cooling to obtain prepreg cloth;
(4) covering with release paper, rolling, and storing.
The dipping time of the basalt fibers in the dipping tank is 10-30 min.
The temperature of the heat flow drying channel is 130-160 ℃.
The high-temperature roasting temperature is 300-400 ℃.
The design principle of the technical scheme of the invention is as follows:
1. the carbon fiber is dried and roasted to remove the contained moisture and impurities, so that the internal channel of the carbon fiber is kept smooth.
2. The invention utilizes acrylamide and hydroxypropyl acrylate to synthesize hydrophilic acrylamide-acrylate resin, thereby being beneficial to taking water as a diluting solvent of the pre-immersion liquid and avoiding the problems of environmental pollution and use safety existing when an organic solvent is taken as the diluting solvent of the pre-immersion liquid.
3. The oxime ether bromide is used as a modifier, and hydroxyl contained in an acrylamide-acrylate resin structure is reacted with the oxime ether bromide to graft an oxime ether structure on the acrylamide-acrylate resin, so that the adhesive property of the acrylamide-acrylate resin is optimized, and the uniform and massive fixation of carbon fibers on a target material is promoted to form a carbon fiber layer with a certain thickness. The bromooxime ether is generally used for synthesizing kresoxim-methyl and trifloxystrobin, and the application creatively uses the bromooxime ether as a modifier of self-made acrylamide-acrylate resin and obtains the technical effect of remarkably improving the strength of the finally prepared composite material through carbon fibers.
4. The invention takes the basalt fiber with relatively low price as the base material, fixes the resin component and the carbon fiber component in the pre-immersion liquid on the outer layer of the basalt fiber by an immersion method, the resin component in the pre-immersion liquid plays a role in gluing, and the resin component is decomposed and gasified after high-temperature roasting, so that a carbon fiber layer is formed on the outer layer of the basalt fiber, thereby reducing the using amount of the carbon fiber and ensuring the strength of the material.
The invention has the beneficial effects that: the modified acrylamide-acrylic resin is prepared by the invention, can be dissolved in water to prepare emulsion, and has good adhesive property; the carbon fiber is used as a main material, a pre-immersion liquid containing the carbon fiber is obtained by adding self-made resin, nano filler, coupling agent and curing agent, the pre-immersion liquid is used for immersing basalt fiber, and a carbon fiber layer can be formed on the outer layer of the basalt fiber after high-temperature roasting, so that the using amount of the carbon fiber in the material is reduced, and the strength of the material is ensured.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
1. Preparation of a pre-immersion liquid:
(1) pretreatment of carbon fibers: placing the carbon fiber in a drying oven at 110 ℃ for drying for 12h, and roasting at 400 ℃ for 3 h;
(2) preparation of acrylamide-acrylate resin emulsion: dissolving 180mmol of acrylamide and 60mmol of hydroxypropyl acrylate in water to obtain a monomer aqueous solution, heating to 70 ℃ for reaction for 5 hours, dropwise adding an ammonium persulfate aqueous solution (10 mmol based on the mass of ammonium persulfate), carrying out heat preservation reaction after dropwise adding is finished, and finishing the reaction to obtain an acrylamide-acrylate resin emulsion;
(3) preparation of modified acrylamide-acrylic resin: dissolving 10mmol of bromooxime ether in methanol to obtain bromooxime ether solution, adding the bromooxime ether solution into the prepared acrylamide-acrylate resin emulsion, heating to 60 ℃ for reaction for 5 hours, dropwise adding a potassium carbonate aqueous solution (10.5 mmol based on the mass of potassium carbonate), keeping the temperature for reaction after dropwise adding is finished, after the reaction is finished, carrying out reduced pressure distillation to recover the methanol and remove water to obtain modified acrylamide-acrylic resin;
(4) preparation of a pre-immersion liquid: 100g of the pretreated carbon fiber, 85g of the modified acrylamide-acrylic resin prepared above, 8g of nano calcium carbonate, 5g of a silane coupling agent KH560 and 2g of toluene diisocyanate were added to water, and mixed at high speed to obtain a pre-dip solution with a solid content of 60%.
2. Processing of the composite material:
(1) setting a dipping tank, and pouring a pre-dipping solution into the dipping tank;
(2) enabling the basalt fibers to pass through a steeping vat at a constant speed, wherein the steeping time of the basalt fibers in the steeping vat is 25min, and removing redundant pre-steeping liquor through a rubber scraping roller after steeping is finished;
(3) enabling the soaked basalt fibers to pass through a 135 ℃ heat flow drying channel, roasting at the high temperature of 400 ℃ for 2 hours, and cooling to obtain prepreg cloth;
(4) covering with release paper, rolling, and storing.
Example 2
The only difference between example 2 and example 1 is that the impregnation time during processing of the composite material is modified to 15 min.
Comparative example 1
The only difference between comparative example 1 and example 1 is that the modification treatment of step (3) was not carried out at the time of preparation of the pre-dip.
Comparative example 2
The only difference between comparative example 2 and example 1 is that epoxy resin E51 is used as a resin component instead of the modified acrylamide-acrylic resin, dicyandiamide curing agent 100S is used as a curing agent instead of toluene diisocyanate, and toluene is used as a diluent instead of water.
The mechanical strength test was performed on the composite materials of the same specifications as those of the above examples and comparative examples, and the results are shown in Table 1. The tensile strength was tested according to GB/T1447-.
TABLE 1 mechanical Strength of the composites
| Group of | Tensile strength/GPa | Interlaminar shear strength/MPa |
| Example 1 | 3.1 | 297 |
| Example 2 | 2.8 | 243 |
| Comparative example 1 | 2.2 | 151 |
| Comparative example 2 | 1.7 | 106 |
| Basalt fiber | 1.1 | 58 |
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. The preparation method of the special high-performance composite material pre-immersion liquid for aerospace is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
(1) pretreatment of carbon fibers: placing the carbon fiber in an oven for drying, and roasting at high temperature;
(2) preparation of acrylamide-acrylate resin emulsion: dissolving acrylamide and hydroxypropyl acrylate in water to obtain a monomer aqueous solution, heating for reaction, dropwise adding an initiator aqueous solution, carrying out heat preservation reaction after dropwise adding is finished, and obtaining an acrylamide-acrylate resin emulsion after the reaction is finished;
(3) preparation of modified acrylamide-acrylic resin: dissolving bromooxime ether in methanol to obtain bromooxime ether solution, adding the bromooxime ether solution into the prepared acrylamide-acrylate resin emulsion, heating for reaction, dropwise adding an acid-binding agent aqueous solution, carrying out heat preservation reaction after dropwise adding is finished, carrying out reaction, and carrying out reduced pressure distillation to recover methanol and remove water to obtain modified acrylamide-acrylic resin;
(4) preparation of a pre-immersion liquid: and adding the pretreated carbon fibers, the prepared modified acrylamide-acrylic resin, the nano filler, the coupling agent and the curing agent into water, and mixing at a high speed to obtain a pre-immersion liquid with the solid content of 50-80%.
2. The preparation method of the special high-performance composite material pre-immersion liquid for aerospace according to claim 1, wherein the preparation method comprises the following steps: the mol ratio of the acrylamide to the hydroxypropyl acrylate to the bromooxime ether to the acid-binding agent is 5-30:3-10:1: 1.05-1.1.
3. The preparation method of the special high-performance composite material pre-immersion liquid for aerospace according to claim 1, wherein the preparation method comprises the following steps: the initiator aqueous solution is prepared by adding water into ammonium persulfate.
4. The preparation method of the special high-performance composite material pre-immersion liquid for aerospace according to claim 1, wherein the preparation method comprises the following steps: the acid-binding agent solution is prepared by adding water into potassium carbonate.
5. The preparation method of the special high-performance composite material pre-immersion liquid for aerospace according to claim 1, wherein the preparation method comprises the following steps: the mass ratio of the carbon fiber, the modified acrylamide-acrylic resin, the nano filler, the coupling agent and the curing agent is 100:50-100:5-15:1-10: 1-10.
6. The preparation method of the special high-performance composite material pre-immersion liquid for aerospace according to claim 1, wherein the preparation method comprises the following steps: the nano filler is one or more of nano calcium carbonate, nano silicon dioxide, nano aluminum oxide and nano titanium dioxide.
7. The preparation method of the special high-performance composite material pre-immersion liquid for aerospace according to claim 1, wherein the preparation method comprises the following steps: the coupling agent is a silane coupling agent.
8. The preparation method of the special high-performance composite material pre-immersion liquid for aerospace according to claim 1, wherein the preparation method comprises the following steps: the curing agent is polyisocyanate.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105733259A (en) * | 2016-02-19 | 2016-07-06 | 深圳市夸克纳米材料有限公司 | Carbon fiber reinforced polyamide p imide prepreg and preparing method thereof |
| CN105968718A (en) * | 2016-05-20 | 2016-09-28 | 北京化工大学 | Preparation method of carbon fiber/graphene/epoxy resin prepreg and carbon fiber composite material |
| CN108219375A (en) * | 2017-12-31 | 2018-06-29 | 厦门大学 | Surface modified carbon fiber prepreg material based on graphene oxide and preparation method thereof |
| CN108794979A (en) * | 2018-03-29 | 2018-11-13 | 航天材料及工艺研究所 | A kind of high compression-strength and high pressure Lapie's carbon fibre composite and preparation method thereof |
| CN109837740A (en) * | 2017-11-27 | 2019-06-04 | 四川东邦碳纤维材料有限公司 | A kind of surface treatment method of carbon fiber and the carbon fiber of preparation |
| WO2019127992A1 (en) * | 2017-12-29 | 2019-07-04 | 洛阳尖端技术研究院 | Prepreg, composite material, and preparation methods therefor and uses thereof |
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2020
- 2020-06-08 CN CN202010514351.XA patent/CN111808310A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105733259A (en) * | 2016-02-19 | 2016-07-06 | 深圳市夸克纳米材料有限公司 | Carbon fiber reinforced polyamide p imide prepreg and preparing method thereof |
| CN105968718A (en) * | 2016-05-20 | 2016-09-28 | 北京化工大学 | Preparation method of carbon fiber/graphene/epoxy resin prepreg and carbon fiber composite material |
| CN109837740A (en) * | 2017-11-27 | 2019-06-04 | 四川东邦碳纤维材料有限公司 | A kind of surface treatment method of carbon fiber and the carbon fiber of preparation |
| WO2019127992A1 (en) * | 2017-12-29 | 2019-07-04 | 洛阳尖端技术研究院 | Prepreg, composite material, and preparation methods therefor and uses thereof |
| CN108219375A (en) * | 2017-12-31 | 2018-06-29 | 厦门大学 | Surface modified carbon fiber prepreg material based on graphene oxide and preparation method thereof |
| CN108794979A (en) * | 2018-03-29 | 2018-11-13 | 航天材料及工艺研究所 | A kind of high compression-strength and high pressure Lapie's carbon fibre composite and preparation method thereof |
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