CN112961470A - Halogen-free flame-retardant high-strength tension-torsion plate for wind power and preparation method thereof - Google Patents
Halogen-free flame-retardant high-strength tension-torsion plate for wind power and preparation method thereof Download PDFInfo
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- CN112961470A CN112961470A CN202110180288.5A CN202110180288A CN112961470A CN 112961470 A CN112961470 A CN 112961470A CN 202110180288 A CN202110180288 A CN 202110180288A CN 112961470 A CN112961470 A CN 112961470A
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- Reinforced Plastic Materials (AREA)
Abstract
The invention discloses a halogen-free flame-retardant high-strength tension-torsion plate for wind power and a preparation method thereof, and the method is characterized in that: the tension-torsion plate is a composite material prepared by curing and molding overlapped halogen-free flame-retardant high-strength resin fiber cloth prepreg at the temperature of 175-215 ℃; the halogen-free flame-retardant high-strength resin fiber cloth prepreg is a fiber impregnation material which is formed by coating a fiber fabric with a halogen-free flame-retardant high-strength resin adhesive through a gluing machine and then baking the fiber fabric; the halogen-free flame-retardant high-strength resin adhesive is prepared by mixing epoxy resin, modified resin A, modified resin B, a toughening agent, a curing agent, a filler, a solvent and an accelerator. The tensile strength of the tension-torsion plate in the axial direction is more than or equal to 520MPa, the shear strength in the axial direction is more than or equal to 45MPa, the temperature resistance is more than or equal to 150 ℃, and the halogen-free flame retardance reaches V-0; the connecting rod is suitable for being used in the megawatt cascade shaft connector connecting rod in wind energy, large engineering machinery and other industries on modern land, sea and the like.
Description
Technical Field
The invention belongs to a tension-torsion plate for wind power, and relates to a halogen-free flame-retardant high-strength tension-torsion plate for wind power and a preparation method thereof. The tension-torsion plate for the halogen-free flame-retardant high-strength wind power (wind power is a wind generating set) is suitable for being used as a connecting rod of a megawatt cascade shaft coupler in wind energy such as modern land, sea and the like, large engineering machinery and other industries, and is particularly suitable for being used as a buffer component for connecting a coupling and a driving bearing and a driven bearing in a connecting rod type coupling of the wind generating set.
Background
The coupling is used as a key stressed part in a transmission system of the wind generating set and has important functions of connecting a high-speed shaft of a gear box and a generator shaft, transmitting power, buffering and damping, shaft system fault tolerance, electric insulation, moment overload protection and the like. At present, the global economy is rapidly developed and the energy is increasingly deficient, and new energy represented by wind power, solar photovoltaic, biological power generation, geothermal power generation, tidal power generation and the like is rapidly rising. In order to adapt to the rapid development of various new energy sources, power distribution and control systems in various electric equipment, particularly wind power generation equipment, are developing towards continuous functionalization and complication, so that the connecting rod coupling matched with the power distribution and control system is required to be lighter, high in performance and more convenient to use and maintain.
Based on this, it has become a trend of industry to replace the original metal and rubber connecting rod coupling with the composite material pulling and twisting plate. The composite tension-torsion plate has the advantages of both a metal disc coupling and a rubber elastic coupling, has high deviation correction capability, high torsional rigidity and overlong service life, does not need maintenance, enables the composite connecting rod coupling to become the best choice of a wind field, is particularly suitable for megawatt-level offshore application, and has the highest working power of 7 MW. Therefore, the novel connecting rod coupling is required to have more excellent comprehensive performance, and particularly, the requirements on tensile strength, halogen-free flame retardance and the like are more severe.
The existing general insulating composite materials (insulating support parts, insulating structural parts, plates and the like) usually need to be added with inorganic powder accounting for 30-50% of the total weight of resin solids to achieve the flame retardant effect (such as V-0 grade and V-1 grade) due to different requirements on the flame retardant effect; in order to solve the problem of high mechanical strength (usually, tensile strength is 520MPa to 657MPa), rubber, phenolic tough resin, inorganic powder accounting for 15 percent to 35 percent of the total weight of resin solids and the like are usually added into matrix resin to improve the tensile strength and the torsional strength of the whole composite material.
In the prior art, the coupler is mostly a pure metal part, and the coupler has the problems of poor fatigue resistance and vibration isolation damping performance, great total weight, easy corrosion, difficult maintenance and replacement, and directly influences the service life of the whole unit. At present, couplings made of high polymer rubber are rarely used, the strength of rubber is poor, the rubber is easy to age, the breakage rate is high, the maintenance and material cost required during use is high, and the basic requirements of modern wind power generation on continuity and high efficiency cannot be met, so that the couplings are not popularized and used all the time.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a halogen-free flame-retardant high-strength tension-torsion plate for wind power and a preparation method thereof. The invention adopts an epoxy composite material, and provides a halogen-free flame-retardant high-strength tension-torsion plate for wind power and a preparation method thereof, wherein the tension-torsion plate has the advantages of high tensile strength of 520 MPa-657 MPa, shear strength of 45 MPa-63 MPa, temperature resistance of more than or equal to 150 ℃, halogen-free flame retardant UL94V-0 level and good performance.
The content of the invention is as follows: the utility model provides a do not have fire-retardant high strength wind-powered electricity generation and use board that turns round which characterized by: the tension-torsion plate is a composite material prepared by curing and molding overlapped halogen-free flame-retardant high-strength resin fiber cloth prepreg (or called halogen-free flame-retardant high-strength resin fiber fabric prepreg) at the temperature of 175-215 ℃;
the halogen-free flame-retardant high-strength resin fiber cloth prepreg is a fiber impregnating material which is formed by coating halogen-free flame-retardant high-strength resin adhesive on a fiber fabric through a gluing machine and then baking the fiber fabric, wherein the impregnating material comprises the following components in percentage by weight: 25-48% of resin semi-cured substance and 52-75% of fiber fabric;
the halogen-free flame-retardant high-strength resin adhesive is prepared by mixing 17-31 parts by weight of epoxy resin, 6-18 parts by weight of modified resin A, 9-21 parts by weight of modified resin B, 3-24 parts by weight of toughening agent, 3-14 parts by weight of curing agent, 5-12 parts by weight of filler, 12-26 parts by weight of solvent and 0.01-0.1 part by weight of accelerator;
the epoxy resin is bisphenol A type epoxy resin [ product production providing enterprises and brands can be: south Asia epoxy resins (Kunshan) Limited, Dow DER-383, Nantong star E-51, Baling petrochemical CYD-128, etc. ], o-cresol novolac epoxy resins [ product manufacturing and providing enterprises and brands may be: NPCN-704/703 from south asian epoxy resin (kunshan) co., ltd, 704# from mayao baihong new materials co., ltd, etc.), phenol novolac epoxy resin [ product production providing company and brand may be: NPPN-638S of south Asia epoxy resin (Kun mountain) Limited, EPON 154 of the American vast New materials group, PFNE77500 of Hunan Jiangsheng materials science and technology Limited, etc.), resorcinol type epoxy resin (the product production providing enterprises and brands may be ERISYS RDGE-H of the Jia Di Da chemical Limited, Shenzhen, YF-554 of the Guangzhou Yifu chemical materials Limited, etc.), biphenyl type novolac epoxy resin (the product production providing enterprises and brands may be BPNE3501LL/9781 of the Hunan Jiangsheng materials science and technology Limited, etc.), and dicyclopentadiene type polycondensation resin epoxy resin (the product production providing enterprises and brands may be DNE260S of the Changchun resin factory, DPNE1501 of the Hunan Jiangsheng materials Limited, etc.);
the modified resin A is one or a mixture of more than two of phosphorus-containing epoxy resin (the product production providing enterprises and brands can be EP0-101 of Guangzhou Qiaoan chemical industry Co., Ltd., D201/202 self-made by Sichuan east Material science and technology group Co., Ltd.), phosphorus-containing phenolic resin (the product production providing enterprises and brands can be DOW92741 of Dow chemical, D992 self-made by Sichuan east Material science and technology group Co., Ltd.), and phenoxy cyclophosphazene compound (the product production providing enterprises and brands can be Jiangsu Aikang biological medicine HPCTP, Japanese great halogen-free flame retardant SPB-100, Jianghu Hongkong jin Punjiu chemical DOPO-HQ, etc.); wherein: the molecular structure of the phenoxy cyclophosphazene compound is shown as the following formula:
the modified resin B is one or a mixture of two of bismaleimide resin (the product production providing enterprise and brand can be SK bismaleimide resin of Shangzhou new material Co., Ltd, the bismaleimide resin of Huizhou electronic insulation material Co., Ltd, HT280 bismaleimide resin of highland new material science Co., Ltd, etc.), nitrile resin (the product production providing enterprise and brand can be B-type nitrile resin, etc. produced by A Co., Ltd), boron phenolic resin (the product production providing enterprise and brand can be FB resin of Tianyu high temperature resin material Co., Ltd, etc.; Anodont);
the curing agent is one or a mixture of two of 4, 4-diaminodiphenylmethane, 4-diaminodiphenyl sulfone and dicyandiamide; the filler is one or a mixture of two of nano montmorillonite, nano vermiculite, nano silicon dioxide, nano aluminum hydroxide, nano aluminum oxide and carbon nano tubes; the accelerant is any one of 2-methylimidazole, 2-ethyl-4-methylimidazole, N-dimethylbenzylamine, boron trifluoride ethylamine and aluminum acetylacetonate;
the toughening agent is LCI and LCEUPPGAnd MPEPEB, the molecular structural formula of which is shown as the following formula:
the invention comprises the following steps: the fiber fabric is one or a combination of two of alkali-free glass fiber checkered cloth, alkali-free glass fiber twill cloth, carbon fiber checkered cloth and basalt fiber checkered cloth.
The invention comprises the following steps: the solvent is one or a mixture of more than two of toluene, xylene, ethylene glycol, methyl ethyl ketone, cyclohexanone, butanone, acetone, N-dimethylformamide and ethanol.
The invention comprises the following steps: the tensile strength of the tension-torsion plate in the axial direction is more than or equal to 520MPa, the shear strength in the axial direction is more than or equal to 45MPa, the temperature resistance is more than or equal to 150 ℃, and the halogen-free flame retardance reaches V-0.
Another aspect of the invention is: the preparation method of the halogen-free flame-retardant high-strength tension-torsion plate for the wind power is characterized by comprising the following steps of:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) preparing materials: taking raw materials of 17-31 parts by weight of epoxy resin, 6-18 parts by weight of modified resin A, 9-21 parts by weight of modified resin B, 3-24 parts by weight of toughening agent, 3-14 parts by weight of curing agent, 5-12 parts by weight of filler, 0.01-0.1 part by weight of accelerator and 12-26 parts by weight of solvent;
the epoxy resin is bisphenol A type epoxy resin [ product production providing enterprises and brands can be: south Asia epoxy resin (Kunshan) Limited, American Dow DER-383, Nantong star E-51, and Baling petrochemical CYD-128, and the like, and the same later, o-cresol type novolac epoxy resin [ product production providing enterprises and brands can be: NPCN-704/703 from south asia epoxy resin (kunshan) co., 704# from maja-hong new materials co., ltd., the same shall apply later ], phenol novolac epoxy resin [ product production providing enterprises and brands may be: NPPN-638S of south Asia epoxy resin (Kun mountain) Inc., EPON 154 of the national Vast Mi high New materials group, PFNE77500 of Hunan Jiasheng materials science and technology Inc., the latter, resorcinol type epoxy resin (product production providing enterprises and brands can be ERISYS RDGE-H of Shenzhen Jia Dida chemical engineering Limited, YF-554 of Guangzhou Yifu chemical engineering Limited, the latter, the same), biphenyl type phenolic epoxy resin (product production providing enterprises and brands can be BPNE3501LL/9781 of Hunan Jiasheng material science and technology Limited, the latter, the same) and epoxy resin of dicyclopentadiene type polycondensation resin (product production providing enterprises and brands can be DNE260S of Taiwan Changchun factory, DP1501 of Hunan Jiasheng material science and technology Limited, the latter, the same);
the modified resin A is one or a mixture of more than two of phosphorus-containing epoxy resin (the product production providing enterprises and brands can be EP0-101 of Kyowa Qiaan chemical engineering Co., Ltd., D201/202 self-made by Sichuan east Material science and technology group Co., Ltd., the same later), phosphorus-containing phenolic resin (the product production providing enterprises and brands can be DOW92741 of Tao chemical, D992 self-made by Sichuan east Material science and technology group Co., Ltd., the same later), and phenoxy cyclophosphazene compound (the product production providing enterprises and brands can be Jiangsu Aikang biological medicine HPCTP, Japan big halogen-free flame retardant SPB-100, Jiangsu Hongyun chemical DOPO-HQ, the later same later); wherein: the molecular structure of the phenoxy cyclophosphazene compound is shown as the following formula (the same applies to the specification):
the modified resin B is one or a mixture of two of bismaleimide resin (the product production providing enterprise and brand can be SK bismaleimide resin of Shangzhou new material Co., Ltd, the bismaleimide resin of Huizhou electronic insulation material Co., Ltd, HT280 bismaleimide resin of highland new material science Co., Ltd, etc.), nitrile resin (the product production providing enterprise and brand can be B-type nitrile resin, etc. produced by A Co., Ltd), boron phenolic resin (the product production providing enterprise and brand can be FB resin of Tianyu high temperature resin material Co., Ltd, etc.; Anodont);
the curing agent is one or a mixture of two of 4, 4-diaminodiphenylmethane, 4-diaminodiphenyl sulfone and dicyandiamide; the filler is one or a mixture of two of nano montmorillonite, nano vermiculite, nano silicon dioxide, nano aluminum hydroxide, nano aluminum oxide and carbon nano tubes; the accelerant is any one of 2-methylimidazole, 2-ethyl-4-methylimidazole, N-dimethylbenzylamine, boron trifluoride ethylamine and aluminum acetylacetonate;
the toughening agent is LCI and LCEUPPGAnd MPEPEB, the molecular structure of which is shown as the following formula (the same applies hereinafter):
(b) adding epoxy resin, modified resin B, toughening agent and solvent (the solvent amount can be 30-70% of the total weight of the solvent) into a glue preparation tank, stirring for 6-24 hours at 50-65 ℃ (constant temperature), adding filler and solvent (namely the rest solvent), stirring for 0.5-3 hours at 50-75 ℃ (constant temperature), adding modified resin A, stirring for 0.5-1.5 hours at 55-85 ℃ (constant temperature), continuing to add curing agent and accelerant, stirring for 0.25-1 hour at 60-75 ℃ (constant temperature), adjusting the forming time of glue solution, sampling, testing the forming time of the glue solution by using a knife method, and preparing the halogen-free flame-retardant high-strength resin adhesive when the forming time is 462-617 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber cloth prepreg:
coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 1-10 m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber cloth prepreg;
c. pressing a tension-torsion plate:
taking halogen-free flame-retardant high-strength resin fiber cloth prepreg according to the required size (same as the prior art) required by the pressing process of the tension-torsion plate, flatly placing the halogen-free flame-retardant high-strength resin fiber cloth prepreg in a mold with the temperature controlled at 135-155 ℃, closing the mold, and carrying out hot baking, curing and molding for 5-26 h under the conditions of the temperature controlled at 185-215 ℃ and the pressure controlled at 20-23 MPa to obtain the tension-torsion plate.
In another aspect of the invention: in the step b, the fiber fabric is one or a combination of two of alkali-free glass fiber checkered cloth, alkali-free glass fiber twill cloth, carbon fiber checkered cloth and basalt fiber checkered cloth.
In another aspect of the invention: in the step a, the solvent is one or a mixture of more than two of toluene, xylene, ethylene glycol, methyl ethyl ketone, cyclohexanone, butanone, acetone and ethanol.
In another aspect of the invention: and c, the prepared tension-torsion plate has the axial tensile strength of more than or equal to 520MPa, the axial shear strength of more than or equal to 45MPa, the temperature resistance of more than or equal to 150 ℃, and the halogen-free flame retardance reaching V-0.
Compared with the prior art, the invention has the following characteristics and beneficial effects:
(1) the invention adopts liquid crystal polymer to toughen and modify matrix resin by a crack nail anchoring mechanism, so that the toughness (tensile strength is more than or equal to 520MPa) of the integral composite material is greatly improved on the basis of ensuring that the compressive strength is more than or equal to 230 MPa;
(2) the invention adopts the resin and filler synergistic flame retardant technology, so that on the basis of reaching the temperature resistance of more than or equal to 150 ℃ (the strength retention rate is more than or equal to 50% at 150 ℃), the tensile strength is more than or equal to 520MPa, and particularly in the aspect of flame retardant performance, the technical problem of non-halogenated V-0 level flame retardant which cannot be achieved by only a small amount of inorganic powder (the inorganic powder only accounts for 6.17-8.22% of the resin solids) is solved, and the production cost of the product is greatly reduced;
(3) the composite material tension-torsion plate is a special insulating composite material which is formed by impregnating high-strength fiber fabrics with epoxy resin glue solution and heating and curing, has excellent tensile property and halogen-free flame retardance, and has the characteristics of light weight, high strength and corrosion resistance compared with metal and rubber couplings; the tensile strength of the tension-torsion plate in the axial direction is more than or equal to 520MPa (the tensile strength is 520 MPa-657 MPa), the shear strength in the axial direction is more than or equal to 45MPa (the shear strength is 45 MPa-63 MPa), the temperature resistance is more than or equal to 150 ℃, and the halogen-free flame retardance reaches V-0; can become a high-quality insulating composite material for tension-torsion overload protection in industries such as modern wind energy, large-scale engineering machinery and the like;
(4) the integral process for preparing the tension-torsion plate is simple, the operation is easy, the product has good dimensional stability and excellent quality, the requirements of high-strength, high-toughness, temperature-resistant and halogen-free flame-retardant composite material structural members in the insulation support protection field in the industries of wind energy, large engineering machinery and the like on modern land, sea and the like are met, and the tension-torsion plate has obvious practical use value and application prospect and strong practicability.
Drawings
Fig. 1 is a schematic diagram of a structure of a halogen-free flame-retardant high-strength tension-torsion plate for wind power according to the embodiment of the invention.
Detailed Description
The following examples are intended to further illustrate the present invention and should not be construed as limiting the scope of the invention, which is intended to be covered by the claims appended hereto.
The amounts of each ingredient component material in the following examples are in parts by weight (e.g., grams or kilograms).
Preparation of the first part of halogen-free flame-retardant high-strength resin adhesive
Example 1-1:
respectively adding 21 parts of o-cresol novolac epoxy resin, 9 parts of bismaleimide resin, 7 parts of LCI and 8 parts of acetone into a glue preparation tank, stirring for 7 hours at 55 ℃, adding 7 parts of nano silicon dioxide and 5 parts of butanone, stirring for 1 hour at 50 ℃, adding 11 parts of phosphorus-containing epoxy resin, stirring for 0.75 hour at 75 ℃, adding 12 parts of 4, 4-diaminodiphenyl sulfone and 0.012 part of accelerator 2-methylimidazole, stirring for 0.35 hour at 65 ℃, fully and uniformly dispersing, sampling, testing the molding time (180 ℃ hot plate) of the glue solution by using a knife method for 524 seconds, and finishing the preparation of the glue solution.
Examples 1 to 2:
adding 17 parts of biphenyl novolac epoxy resin, 13 parts of nitrile resin, 19 parts of MPEPEB and 17 parts of butanone into a glue preparation tank respectively, stirring for 6 hours at 50 ℃, adding 12 parts of nano montmorillonite and 5 parts of acetone, stirring for 1 hour at 55 ℃, adding 15 parts of phenoxy cyclophosphazene compound, stirring for 1 hour at 65 ℃, adding 3 parts of dicyandiamide and 0.08 part of accelerator aluminum acetylacetonate, continuously stirring for 0.45 hour at 72 ℃, fully and uniformly dispersing, sampling, testing the molding time (180 ℃ hot plate) of glue solution by using a knife method for 573 seconds, and finishing the preparation of the glue solution.
Examples 1 to 3:
respectively adding 23 parts of epoxy resin, 17 parts of boron phenolic resin, 17 parts of MPEPEB (propylene diene monomer) and 9 parts of cyclohexanone of dicyclopentadiene polycondensation resin into a glue preparation tank, stirring for 19 hours at 50 ℃, adding 8 parts of nano montmorillonite and 7 parts of cyclohexanone, stirring for 2 hours at 65 ℃, adding 12 parts of phosphorus-containing phenolic resin, stirring for 1 hour at 65 ℃, adding 5 parts of dicyandiamide and 0.02 part of accelerator 2-ethyl-4-methylimidazole, continuously stirring for 0.45 hour at 65 ℃, fully and uniformly dispersing, sampling, testing the molding time (180 ℃ hot plate) of glue solution by using a knife method for 608 seconds, and finishing the preparation of the glue solution.
Examples 1 to 4:
19 parts of bisphenol A type epoxy resin, 21 parts of bismaleimide resin and LCEU are respectively added into a glue preparation tankPPG15 parts of dimethylbenzene and 9 parts of dimethylbenzene, the mixture is stirred for 19 hours at 55 ℃, 5 parts of carbon nano tube and 13 parts of ethylene glycol are added, the mixture is stirred for 2 hours at 60 ℃, 12 parts of phosphorus-containing epoxy resin is added, the mixture is stirred for 1.5 hours at 75 ℃, 9 parts of 4, 4-diamino diphenyl sulfone and 0.06 part of accelerator boron trifluoride ethylamine trifluoride are added, the mixture is stirred for 0.55 hour at 75 ℃ to be fully and uniformly dispersed, a sample is taken, the molding time (180 ℃ hot plate) of the glue solution is tested by a knife method for 611 seconds, and the glue solution is prepared.
Examples 1 to 5:
22 parts of bisphenol A epoxy resin, 15 parts of bismaleimide resin, 3 parts of LCI and 6 parts of methyl ethyl ketone are respectively added into a glue preparation tank, the mixture is stirred for 11.5 hours at the temperature of 60 ℃, 7 parts of nano aluminum hydroxide and 6 parts of acetone are added, the mixture is stirred for 0.5 hour at the temperature of 55 ℃, 18 parts of phenoxy cyclophosphazene compound is added, the mixture is stirred for 1.25 hours at the temperature of 60 ℃, 11 parts of 4, 4-diamino diphenyl sulfone and 0.014 part of accelerator 2-methylimidazole are added, the mixture is continuously stirred for 0.25 hour at the temperature of 62 ℃, after the mixture is fully dispersed uniformly, a sample is taken, the molding time (180 ℃ hot plate) of the glue solution is tested by using a knife method for 491 seconds, and the glue solution is prepared.
Examples 1 to 6:
adding 25 parts of phenol novolac epoxy resin, 11 parts of nitrile resin and LCEU into a glue preparation tankPPG13 parts of butanone and 15 parts of butanone, stirring the mixture for 16 hours at the temperature of 55 ℃, and adding 8 parts of nano silicon dioxide and butanone8 parts of the raw materials are stirred for 1.5 hours at 70 ℃, 6 parts of phosphorus-containing phenolic resin is added, the mixture is stirred for 0.5 hour at 55 ℃, 6 parts of 4, 4-diaminodiphenylmethane and 0.02 part of accelerator 2-ethyl-4-methylimidazole are added, the mixture is continuously stirred for 0.35 hour at 60 ℃ to be fully and uniformly dispersed, then sampling is carried out, the forming time (180 ℃ hot plate) 617 seconds of the glue solution is tested by a knife method, and the glue solution is prepared.
Examples 1 to 7:
adding 27 parts of resorcinol epoxy resin, 17 parts of nitrile resin, 17 parts of MPEPEB and 15 parts of butanone into a glue preparation tank respectively, stirring for 21 hours at 60 ℃, adding 9 parts of nano aluminum oxide and 6 parts of methyl ethyl ketone, stirring for 1.75 hours at 55 ℃, adding 13 parts of phosphorus-containing phenolic resin, stirring for 0.75 hour at 60 ℃, adding 7 parts of 4, 4-diamino diphenyl sulfone and 0.016 part of accelerator 2-methylimidazole, stirring for 0.45 hour at 70 ℃, fully and uniformly dispersing, sampling, testing the molding time (180 ℃ hot plate) of glue solution by using a knife method for 607 seconds, and finishing the preparation of the glue solution.
Examples 1 to 8:
adding 24 parts of o-cresol novolac epoxy resin, 18 parts of boron novolac resin, 11 parts of LCI and 14 parts of methyl ethyl ketone into a glue preparation tank, stirring for 11 hours at 55 ℃, adding 6 parts of nano montmorillonite and 12 parts of ethylene glycol, stirring for 3 hours at 60 ℃, adding 9 parts of phenoxy cyclophosphazene compound, stirring for 1 hour at 75 ℃, adding 11 parts of 4, 4-diaminodiphenylmethane and 0.04 part of boron trifluoride ethylamine trifluoride as an accelerator, stirring for 0.55 hour at 72 ℃, fully and uniformly dispersing, sampling, testing the molding time (180 ℃ hot plate) of glue solution by using a knife method for 592 seconds, and finishing the preparation of the glue solution.
Examples 1 to 9:
adding 21 parts of resorcinol epoxy resin, 14 parts of bismaleimide resin, 21 parts of MPEPEB and 14 parts of cyclohexanone into a glue preparation tank respectively, stirring for 18 hours at 60 ℃, adding 8 parts of nano-silica and 6 parts of acetone, stirring for 2 hours at 60 ℃, adding 14 parts of phosphorus-containing epoxy resin, stirring for 1.25 hours at 80 ℃, adding 6 parts of dicyandiamide and 0.016 part of accelerator 2-ethyl-4-methylimidazole, stirring for 0.45 hour at 65 ℃, fully and uniformly dispersing, sampling, testing the molding time (180 ℃ hot plate) of the glue solution by using a knife method for 462 seconds, and finishing the preparation of the glue solution.
Examples 1 to 10:
adding 26 parts of bisphenol A epoxy resin, 11 parts of boron phenolic resin and LCEU into a glue preparation tankPPG16 parts of toluene and 8 parts of toluene, stirring the mixture for 22 hours at the temperature of 50 ℃, adding 7 parts of carbon nano tube and 9 parts of cyclohexanone, stirring the mixture for 2.5 hours at the temperature of 75 ℃, adding 16 parts of phenoxy cyclophosphazene compound, stirring the mixture for 1.5 hours at the temperature of 80 ℃, adding 12 parts of 4, 4-diamino diphenyl sulfone and 0.013 part of accelerator 2-ethyl-4-methylimidazole, stirring the mixture for 0.45 hour at the temperature of 63 ℃, fully and uniformly dispersing the mixture, sampling the mixture, testing the molding time of glue solution by using a knife method (a hot plate at the temperature of 180 ℃)493 seconds, and finishing the preparation of the glue solution.
Examples 1 to 11:
respectively adding 29 parts of o-cresol novolac epoxy resin, 14 parts of nitrile resin, 8 parts of LCI and 17 parts of ethylene glycol into a glue preparation tank, stirring for 13 hours at 65 ℃, adding 10 parts of nano montmorillonite and 9 parts of acetone, stirring for 2.75 hours at 60 ℃, adding 15 parts of phosphorus-containing phenolic resin, stirring for 0.75 hour at 75 ℃, adding 7 parts of 4, 4-diaminodiphenyl sulfone and 0.015 part of accelerator 2-methylimidazole, stirring for 0.75 hour at 70 ℃, fully and uniformly dispersing, sampling, testing the molding time (180 ℃ hot plate) of glue solution by using a knife method for 551 seconds, and finishing the preparation of the glue solution.
Examples 1 to 12:
adding 25 parts of o-cresol novolac epoxy resin, 16 parts of bismaleimide resin and biphenyl novolac epoxy resin LCEU into a glue preparation tank respectivelyPPG18 parts of nano silicon dioxide and 13 parts of butanone are added after being stirred for 21 hours at 60 ℃, 6 parts of nano silicon dioxide and 11 parts of methyl ethyl ketone are added, the mixture is stirred for 1.25 hours at 65 ℃, 17 parts of phosphorus-containing phenolic resin is added, the mixture is stirred for 1 hour at 65 ℃, 8 parts of 4, 4-diaminodiphenylmethane and 0.1 part of accelerant aluminum acetylacetonate are added, the mixture is continuously stirred for 0.55 hour at 70 ℃ to be fully and uniformly dispersed, then sampling is carried out, the molding time (hot plate at 180 ℃) of the glue solution is tested for 476 seconds by a knife method, and the glue solution is prepared.
Examples 1 to 13:
respectively adding 10 parts of o-cresol novolac epoxy resin, 14 parts of dicyclopentadiene polycondensation resin epoxy resin, 20 parts of nitrile resin, 16 parts of MPEPEB and 16 parts of ethanol into a glue preparation tank, stirring for 19 hours at 60 ℃, adding 11 parts of nano aluminum hydroxide and 7 parts of butanone, stirring for 1 hour at 70 ℃, adding 11 parts of phenoxy cyclic phosphazene compound, stirring for 1.5 hours at 85 ℃, adding 4 parts of dicyandiamide and 0.08 part of accelerator boron trifluoride ethylamine, continuing stirring for 0.55 hour at 70 ℃, fully and uniformly dispersing, sampling, testing the molding time (180 ℃ hot plate) for 495 seconds by using a knife method, and finishing the preparation of the glue solution.
Examples 1 to 14:
respectively adding 9 parts of o-cresol novolac epoxy resin, 15 parts of bismaleimide resin, 19 parts of nitrile resin, 12 parts of LCI and 11 parts of butanone into a glue preparation tank, stirring for 15 hours at 65 ℃, adding 8 parts of nano montmorillonite and 4 parts of acetone, stirring for 1.75 hours at 50 ℃, adding 8 parts of phenoxyl cyclophosphazene compound, stirring for 1.15 hours at 80 ℃, adding 7 parts of 4, 4-diaminodiphenyl sulfone and 0.01 part of accelerator 2-ethyl-4-methylimidazole, continuously stirring for 0.45 hour at 65 ℃, fully dispersing uniformly, sampling, testing the molding time (180 ℃ hot plate) of the glue solution by using a knife method for 533 seconds, and finishing the preparation of the glue solution.
Examples 1 to 15:
respectively adding 11 parts of o-cresol novolac epoxy resin, 11 parts of resorcinol epoxy resin, 19 parts of boron novolac resin, 18 parts of LCI and 17 parts of acetone into a glue preparation tank, stirring for 18 hours at 55 ℃, adding 9 parts of nano silicon dioxide and 11 parts of ethylene glycol, stirring for 1.25 hours at 75 ℃, adding 9 parts of phosphorus-containing novolac resin, stirring for 0.55 hour at 70 ℃, adding 9 parts of 4, 4-diaminodiphenylmethane and 0.06 part of accelerator aluminum acetylacetonate, continuously stirring for 0.75 hour at 75 ℃, fully and uniformly dispersing, sampling, testing the molding time (180 ℃ hot plate) 584 seconds of the glue solution by using a knife method, and finishing the preparation of the glue solution.
Examples 1 to 16:
6 parts of o-cresol novolac epoxy resin, 17 parts of dicyclopentadiene polycondensation resin epoxy resin, 18 parts of nitrile resin and LCEU are respectively added into a glue preparation tankPPG22 parts of nano montmorillonite and 8 parts of butanone, stirring the mixture for 24 hours at 65 ℃, adding 10 parts of nano montmorillonite and 6 parts of xylene, stirring the mixture for 2.15 hours at 70 ℃, adding 6 parts of phenoxy cyclophosphazene compound and 7 parts of phosphorus-containing phenolic resin, stirring the mixture for 0.75 hour at 75 ℃, adding 11 parts of 4, 4-diaminodiphenyl sulfone and 0.011 part of accelerator 2-ethyl-4-methylimidazole, continuously stirring the mixture for 0.45 hour at 65 ℃, fully and uniformly dispersing the mixture, sampling the mixture, testing the molding time (hot plate at 180 ℃)591 seconds of glue solution by using a knife method, and finishing the preparation of the glue solution.
Examples 1 to 17:
respectively adding 15 parts of o-cresol novolac epoxy resin, 7 parts of bisphenol A epoxy resin, 6 parts of resorcinol epoxy resin, 5 parts of nitrile resin, 12 parts of boron phenolic resin, 15 parts of MPEPEB and 12 parts of methyl ethyl ketone into a glue preparation tank, stirring for 21 hours at 65 ℃, adding 12 parts of nano silicon dioxide and 11 parts of cyclohexanone, stirring for 1.25 hours at 60 ℃, adding 8 parts of phosphorus-containing epoxy resin and 10 parts of phosphorus-containing phenolic resin, stirring for 1.5 hours at 70 ℃, adding 8 parts of 4, 4-diaminodiphenyl sulfone, 1 part of dicyandiamide and 0.07 part of accelerator boron ethylamine trifluoride, continuously stirring for 0.55 hours at 70 ℃, fully and uniformly dispersing, sampling, and testing the molding time (180 ℃ hot plate) by using a knife glue solution method for 564 seconds to finish the preparation of the glue solution.
Examples 1 to 18:
5 parts of phenol novolac epoxy resin, 6 parts of o-cresol novolac epoxy resin, 8 parts of dicyclopentadiene polycondensation resin epoxy resin, 3 parts of nitrile resin, 13 parts of bismaleimide resin, 13 parts of LCI and 16 parts of butanone are respectively added into a glue preparation tank, stirred for 22 hours at 60 ℃, added with 8 parts of carbon nano tube and 7 parts of toluene, stirred for 2.5 hours at 70 ℃, added with 6 parts of phosphorus-containing epoxy resin and 6 parts of phosphorus-containing phenolic resin, stirred for 1.05 hours at 80 ℃, added with 9 parts of non-4, 4-diaminodiphenyl sulfone, 3 parts of 4, 4-diaminodiphenyl methane and 0.014 part of accelerator 2-methylimidazole, stirred for 0.75 hours at 65 ℃ to be fully and uniformly dispersed, sampled, and tested for molding time (180 ℃) by a glue solution method for 498 seconds by a hot plate, and the glue solution is prepared.
Examples 1 to 19:
adding 6 parts of resorcinol epoxy resin, 9 parts of o-cresol novolac epoxy resin, 11 parts of biphenyl novolac epoxy resin, 15 parts of bismaleimide resin, 4 parts of nitrile resin and LCEU into a glue preparation tank respectivelyPPG23 parts of alcohol and 15 parts of nano-montmorillonite, stirring for 23 hours at 60 ℃, adding 7 parts of nano-montmorillonite and 5 parts of acetone, stirring for 2.75 hours at 65 ℃, adding 5 parts of phenoxy cyclophosphazene compound and 11 parts of phosphorus-containing phenolic resin, stirring for 1.25 hours at 80 ℃, adding 8 parts of 4, 4-diaminodiphenyl sulfone, 2 parts of dicyandiamide and 0.07 part of accelerator aluminum acetylacetonate, continuously stirring for 1 hour at 70 ℃, fully and uniformly dispersing, sampling, testing the molding time (hot plate at 180 ℃) of glue solution by using a knife method for 479 seconds, and finishing the preparation of the glue solution.
Examples 1 to 20:
respectively adding 12 parts of bisphenol A type epoxy resin, 11 parts of biphenyl type phenolic aldehyde epoxy resin, 8 parts of dicyclopentadiene polycondensation resin epoxy resin, 11 parts of bismaleimide resin, 10 parts of boron phenolic resin, 17 parts of MPEPEB, 4 parts of xylene and 4 parts of ethylene glycol into a glue preparation tank, stirring for 21 hours at 60 ℃, adding 8 parts of nano silicon dioxide and 9 parts of butanone, stirring for 1.5 hours at 60 ℃, adding 8 parts of phosphorus-containing epoxy resin and 6 parts of phenoxy cyclic phosphazene compound, stirring for 1.05 hours at 75 ℃, adding 9 parts of 4, 4-diaminodiphenyl sulfone, 5 parts of 4, 4-diaminodiphenyl methane and 0.018 parts of accelerator 2-ethyl-4-methylimidazole, continuously stirring for 0.75 hour at 65 ℃, sampling, testing the forming glue solution time (hot plate at 180 ℃)519 seconds by using a small knife method after fully and uniformly dispersing the materials, and finishing the preparation of the glue solution.
Examples 1 to 21:
respectively adding 11 parts of bisphenol A type epoxy resin, 9 parts of phenol type novolac epoxy resin, 9 parts of dicyclopentadiene polycondensation resin epoxy resin, 8 parts of bismaleimide resin, 9 parts of nitrile resin, 14 parts of MPEPEB and 13 parts of butanone into a glue preparation tank, stirring for 19 hours at 65 ℃, adding 11 parts of nano aluminum oxide, 4 parts of acetone and 3 parts of cyclohexanone, stirring for 0.75 hour at 70 ℃, adding 6 parts of phosphorus-containing epoxy resin, 2 parts of phenoxy cyclic phosphazene compound and 5 parts of phosphorus-containing phenolic resin, stirring for 1.5 hours at 80 ℃, adding 7 parts of 4, 4-diaminodiphenyl sulfone, 2 parts of dicyandiamide and 0.017 part of accelerator 2-ethyl-4-methylimidazole, continuously stirring for 0.55 hour at 65 ℃, sampling, testing the glue solution molding time (hot plate at 180 ℃) by using a method for 547 seconds, and finishing the preparation of the glue solution.
Preparation of second part halogen-free flame-retardant high-strength resin fiber fabric prepreg
Example 2-1:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 7 hours at 55 ℃, adding filler and solvent, stirring for 1 hour at 50 ℃, adding modified resin A, stirring for 0.75 hour at 75 ℃, adding curing agent and accelerator, stirring for 0.35 hour at 65 ℃, fully and uniformly dispersing, sampling, testing the forming time of glue solution by using a knife method, and completing the preparation of the glue solution when the forming time is 524 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 4m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Example 2-2:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 6 hours at 50 ℃, adding filler and solvent, stirring for 1 hour at 55 ℃, adding modified resin A, stirring for 1 hour at 65 ℃, adding curing agent and accelerator, stirring for 0.45 hour at 72 ℃, fully and uniformly dispersing, sampling, testing the forming time of glue solution by using a knife method, and completing the preparation of the glue solution when the forming time is 573 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 5.5m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 3:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 19 hours at 50 ℃, adding filler and solvent, stirring for 2 hours at 65 ℃, adding modified resin A, stirring for 1 hour at 65 ℃, adding a curing agent and an accelerant, stirring for 0.45 hour at 65 ℃, fully and uniformly dispersing, sampling, testing the forming time of glue solution by using a knife method, and when the forming time is 608 seconds under the condition of a hot plate at 180 ℃, finishing the preparation of the glue solution;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 7m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 4:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 19 hours at 55 ℃, adding filler and solvent, stirring for 2 hours at 60 ℃, adding modified resin A, stirring for 1.5 hours at 75 ℃, adding curing agent and accelerator, stirring for 0.55 hour at 75 ℃, fully and uniformly dispersing, sampling, testing the forming time of glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 611 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 8m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 5:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 11.5 hours at 60 ℃, adding filler and solvent, stirring for 0.5 hour at 55 ℃, adding modified resin A, stirring for 1.25 hours at 60 ℃, adding curing agent and accelerator, stirring for 0.25 hour at 62 ℃, fully and uniformly dispersing, sampling, testing the forming time of the glue solution by using a knife method, and preparing the glue solution when the forming time is 491 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 2m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 6:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 16 hours at 55 ℃, adding filler and solvent, stirring for 1.5 hours at 70 ℃, adding modified resin A, stirring for 0.5 hour at 55 ℃, adding curing agent and accelerator, stirring for 0.35 hour at 60 ℃, fully and uniformly dispersing, sampling, testing the forming time of the glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 617 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 10m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 7:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 21 hours at 60 ℃, adding filler and solvent, stirring for 1.75 hours at 55 ℃, adding modified resin A, stirring for 0.75 hour at 60 ℃, adding curing agent and accelerator, stirring for 0.45 hour at 70 ℃, fully and uniformly dispersing, sampling, testing the forming time of the glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 607 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 7m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 8:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 11 hours at 55 ℃, adding filler and solvent, stirring for 3 hours at 60 ℃, adding modified resin A, stirring for 1 hour at 75 ℃, adding curing agent and accelerator, stirring for 0.55 hour at 72 ℃, fully and uniformly dispersing, sampling, testing the forming time of glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 592 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 5.5m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 9:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 18 hours at 60 ℃, adding filler and solvent, stirring for 2 hours at 60 ℃, adding modified resin A, stirring for 1.25 hours at 80 ℃, adding curing agent and accelerator, stirring for 0.45 hour at 65 ℃, fully and uniformly dispersing, sampling, testing the forming time of glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 462 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 2m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 10:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 22 hours at 50 ℃, adding filler and solvent, stirring for 2.5 hours at 75 ℃, adding modified resin A, stirring for 1.5 hours at 80 ℃, adding curing agent and accelerator, stirring for 0.45 hour at 63 ℃, fully and uniformly dispersing, sampling, testing the forming time of the glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 493 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 2m/min, thus obtaining the halogen-free flame-retardant high-strength resin glass fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 11:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 13 hours at 65 ℃, adding filler and solvent, stirring for 2.75 hours at 60 ℃, adding modified resin A, stirring for 0.75 hour at 75 ℃, adding curing agent and accelerator, stirring for 0.75 hour at 70 ℃, fully and uniformly dispersing, sampling, testing the forming time of the glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 551 seconds at 180 ℃ under the condition of a hot plate;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 5m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 12:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 21 hours at 60 ℃, adding filler and solvent, stirring for 1.25 hours at 65 ℃, adding modified resin A, stirring for 1 hour at 65 ℃, adding a curing agent and an accelerator, stirring for 0.55 hour at 70 ℃, fully and uniformly dispersing, sampling, testing the forming time of glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 476 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 1m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 13:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 19 hours at 60 ℃, adding filler and solvent, stirring for 1 hour at 70 ℃, adding modified resin A, stirring for 1.5 hours at 85 ℃, adding a curing agent and an accelerator, stirring for 0.55 hour at 70 ℃, fully and uniformly dispersing, sampling, testing the forming time of glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 495 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 2m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 14:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 15 hours at 65 ℃, adding filler and solvent, stirring for 1.75 hours at 50 ℃, adding modified resin A, stirring for 1.15 hours at 80 ℃, adding curing agent and accelerator, stirring for 0.45 hour at 65 ℃, fully and uniformly dispersing, sampling, testing the forming time of the glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 533 seconds at 180 ℃ under the condition of a hot plate;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 4m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 15:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 18 hours at 55 ℃, adding filler and solvent, stirring for 1.25 hours at 75 ℃, adding modified resin A, stirring for 0.55 hour at 70 ℃, adding curing agent and accelerator, stirring for 0.75 hour at 75 ℃, fully and uniformly dispersing, sampling, testing the forming time of the glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 584 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 5.5m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 16:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 24 hours at 65 ℃, adding filler and solvent, stirring for 2.15 hours at 70 ℃, adding modified resin A, stirring for 0.75 hour at 75 ℃, adding curing agent and accelerator, stirring for 0.45 hour at 65 ℃, fully and uniformly dispersing, sampling, testing the forming time of the glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 591 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 5.5m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 17:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 21 hours at 65 ℃, adding filler and solvent, stirring for 1.25 hours at 60 ℃, adding modified resin A, stirring for 1.5 hours at 70 ℃, adding a curing agent and an accelerator, stirring for 0.55 hour at 70 ℃, fully and uniformly dispersing, sampling, testing the forming time of the glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 564 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg: coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 5m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 18:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 22 hours at 60 ℃, adding filler and solvent, stirring for 2.5 hours at 70 ℃, adding modified resin A, stirring for 1.05 hours at 80 ℃, adding curing agent and accelerator, stirring for 0.75 hour at 65 ℃, fully and uniformly dispersing, sampling, testing the forming time of the glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 498 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg:
coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 3m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 19:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 23 hours at 60 ℃, adding filler and solvent, stirring for 2.75 hours at 65 ℃, adding modified resin A, stirring for 1.25 hours at 80 ℃, adding curing agent and accelerator, stirring for 1 hour at 70 ℃, fully and uniformly dispersing, sampling, testing the forming time of glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 479 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg:
coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 2.5m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
Examples 2 to 20:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 21 hours at 60 ℃, adding filler and solvent, stirring for 1.5 hours at 60 ℃, adding modified resin A, stirring for 1.05 hours at 75 ℃, adding curing agent and accelerator, stirring for 0.75 hour at 65 ℃, fully and uniformly dispersing, sampling, testing the forming time of the glue solution by using a knife method, and completing the preparation of the glue solution when the forming time is 519 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg:
coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 4m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is more than or equal to 95 percent, and the content of volatile matters is less than or equal to 2 percent;
examples 2 to 21:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
(b) respectively adding epoxy resin, modified resin B and solvent with the formula amount into a glue preparation tank, stirring for 19 hours at 65 ℃, adding filler and solvent, stirring for 0.75 hour at 70 ℃, adding modified resin A, stirring for 1.5 hours at 80 ℃, adding curing agent and accelerator, stirring for 0.55 hour at 65 ℃, fully and uniformly dispersing, sampling, testing the forming time of the glue solution by using a knife method, and finishing the preparation of the glue solution when the forming time is 547 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber fabric prepreg:
coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 4m/min, thus obtaining the halogen-free flame-retardant high-strength resin glass fiber fabric prepreg; indexes of the fiber fabric prepreg are as follows: the content of soluble resin is greater than or equal to 95 percent, and the volatile matter is less than or equal to 2 percent.
The following table 1 shows the preparation process parameters, the central control technical indexes and the test results of the halogen-free flame-retardant high-strength resin fiber fabric prepreg of the embodiment of the invention.
Table 1: the preparation process parameters and the central control technical indexes of the halogen-free flame-retardant high-strength resin fiber fabric prepreg of the embodiment are as follows:
preparation of third part tension-torsion plate
a. Taking the components of the ingredients, wherein the weight ratio of the ingredients is the same as that of any one of the embodiments 1-21;
b. taking a prepreg, wherein the components and the weight ratio of the prepreg are the same as those in any one of embodiments 2-1-2-21;
c. examples 3-1 to 3-21 compression of tension plates:
according to the requirements of a tension-torsion plate pressing process for halogen-free flame-retardant high-strength resin glass fiber fabric prepreg with required size, the halogen-free flame-retardant high-strength resin glass fiber fabric prepreg is flatly placed in a mold with the temperature controlled at 135-155 ℃, the mold is closed, the temperature is controlled at 185-215 ℃, and the pressure is controlled at 20-23 MPa, the thermal baking curing molding is carried out for 5-26 h, and then the tension-torsion plate is prepared.
The following table 2 shows the technical performance test results of the tension torsion plate pressing of the embodiment of the invention.
Table 2: results of technical Property testing of the articles obtained in examples
Example 4:
a tension-torsion plate for halogen-free flame-retardant high-strength wind power is a composite material prepared by curing and molding overlapped halogen-free flame-retardant high-strength resin fiber cloth prepreg at the temperature of 175 ℃;
the halogen-free flame-retardant high-strength resin fiber cloth prepreg is a fiber impregnating material which is formed by coating halogen-free flame-retardant high-strength resin adhesive on a fiber fabric through a gluing machine and then baking the fiber fabric, wherein the impregnating material comprises the following components in percentage by weight: 25% of resin semi-cured substance and 75% of fiber fabric;
the halogen-free flame-retardant high-strength resin adhesive is prepared by mixing 17 parts by weight of epoxy resin, 6 parts by weight of modified resin A, 9 parts by weight of modified resin B, 3 parts by weight of toughening agent, 3 parts by weight of curing agent, 5 parts by weight of filler, 12 parts by weight of solvent and 0.01 part by weight of accelerator.
Example 5:
a tension-torsion plate for halogen-free flame-retardant high-strength wind power is a composite material prepared by curing and molding overlapped halogen-free flame-retardant high-strength resin fiber cloth prepreg at 215 ℃;
the halogen-free flame-retardant high-strength resin fiber cloth prepreg is a fiber impregnating material which is formed by coating halogen-free flame-retardant high-strength resin adhesive on a fiber fabric through a gluing machine and then baking the fiber fabric, wherein the impregnating material comprises the following components in percentage by weight: the weight percentage of the resin semi-cured product is 48 percent, and the weight percentage of the fiber fabric is 52 percent;
the halogen-free flame-retardant high-strength resin adhesive is prepared by mixing 31 parts by weight of epoxy resin, 18 parts by weight of modified resin A, 21 parts by weight of modified resin B, 24 parts by weight of toughening agent, 14 parts by weight of curing agent, 12 parts by weight of filler, 26 parts by weight of solvent and 0.1 part by weight of accelerator.
Example 6:
a tension-torsion plate for halogen-free flame-retardant high-strength wind power is a composite material prepared by curing and molding overlapped halogen-free flame-retardant high-strength resin fiber cloth prepreg at the temperature of 195 ℃;
the halogen-free flame-retardant high-strength resin fiber cloth prepreg is a fiber impregnating material which is formed by coating halogen-free flame-retardant high-strength resin adhesive on a fiber fabric through a gluing machine and then baking the fiber fabric, wherein the impregnating material comprises the following components in percentage by weight: the weight percentage of the resin semi-cured product is 36 percent, and the weight percentage of the fiber fabric is 64 percent;
the halogen-free flame-retardant high-strength resin adhesive is prepared by mixing 24 parts by weight of epoxy resin, 12 parts by weight of modified resin A, 15 parts by weight of modified resin B, 13.5 parts by weight of toughening agent, 8.5 parts by weight of curing agent, 8.5 parts by weight of filler, 19 parts by weight of solvent and 0.05 part by weight of accelerator.
Example 7:
a preparation method of a halogen-free flame-retardant high-strength tension-torsion plate for wind power comprises the following steps:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) preparing materials: taking raw materials of 17 parts by weight of epoxy resin, 6 parts by weight of modified resin A, 9 parts by weight of modified resin B, 3 parts by weight of toughening agent, 3 parts by weight of curing agent, 5 parts by weight of filler, 0.01 part by weight of accelerator and 12 parts by weight of solvent;
(b) adding epoxy resin, modified resin B, toughening agent and solvent (the solvent amount can be 30 percent of the total weight of the solvent) into a glue preparation tank, stirring for 24 hours at the temperature of 50 ℃ (constant temperature), adding filler and solvent (namely the rest 70 percent of the solvent) and stirring for 3 hours at the temperature of 50 ℃ (constant temperature), then adding modified resin A and stirring for 1.5 hours at the temperature of 55 ℃ (constant temperature), continuously adding curing agent and accelerant and stirring for 0.25 to 1 hour at the temperature of 60 ℃ (constant temperature), adjusting the molding time of glue solution, sampling, testing the molding time of the glue solution by using a knife method, and preparing the halogen-free flame-retardant high-strength resin adhesive when the molding time is 462 to 617 seconds under the condition of a hot plate at 180 ℃;
b. preparing a halogen-free flame-retardant high-strength resin fiber cloth prepreg:
coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 1-10 m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber cloth prepreg;
c. pressing a tension-torsion plate:
taking halogen-free flame-retardant high-strength resin fiber cloth prepreg according to the required size (same as the prior art) required by the pressing process of the tension-torsion plate, flatly placing the halogen-free flame-retardant high-strength resin fiber cloth prepreg in a mold with the temperature controlled at 135 ℃, closing the mold, and carrying out hot baking, curing and molding for 26 hours under the conditions of the temperature controlled at 185 ℃ and the pressure of 20MPa to obtain the tension-torsion plate.
Example 8:
a preparation method of a halogen-free flame-retardant high-strength tension-torsion plate for wind power comprises the following steps:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) preparing materials: taking the raw materials of 31 parts by weight of epoxy resin, 18 parts by weight of modified resin A, 21 parts by weight of modified resin B, 24 parts by weight of toughening agent, 14 parts by weight of curing agent, 12 parts by weight of filler, 0.1 part by weight of accelerator and 26 parts by weight of solvent;
(b) adding epoxy resin, modified resin B, toughening agent and solvent (the solvent amount can be 70 percent of the total weight of the solvent) into a glue preparation tank, stirring for 6 hours at the temperature of 65 ℃ (constant temperature), adding filler and solvent (namely the rest 30 percent of the solvent) and stirring for 0.5 hour at the temperature of 75 ℃ (constant temperature), adding modified resin A and stirring for 0.5 hour at the temperature of 85 ℃ (constant temperature), continuously adding curing agent and accelerator and stirring for 0.25 to 1 hour at the temperature of 75 ℃ (constant temperature), adjusting the molding time of glue solution, sampling, testing the molding time of the glue solution by using a knife method, and preparing the halogen-free flame-retardant high-strength resin adhesive under the condition of a hot plate at 180 ℃ and when the molding time is 462 to 617 seconds;
b. preparing a halogen-free flame-retardant high-strength resin fiber cloth prepreg:
coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 1-10 m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber cloth prepreg;
c. pressing a tension-torsion plate:
taking halogen-free flame-retardant high-strength resin fiber cloth prepreg according to the required size (same as the prior art) required by the pressing process of the tension-torsion plate, flatly placing the halogen-free flame-retardant high-strength resin fiber cloth prepreg in a mold with the temperature controlled at 135-155 ℃, closing the mold, and carrying out hot baking, curing and molding for 5 hours under the conditions of controlling the temperature at 215 ℃ and the pressure at 23MPa to obtain the tension-torsion plate.
Example 9:
a preparation method of a halogen-free flame-retardant high-strength tension-torsion plate for wind power comprises the following steps:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) preparing materials: taking the raw materials of 24 parts by weight of epoxy resin, 12 parts by weight of modified resin A, 10 parts by weight of modified resin B, 13 parts by weight of toughening agent, 13 parts by weight of curing agent, 13 parts by weight of filler, 0.05 part by weight of accelerator and 19 parts by weight of solvent;
(b) adding epoxy resin, modified resin B, toughening agent and solvent (the solvent amount can be 50 percent of the total weight of the solvent) into a glue preparation tank, stirring for 15 hours at a temperature of 58 ℃ (constant temperature), adding filler and solvent (namely the rest 50 percent of the solvent) and stirring for 2 hours at a temperature of 62 ℃ (constant temperature), adding modified resin A and stirring for 1 hour at a temperature of 70 ℃ (constant temperature), continuously adding curing agent and accelerator and stirring for 0.25 to 1 hour at a temperature of 67 ℃ (constant temperature), adjusting the molding time of glue solution, sampling, testing the molding time of the glue solution by using a knife method, and preparing the halogen-free flame-retardant high-strength resin adhesive under the condition of a hot plate at 180 ℃ when the molding time is 462 to 617 seconds;
b. preparing a halogen-free flame-retardant high-strength resin fiber cloth prepreg:
coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 1-10 m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber cloth prepreg;
c. pressing a tension-torsion plate:
taking halogen-free flame-retardant high-strength resin fiber cloth prepreg according to the required size (same as the prior art) required by the pressing process of the tension-torsion plate, flatly placing the halogen-free flame-retardant high-strength resin fiber cloth prepreg in a mold with the temperature controlled at 135-155 ℃, closing the mold, controlling the temperature at 200 ℃ and the pressure at 21MPa, baking, curing and molding for 15 hours, and thus obtaining the tension-torsion plate.
In examples 4 to 9 above:
the epoxy resin is one or a mixture of more than two of bisphenol A epoxy resin, o-cresol novolac epoxy resin, phenol novolac epoxy resin, resorcinol epoxy resin, biphenyl novolac epoxy resin and dicyclopentadiene polycondensation resin;
the modified resin A is one or a mixture of more than two of phosphorus-containing epoxy resin, phosphorus-containing phenolic resin and phenoxy cyclophosphazene compounds; the molecular structure of the phenoxy cyclophosphazene compound is the same as that of the phenoxy cyclophosphazene compound;
the modified resin B is one or a mixture of two of bismaleimide resin, nitrile resin and boron phenolic resin; the curing agent is one or a mixture of two of 4, 4-diaminodiphenylmethane, 4-diaminodiphenyl sulfone and dicyandiamide; the filler is one or a mixture of two of nano montmorillonite, nano vermiculite, nano silicon dioxide, nano aluminum hydroxide, nano aluminum oxide and carbon nano tubes; the accelerant is any one of 2-methylimidazole, 2-ethyl-4-methylimidazole, N-dimethylbenzylamine, boron trifluoride ethylamine and aluminum acetylacetonate;
the toughening agent is LCI and LCEUPPGAnd MPEPEB, the molecular structural formula of which is the same as above;
the fiber fabric is one or a combination of two of alkali-free glass fiber checkered cloth, alkali-free glass fiber twill cloth, carbon fiber checkered cloth and basalt fiber checkered cloth.
The solvent is one or a mixture of more than two of toluene, xylene, ethylene glycol, methyl ethyl ketone, cyclohexanone, butanone, acetone, N-dimethylformamide and ethanol;
the tensile strength of the tension-torsion plate in the axial direction is more than or equal to 520MPa (the tensile strength reaches 520 MPa-657 MPa), the shear strength in the axial direction is more than or equal to 45MPa (the shear strength reaches 45 MPa-63 MPa), the temperature resistance is more than or equal to 150 ℃, and the halogen-free flame retardance reaches V-0;
in the above embodiment: the percentages used, not specifically indicated, are percentages by weight or known to those skilled in the art; the proportions used, not specifically noted, are mass (weight) proportions; the parts by weight may each be grams or kilograms.
In the above embodiment: the process parameters (temperature, time, pressure, etc.) and the amounts of the components in each step are within the range, and any point can be applicable. The present invention and the technical contents not specifically described in the above examples are the same as those of the prior art, and the raw materials are all commercially available products.
The present invention is not limited to the above-described embodiments, and the present invention can be implemented with the above-described advantageous effects.
Claims (8)
1. The utility model provides a do not have fire-retardant high strength wind-powered electricity generation and use board that turns round which characterized by: the tension-torsion plate is a composite material prepared by curing and molding overlapped halogen-free flame-retardant high-strength resin fiber cloth prepreg at the temperature of 175-215 ℃;
the halogen-free flame-retardant high-strength resin fiber cloth prepreg is a fiber impregnating material which is formed by coating halogen-free flame-retardant high-strength resin adhesive on a fiber fabric through a gluing machine and then baking the fiber fabric, wherein the impregnating material comprises the following components in percentage by weight: 25-48% of resin semi-cured substance and 52-75% of fiber fabric;
the halogen-free flame-retardant high-strength resin adhesive is prepared by mixing 17-31 parts by weight of epoxy resin, 6-18 parts by weight of modified resin A, 9-21 parts by weight of modified resin B, 3-24 parts by weight of toughening agent, 3-14 parts by weight of curing agent, 5-12 parts by weight of filler, 12-26 parts by weight of solvent and 0.01-0.1 part by weight of accelerator;
the epoxy resin is one or a mixture of more than two of bisphenol A epoxy resin, o-cresol novolac epoxy resin, phenol novolac epoxy resin, resorcinol epoxy resin, biphenyl novolac epoxy resin and dicyclopentadiene polycondensation resin;
the modified resin A is one or a mixture of more than two of phosphorus-containing epoxy resin, phosphorus-containing phenolic resin and phenoxy cyclophosphazene compounds;
the modified resin B is one or a mixture of two of bismaleimide resin, nitrile resin and boron phenolic resin;
the curing agent is one or a mixture of two of 4, 4-diaminodiphenylmethane, 4-diaminodiphenyl sulfone and dicyandiamide;
the filler is one or a mixture of two of nano montmorillonite, nano vermiculite, nano silicon dioxide, nano aluminum hydroxide, nano aluminum oxide and carbon nano tubes;
the accelerant is any one of 2-methylimidazole, 2-ethyl-4-methylimidazole, N-dimethylbenzylamine, boron trifluoride ethylamine and aluminum acetylacetonate;
the toughening agent is LCI and LCEUPPGAnd MPEPEB, the molecular structural formula of which is shown as the following formula:
LCEUPPG 
LCI
2. the halogen-free flame-retardant high-strength tension-torsion plate for wind power as claimed in claim 1, which is characterized in that: the fiber fabric is one or a combination of two of alkali-free glass fiber checkered cloth, alkali-free glass fiber twill cloth, carbon fiber checkered cloth and basalt fiber checkered cloth.
3. The halogen-free flame-retardant high-strength tension-torsion plate for wind power as claimed in claim 1 or 2, which is characterized in that: the solvent is one or a mixture of more than two of toluene, xylene, ethylene glycol, methyl ethyl ketone, cyclohexanone, butanone, acetone, N-dimethylformamide and ethanol.
4. The halogen-free flame-retardant high-strength tension-torsion plate for wind power as claimed in claim 1 or 2, which is characterized in that: the tensile strength of the tension-torsion plate in the axial direction is more than or equal to 520MPa, the shear strength in the axial direction is more than or equal to 45MPa, the temperature resistance is more than or equal to 150 ℃, and the halogen-free flame retardance reaches V-0.
5. The preparation method of the halogen-free flame-retardant high-strength tension-torsion plate for the wind power is characterized by comprising the following steps of:
a. preparing a halogen-free flame-retardant high-strength resin adhesive:
(a) preparing materials: taking raw materials of 17-31 parts by weight of epoxy resin, 6-18 parts by weight of modified resin A, 9-21 parts by weight of modified resin B, 3-24 parts by weight of toughening agent, 3-14 parts by weight of curing agent, 5-12 parts by weight of filler, 0.01-0.1 part by weight of accelerator and 12-26 parts by weight of solvent;
the epoxy resin is one or a mixture of more than two of bisphenol A epoxy resin, o-cresol novolac epoxy resin, phenol novolac epoxy resin, resorcinol epoxy resin, biphenyl novolac epoxy resin and dicyclopentadiene polycondensation resin;
the modified resin A is one or a mixture of more than two of phosphorus-containing epoxy resin, phosphorus-containing phenolic resin and phenoxy cyclophosphazene compounds;
the modified resin B is one or a mixture of two of bismaleimide resin, nitrile resin and boron phenolic resin;
the curing agent is one or a mixture of two of 4, 4-diaminodiphenylmethane, 4-diaminodiphenyl sulfone and dicyandiamide;
the filler is one or a mixture of two of nano montmorillonite, nano vermiculite, nano silicon dioxide, nano aluminum hydroxide, nano aluminum oxide and carbon nano tubes;
the accelerant is any one of 2-methylimidazole, 2-ethyl-4-methylimidazole, N-dimethylbenzylamine, boron trifluoride ethylamine and aluminum acetylacetonate;
the toughening agent is LCI and LCEUPPGAnd MPEPEB, the molecular structure of which is as follows:
LCEUPPG 
LCI
(b) adding epoxy resin, modified resin B, toughening agent and solvent into a glue preparation tank, stirring for 6-24 hours at the temperature of 50-65 ℃, adding filler and solvent, stirring for 0.5-3 hours at the temperature of 50-75 ℃, adding modified resin A, stirring for 0.5-1.5 hours at the temperature of 55-85 ℃, continuously adding curing agent and accelerator, stirring for 0.25-1 hour at the temperature of 60-75 ℃, adjusting the forming time of glue solution, sampling, testing the forming time of the glue solution by using a knife method, and preparing the halogen-free flame-retardant high-strength resin adhesive under the condition of a hot plate at 180 ℃ and when the forming time is 462-617 seconds;
b. preparing a halogen-free flame-retardant high-strength resin fiber cloth prepreg:
coating the halogen-free flame-retardant high-strength resin adhesive in the step a on a fiber fabric through a gluing machine, and pre-drying the fiber fabric through a drying tunnel of the gluing machine, wherein the drying tunnel of the gluing machine is 24m long and is divided into 4 sections (one section, two sections, three sections and four sections in sequence) and 6m of each section, and the baking temperature range is 95-165 ℃, wherein: the temperature of the first section is 95-105 ℃, the temperature of the second section is 135-145 ℃, the temperature of the third section is 155-165 ℃, the temperature of the fourth section is 100-110 ℃, and the speed of a gluing machine is 1-10 m/min, thus obtaining the halogen-free flame-retardant high-strength resin fiber cloth prepreg;
c. pressing a tension-torsion plate:
taking halogen-free flame-retardant high-strength resin fiber cloth prepreg according to the required size required by the pressing process of the tension-torsion plate, flatly placing the halogen-free flame-retardant high-strength resin fiber cloth prepreg in a mold with the temperature controlled at 135-155 ℃, closing the mold, and carrying out hot baking, curing and molding for 5-26 h under the conditions of the temperature controlled at 185-215 ℃ and the pressure of 20-23 MPa to obtain the tension-torsion plate.
6. The preparation method of the halogen-free flame-retardant high-strength tension-torsion plate for wind power as claimed in claim 5, which is characterized by comprising the following steps: in the step b, the fiber fabric is one or a combination of two of alkali-free glass fiber checkered cloth, alkali-free glass fiber twill cloth, carbon fiber checkered cloth and basalt fiber checkered cloth.
7. The preparation method of the halogen-free flame-retardant high-strength tension-torsion plate for wind power as claimed in claim 5 or 6, which is characterized by comprising the following steps: in the step a, the solvent is one or a mixture of more than two of toluene, xylene, ethylene glycol, methyl ethyl ketone, cyclohexanone, butanone, acetone and ethanol.
8. The preparation method of the halogen-free flame-retardant high-strength tension-torsion plate for wind power as claimed in claim 5 or 6, which is characterized by comprising the following steps: and c, the prepared tension-torsion plate has the axial tensile strength of more than or equal to 520MPa, the axial shear strength of more than or equal to 45MPa, the temperature resistance of more than or equal to 150 ℃, and the halogen-free flame retardance reaching V-0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110180288.5A CN112961470A (en) | 2021-02-08 | 2021-02-08 | Halogen-free flame-retardant high-strength tension-torsion plate for wind power and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110180288.5A CN112961470A (en) | 2021-02-08 | 2021-02-08 | Halogen-free flame-retardant high-strength tension-torsion plate for wind power and preparation method thereof |
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| CN112961470A true CN112961470A (en) | 2021-06-15 |
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|---|---|---|---|
| CN202110180288.5A Pending CN112961470A (en) | 2021-02-08 | 2021-02-08 | Halogen-free flame-retardant high-strength tension-torsion plate for wind power and preparation method thereof |
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| CN106626617A (en) * | 2016-09-14 | 2017-05-10 | 四川东材科技集团股份有限公司 | Glass fibrofelt laminated plate and preparation method thereof |
| CN111040382A (en) * | 2019-12-27 | 2020-04-21 | 四川东材科技集团股份有限公司 | Melamine-epoxy glass fiber pipe and preparation method thereof |
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Application publication date: 20210615 |