CN111777843A - Preparation method of carbon fiber epoxy resin-based composite insulating material - Google Patents
Preparation method of carbon fiber epoxy resin-based composite insulating material Download PDFInfo
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- CN111777843A CN111777843A CN202010628438.XA CN202010628438A CN111777843A CN 111777843 A CN111777843 A CN 111777843A CN 202010628438 A CN202010628438 A CN 202010628438A CN 111777843 A CN111777843 A CN 111777843A
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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
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
- C08L63/10—Epoxy resins modified by unsaturated compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D263/00—Heterocyclic compounds containing 1,3-oxazole or hydrogenated 1,3-oxazole rings
- C07D263/52—Heterocyclic compounds containing 1,3-oxazole or hydrogenated 1,3-oxazole rings condensed with carbocyclic rings or ring systems
- C07D263/54—Benzoxazoles; Hydrogenated benzoxazoles
- C07D263/58—Benzoxazoles; Hydrogenated benzoxazoles with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 2
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- C—CHEMISTRY; METALLURGY
- 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
- C08G59/40—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 curing agents used
- C08G59/50—Amines
- C08G59/5046—Amines heterocyclic
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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
- 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
- C08J2363/10—Epoxy resins modified by unsaturated compounds
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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
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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Abstract
The invention discloses a preparation method of a carbon fiber epoxy resin-based composite insulating material, which relates to the technical field of composite materials, and prepares a novel epoxy resin curing agent, wherein the curing agent not only can realize the curing of epoxy resin, but also can endow a resin matrix with good insulating property; and the insulating property of the resin matrix is further optimized by the matching use of the insulating filler in the dipping solution, so that the finally prepared composite material has excellent insulating property, the problem of good carbon fiber conductivity is solved, and the application range of the carbon fiber reinforced epoxy resin composite material is expanded.
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 carbon fiber epoxy resin based composite insulating material.
Background art:
in a broad sense, composite material refers to a material composed of two or more components (units) of different properties or different textures. The components of the composite material are divided into a matrix and a reinforcement, and the component continuously distributed in the matrix is generally called a matrix, such as a polymer (resin) matrix, a metal matrix and a ceramic matrix; the substance in which fibers, particles, whiskers, or the like are dispersed in a matrix is called a reinforcement.
In the 21 st century, the development and application of Advanced Composite Materials (ACM) will enter a rapid development period, and therefore the development of reinforcements for composite materials is very important. All components that have the functions of improving strength and improving performance in the polymer matrix composite material can be called reinforcing materials. The varieties of the novel fibrous reinforcing materials for the composite material taking the epoxy resin as the matrix are as follows: glass fibers, carbon fibers, ultra-high relative molecular mass polyethylene fibers, polyaramid (aramid) fibers, PBO fibers, boron fibers, and the like.
A specialty fiber consisting of carbon. The graphite fiber has the characteristics of high temperature resistance, friction resistance, electric conduction, heat conduction, corrosion resistance and the like, is fibrous and soft in appearance, can be processed into various fabrics, and has high strength and modulus along the fiber axis direction due to the preferred orientation of the graphite microcrystalline structure along the fiber axis. The carbon fibers have a low density and thus a high specific strength and a high specific modulus. The carbon fiber is mainly used as a reinforcing material to be compounded with resin, metal, ceramic, carbon and the like to manufacture an advanced composite material. The specific strength and the specific modulus of the carbon fiber reinforced epoxy resin composite material are the highest in the existing engineering materials.
The carbon fiber epoxy resin-based composite insulating material is prepared by combining resin with insulating property and the carbon fiber through an impregnation method, so that the prepared composite material has the dual characteristics of the carbon fiber and the resin.
The invention content is as follows:
the technical problem to be solved by the invention is to provide a preparation method of a carbon fiber epoxy resin matrix composite insulating material, which endows a resin matrix with excellent insulating property through the preparation of an insulating curing agent and the addition of an insulating filler, thereby solving the problem of good conductivity of carbon fibers and expanding the application range of the carbon fiber epoxy resin matrix composite material.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a preparation method of a carbon fiber epoxy resin based composite insulating material comprises the following preparation steps:
(1) adding 2-aminobenzoxazole-7-boric acid, 1, 5-dibromo-3-pentanone and a catalyst into a mixed solvent of dioxane and water, stirring, refluxing, reacting, cooling to room temperature after the reaction is finished, removing the solvent, adding methanol for dissolving, recrystallizing and drying to obtain an insulating curing agent;
(2) adding the insulating filler, the insulating curing agent, the film forming agent and the defoaming agent which are calcined at high temperature into the waterborne epoxy acrylic emulsion, and adding water to adjust the solid content to obtain a gum dipping solution:
(3) the carbon fiber cloth is treated by dipping solution and heated and cured to obtain prepreg;
(4) and cutting the prepreg, stacking the cut prepreg into a plurality of layers, and placing the layers in a hot press for pressing to obtain the carbon fiber epoxy resin based composite insulating material.
The catalyst is tetrakis (triphenylphosphine) palladium.
The molar ratio of the 2-aminobenzoxazole-7-boric acid to the 1, 5-dibromo-3-pentanone to the catalyst is 1:1: 1-5%.
The mass ratio of the waterborne epoxy acrylic emulsion to the insulating filler to the insulating curing agent to the film forming agent to the defoaming agent is 80-130:10-30:5-20:1-10: 1-10.
The solid content of the waterborne epoxy acrylic emulsion is 40-60%.
The insulating filler is one or a mixture of sepiolite powder and kaolin, and the high-temperature calcination temperature is 400-600 ℃.
The film forming agent is an alcohol ether solvent.
The defoaming agent is a polysiloxane defoaming agent.
The dipping time of the carbon fiber cloth in the dipping solution is 5-30 min.
The temperature of the heating curing is 145-155 ℃, and the time is 0.5-2 h.
The pressure of the pressing is 2-4MPa, the temperature is 150-180 ℃, and the time is 5-30 min.
1. The aqueous epoxy acrylic emulsion is used as a resin component to prepare the aqueous dipping solution, so that the problem of environmental pollution caused by volatilization of an organic solvent in the process of dissolving the resin by the organic solvent is solved.
2. The insulating curing agent with dual functions of curing resin and reinforcing the insulating property of the resin is prepared by using 2-aminobenzoxazole-7-boric acid and 1, 5-dibromo-3-pentanone, but the conventional curing agent in the field only has the function of curing the resin and cannot obtain the technical effect of reinforcing the insulating property of the resin.
3. According to the invention, the insulating filler is added into the dipping solution, the sepiolite powder, the calcined kaolin and the asbestos powder have insulating properties, and the insulating properties of the resin matrix can be enhanced by taking the sepiolite powder, the calcined kaolin and the asbestos powder as the insulating filler, so that the insulating properties of the prepared composite material are optimized.
4. In the invention, the dipping solution is dipped and attached to the carbon fiber cloth, and then a resin layer is formed on the carbon fiber cloth after curing, and the resin layer has excellent insulating property, thereby solving the problem of carbon fiber conductivity, and enabling the prepared composite material to be applied to the technical field with requirements on insulating property.
5. The invention realizes the compounding of the multilayer prepreg through hot pressing and ensures the firm bonding between the adjacent prepregs.
Although the addition of the insulating filler can optimize the insulating property of the resin matrix, the blending compatibility and the water dispersibility of the insulating filler and the resin are poor, and the insulating filler and the resin are difficult to uniformly disperse in the dipping solution, so the dipping solution needs to be stirred and uniformly mixed before dipping, otherwise, the aggregation of the insulating filler is caused, and the insulating property of the finally prepared composite material is influenced. Aiming at the problem, the invention carries out modification treatment on the insulating filler, so that the modified insulating filler can be uniformly dispersed in the dipping solution, and meanwhile, the modified insulating filler has good blending compatibility with resin.
The technical problem to be solved by the invention can also be realized by adopting the following technical scheme:
a preparation method of a carbon fiber epoxy resin based composite insulating material comprises the following preparation steps:
(1) adding 2-aminobenzoxazole-7-boric acid, 1, 5-dibromo-3-pentanone and a catalyst into a mixed solvent of dioxane and water, stirring, refluxing, reacting, cooling to room temperature after the reaction is finished, removing the solvent, adding methanol for dissolving, recrystallizing and drying to obtain an insulating curing agent;
(2) adding an insulating filler into water, stirring to completely wet the insulating filler, adding polyethylene glycol, heating to reflux, keeping the temperature, stirring, filtering, drying filter residues, calcining at high temperature, and crushing into powder to obtain a water-dispersible insulating filler;
(3) adding a water-dispersible insulating filler, an insulating curing agent, a film-forming agent and a defoaming agent into the waterborne epoxy acrylic emulsion, and adding water to adjust the solid content to obtain a gum dipping solution:
(4) the carbon fiber cloth is treated by dipping solution and heated and cured to obtain prepreg;
(5) and cutting the prepreg, stacking the cut prepreg into a plurality of layers, and placing the layers in a hot press for pressing to obtain the carbon fiber epoxy resin based composite insulating material.
The mass ratio of the insulating filler to the polyethylene glycol is 1-10: 5-20.
The control parameters of the other steps are completely the same as the technical scheme.
Hydrogen bonds are formed between hydroxyl groups in the polyethylene glycol structure and active hydroxyl groups on the surfaces of the sepiolite and the kaolin, the sepiolite and the kaolin are dispersed into particles, the sepiolite and the kaolin are converted into nano-sized powder after high-temperature calcination, and the intermolecular repulsive force is increased, so that the blending compatibility of the sepiolite and the kaolin with a resin matrix and the dispersibility of the sepiolite and the kaolin in water are improved.
The invention has the beneficial effects that: the novel epoxy resin curing agent is prepared, and not only can the curing of epoxy resin be realized, but also the resin matrix can be endowed with good insulating property; and the insulating property of the resin matrix is further optimized by the matching use of the insulating filler in the dipping solution, so that the finally prepared composite material has excellent insulating property, the problem of good carbon fiber conductivity is solved, and the application range of the carbon fiber reinforced epoxy resin composite material is expanded.
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.
Carbon fiber cloth was purchased from 3k carbon fiber cloth of chiben composites, inc.
The water-based epoxy acrylic emulsion is purchased from Anhui formal coating new materials Co., Ltd, has a solid content of 46% +/-1% and a pH value of 7-8.
The sepiolite powder was obtained from 300 mesh clay-like sepiolite powder from Shijiazhuan Tianyuan mining Co.
Example 1
(1) Adding 50mmol of 2-aminobenzoxazole-7-boric acid, 50mmol of 1, 5-dibromo-3-pentanone and 2mmol of tetrakis (triphenylphosphine) palladium into a mixed solvent of 200mL of dioxane and 100mL of water, stirring, refluxing, reacting for 8 hours, cooling to room temperature after the reaction is finished, removing the solvent, adding 100mL of methanol for dissolving, recrystallizing and drying to obtain the insulating curing agent.1H NMR(DMSO-d6,400MHz),:7.74(s,4H),7.49-7.35(m,6H),2.81-2.78(m,8H)；ESI-MS:m/z＝351.14[M+1]+.
(2) Adding 25g of sepiolite powder calcined at the high temperature of 550 ℃ for 3 hours, 18g of insulating curing agent, 2g of propylene glycol butyl ether and 1g of polysiloxane defoaming agent DQ-N139 into 100g of waterborne epoxy acrylic emulsion, and adding water to adjust the solid content to 55% to obtain a gum dipping solution.
(3) And (2) allowing the carbon fiber cloth to pass through a dipping solution, wherein the dipping time of the carbon fiber cloth in the dipping solution is 15min, and heating to 150 ℃ for curing for 1h to obtain the prepreg.
(4) And cutting the prepreg, stacking the cut prepreg into five layers, and pressing the five layers in a hot press at the pressure of 3MPa and the temperature of 160 ℃ for 20min to obtain the carbon fiber epoxy resin-based composite insulating material.
Example 2
(1) Adding 50mmol of 2-aminobenzoxazole-7-boric acid, 50mmol of 1, 5-dibromo-3-pentanone and 2mmol of tetrakis (triphenylphosphine) palladium into a mixed solvent of 200mL of dioxane and 100mL of water, stirring, refluxing, reacting for 8 hours, cooling to room temperature after the reaction is finished, removing the solvent, adding 100mL of methanol for dissolving, recrystallizing and drying to obtain the insulating curing agent.
(2) 30g of kaolin calcined at the high temperature of 550 ℃ for 3 hours, 18g of insulating curing agent, 2g of propylene glycol butyl ether and 1g of polysiloxane defoaming agent DQ-N139 are added into 100g of waterborne epoxy acrylic emulsion, and water is added to adjust the solid content to 55 percent to obtain the gum dipping solution.
(3) And (2) allowing the carbon fiber cloth to pass through a dipping solution, wherein the dipping time of the carbon fiber cloth in the dipping solution is 15min, and heating to 150 ℃ for curing for 1h to obtain the prepreg.
(4) And cutting the prepreg, stacking the cut prepreg into five layers, and pressing the five layers in a hot press at the pressure of 4MPa and the temperature of 160 ℃ for 20min to obtain the carbon fiber epoxy resin-based composite insulating material.
Example 3
The insulating filler of example 1 was modified, and the rest was the same as example 1.
(1) Adding 50mmol of 2-aminobenzoxazole-7-boric acid, 50mmol of 1, 5-dibromo-3-pentanone and 2mmol of tetrakis (triphenylphosphine) palladium into a mixed solvent of 200mL of dioxane and 100mL of water, stirring, refluxing, reacting for 8 hours, cooling to room temperature after the reaction is finished, removing the solvent, adding 100mL of methanol for dissolving, recrystallizing and drying to obtain the insulating curing agent.
(2) Adding 10g of sepiolite powder into water, stirring to completely wet the insulating filler, adding 10g of polyethylene glycol 400, heating to reflux, keeping the temperature, stirring for 3 hours, filtering, drying filter residues, calcining at 550 ℃ for 3 hours, crushing into powder, and sieving with a 300-mesh sieve to obtain the water-dispersible sepiolite powder.
(3) Adding 25g of water-dispersible sepiolite powder, 18g of insulating curing agent, 2g of propylene glycol butyl ether and 1g of polysiloxane defoaming agent DQ-N139 into 100g of waterborne epoxy acrylic emulsion, and adding water to adjust the solid content to 55% to obtain a gum dipping solution.
(4) And (2) allowing the carbon fiber cloth to pass through a dipping solution, wherein the dipping time of the carbon fiber cloth in the dipping solution is 15min, and heating to 150 ℃ for curing for 1h to obtain the prepreg.
(5) And cutting the prepreg, stacking the cut prepreg into five layers, and pressing the five layers in a hot press at the pressure of 3MPa and the temperature of 160 ℃ for 20min to obtain the carbon fiber epoxy resin-based composite insulating material.
Comparative example 1
The curing agent in example 1 was replaced with dicyandiamide, and the rest was the same as in example 1.
Comparative example 2
The curing agent in example 1 was replaced with m-phenylenediamine, and the rest was the same as in example 1.
The volume resistivity of the carbon fiber epoxy resin matrix composite insulating material prepared by the volume resistivity is tested according to the national standard GB/T1410-2006 volume resistivity and surface resistivity test method of the solid insulating material, and the test result is shown in Table 1.
TABLE 1
| Test items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
| Volume resistivity omega cm | 4.7×1012 | 5.3×1012 | 8.6×1012 | 3.5×109 | 4.1×109 |
As can be seen from Table 1, compared with the existing common curing agents dicyandiamide and m-phenylenediamine, the insulation curing agent of the invention can improve the insulation performance of the prepared carbon fiber epoxy resin matrix composite insulation material, and the insulation performance of the prepared carbon fiber epoxy resin matrix composite insulation material can also be improved by modifying the insulation filler.
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 (10)
1. A preparation method of a carbon fiber epoxy resin based composite insulating material is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
(1) adding 2-aminobenzoxazole-7-boric acid, 1, 5-dibromo-3-pentanone and a catalyst into a mixed solvent of dioxane and water, stirring, refluxing, reacting, cooling to room temperature after the reaction is finished, removing the solvent, adding methanol for dissolving, recrystallizing and drying to obtain an insulating curing agent;
(2) adding the insulating filler, the insulating curing agent, the film forming agent and the defoaming agent which are calcined at high temperature into the waterborne epoxy acrylic emulsion, and adding water to adjust the solid content to obtain a gum dipping solution:
(3) the carbon fiber cloth is treated by dipping solution and heated and cured to obtain prepreg;
(4) and cutting the prepreg, stacking the cut prepreg into a plurality of layers, and placing the layers in a hot press for pressing to obtain the carbon fiber epoxy resin based composite insulating material.
2. The method for preparing the carbon fiber epoxy resin-based composite insulating material according to claim 1, characterized in that: the catalyst is tetrakis (triphenylphosphine) palladium.
3. The method for preparing the carbon fiber epoxy resin-based composite insulating material according to claim 1, characterized in that: the molar ratio of the 2-aminobenzoxazole-7-boric acid to the 1, 5-dibromo-3-pentanone to the catalyst is 1:1: 1-5%.
4. The method for preparing the carbon fiber epoxy resin-based composite insulating material according to claim 1, characterized in that: the mass ratio of the waterborne epoxy acrylic emulsion to the insulating filler to the insulating curing agent to the film forming agent to the defoaming agent is 80-130:10-30:5-20:1-10: 1-10.
5. The method for preparing the carbon fiber epoxy resin-based composite insulating material according to claim 1, characterized in that: the solid content of the waterborne epoxy acrylic emulsion is 40-60%.
6. The method for preparing the carbon fiber epoxy resin-based composite insulating material according to claim 1, characterized in that: the insulating filler is one or a mixture of sepiolite powder and kaolin, and the high-temperature calcination temperature is 400-600 ℃.
7. The method for preparing the carbon fiber epoxy resin-based composite insulating material according to claim 1, characterized in that: the film forming agent is an alcohol ether solvent, and the defoaming agent is a polysiloxane defoaming agent.
8. The method for preparing the carbon fiber epoxy resin-based composite insulating material according to claim 1, characterized in that: the dipping time of the carbon fiber cloth in the dipping solution is 5-30 min.
9. The method for preparing the carbon fiber epoxy resin-based composite insulating material according to claim 1, characterized in that: the temperature of the heating curing is 145-155 ℃, and the time is 0.5-2 h.
10. The method for preparing the carbon fiber epoxy resin-based composite insulating material according to claim 1, characterized in that: the pressure of the pressing is 2-4MPa, the temperature is 150-180 ℃, and the time is 5-30 min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010628438.XA CN111777843A (en) | 2020-07-02 | 2020-07-02 | Preparation method of carbon fiber epoxy resin-based composite insulating material |
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| CN202010628438.XA CN111777843A (en) | 2020-07-02 | 2020-07-02 | Preparation method of carbon fiber epoxy resin-based composite insulating material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114957741A (en) * | 2021-12-29 | 2022-08-30 | 江苏志纤复能科技有限公司 | Novel low-temperature co-curing high-damping composite material and preparation method thereof |
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2020
- 2020-07-02 CN CN202010628438.XA patent/CN111777843A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114957741A (en) * | 2021-12-29 | 2022-08-30 | 江苏志纤复能科技有限公司 | Novel low-temperature co-curing high-damping composite material and preparation method thereof |
| CN114957741B (en) * | 2021-12-29 | 2024-01-02 | 江苏志纤复能科技有限公司 | Low-temperature co-cured high-damping composite material and preparation method thereof |
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