CN105086351A - Hot-melting phenolic resin prepreg and preparation method thereof - Google Patents
Hot-melting phenolic resin prepreg and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a hot-melting phenolic resin prepreg and a preparation method thereof. The hot-melting phenolic resin prepreg comprises a fiber-reinforced material and the following materials by mass: 50 to 100 parts of thermoset phenolic resin, 1 to 10 parts of a film forming agent, and 1 to 10 parts of a boron-containing additive, wherein the mass ratio of the fiber-reinforced material to the thermoset phenolic resin is (1-3):1. The hot-melting phenolic resin prepreg is slow in curing rate, and relatively high in heat resistance; the preparation method is simple.
Description
Technical field
The invention belongs to prepreg manufacturing technology field, relate to a kind of hot melt process resol preimpregnation material and preparation method thereof.
Background technology
The quality of prepreg directly has influence on the performance quality of composite element.The preparation of prepreg mainly contains two kinds: solution dipping method and Hot-melt film method.Wherein solution dipping method mainly has that volatile content is too high, prepreg resin controls inaccurate, a large amount of solvent evaporates, and environmental pollution comparatively waits not enough.Therefore hot melt process prepeg process progressively becomes the developing direction of current prepreg.In advanced composite material preparation, the development of mainly epoxy prepreg prepared in recent years by sweat connecting material, wherein the disclosed patent of China has epoxy matrix resin, prepreg and preparation method thereof and the device (publication number CN102108188A) preparing prepreg employing, epoxy resin composition for fiber-reinforced composite material, prepreg and fibre reinforced composites (publication number CN1926188A), above patent utilization improves the sweat connecting material finally obtaining excellent performance to the solidifying agent of epoxy resin and solidification value.
Resol because of raw material be easy to get, with low cost, excellent thermotolerance, erosion resistance, flame retardant resistance, good mechanical property, the good characteristic such as unique ablation resistance, be widely used in the aspects such as molded composite material, veneer sheet, friction materials, thermal and sound insulating materials, now become irreplaceable important materials in national defense construction and development in science and technology, it is one of most widely used at present matrix material, but due to simple resol, to there is fragility in preparation technology large, solidification rate is fast, the problem that action pane is narrow.The mainly solution dipping method used for resol in current factory prepares prepreg, finally makes matrix material.In order to meet the development of new and high technology, the modification of resol and prepreg new preparation process are the focuses that people pay close attention to always.And very few to the research of hot melt process alkyd resin based prepreg so far, especially need research to meeting resol use properties and manufacturability aspect simultaneously.
Summary of the invention
The object of the invention is to the shortcoming overcoming above-mentioned prior art, provide a kind of hot melt process resol preimpregnation material and preparation method thereof, the solidification rate of this hot melt process resol preimpregnation material is slow, and thermotolerance is higher, and preparation method is simple.
For achieving the above object, hot melt process resol preimpregnation material of the present invention by fibre reinforcement material and by mass fraction be the heat-reactive phenolic resin of 50 ~ 100 parts, being prepared from containing boron additive of the membrane-forming agent of 1 ~ 10 part and 1 ~ 10 part, wherein, the mass ratio of fibre reinforcement material and heat-reactive phenolic resin is 1 ~ 3:1.
Described heat-reactive phenolic resin is one or more mixtures mixed in any proportion in ba phenolic resin, Mo-phenolic resin, W-phenolic resin, ammonia resol, phosphorous-containing phenolic resin, phenol cyanate resin and benzoxazine colophony.
Described membrane-forming agent is one or more mixtures mixed in any proportion in PAUR, polyether(poly)urethane, aliphatic polyurethane, acroleic acid polyurethane, aromatic urethane, end amido liquid acrylonitrile butadiene rubber, hydroxyl terminated butyl nitrile (HTBN) rubber, epoxy terminated paracril, nbr carboxyl terminal, polyethersulfone, polysulfones, poly ether imide, polyketone ether, polyphenylene oxide and polyaryletherketone.
Described is inorganic compounds of boron boric acid containing boron additive, boron oxide, borax, Sodium Tetraborate, phenyl-boron dihydroxide, diphenyl-borinic acids, naphthalene boronic acids, luxuriant and rich with fragrance boric acid, anthracene boric acid, benzyloxy phenylo boric acid, hydroxybenzene boric acid, methylol phenylo boric acid, isopropylphenylboronic acid, phenetole boric acid, dibromobenzene boric acid, dichlorobenzene boric acid, ethylbenzene boric acid, Carboxybenzeneboronic acid, aryl boron bakelite resin, one or more mixtures mixed in any proportion of thermosetting boron-containing phenolic resin and thermoplasticity boron bakelite resin.
Described fibre reinforcement material is by a kind of plain weave of braiding in high-strength glass fibre, high-elastic glass fibre, aromatic polyamide fibre, carbon fiber, boron fibre, aramid fiber, high molecular weight polyethylene fiber, human relations fiber difficult to understand and basalt fibre or the woven fiber glass of twill or carbon cloth.
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) take fibre reinforcement material, heat-reactive phenolic resin, membrane-forming agent by claim 1 and contain boron additive, heat-reactive phenolic resin is joined in reaction flask, and be heated to molten state, wherein, in heat-processed, add membrane-forming agent and contain boron additive, constant temperature stirs again, obtains phenolic resin blend, then phenolic resin blend described in freezing;
2) by step 1) phenolic resin blend that obtains dries, then pours in sweat connecting machine and make resin molding, then be cooled to room temperature, obtain the phenolic resin film of Resin film infusion;
3) by step 2) phenolic resin film of Resin film infusion that obtains and fibre reinforcement material carry out compound, obtains hot melt process resol preimpregnation material.
Step 1) in heat-reactive phenolic resin is added in reaction flask, and the concrete operations being heated to molten state are: added in reaction flask by heat-reactive phenolic resin, and are heated to 60 ~ 90 DEG C and make heat-reactive phenolic resin melting;
Step 1) in the process that stirs of constant temperature in reaction flask the rotating speed of heat-reactive phenolic resin be 100 ~ 500 revs/min, the time that constant temperature stirs is 80 ~ 240 minutes.
By step 1) phenolic resin blend that obtains dries, and the temperature then pouring sweat connecting machine in the process making resin molding in sweat connecting machine into is 60 ~ 95 DEG C, and film forming linear velocity is 1 ~ 3 m/min, and cold plate temperature is 10 ~ 20 DEG C.
Step 2) in by step 1) concrete operations of drying of the phenolic resin blend that obtains are: by step 1) phenolic resin blend that the obtains convection oven that is placed in 60 ~ 90 DEG C places 20 ~ 50 minutes.
Step 3) concrete operations be: by step 2) phenolic resin film of Resin film infusion that obtains carries out compound with fibre reinforcement material after four hot-rollings heating, and then rolling, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 70 ~ 105 DEG C, the linear velocity of hot-rolling is 1 ~ 3 m/min, and the temperature of cold roller is 10 ~ 20 DEG C.
The present invention has following beneficial effect:
Hot melt process resol preimpregnation material of the present invention is by fibre reinforcement material, heat-reactive phenolic resin, membrane-forming agent and be prepared from containing boron additive, by introducing heat-reactive phenolic resin in fibre reinforcement material, the film-forming properties of effective enhancing hot melt process resol preimpregnation material, utilize the thermotolerance improving hot melt process resol preimpregnation material containing boron additive simultaneously, thus make the hot melt process resol preimpregnation material be prepared from have the advantages that curing speed is low, thermotolerance is higher, solidification value is less than 75 ~ 105 DEG C.Simultaneously in preparation process, only need by by heat-reactive phenolic resin, membrane-forming agent and be poured into sweat connecting machine containing the phenolic resin blend that boron additive is prepared from and be prepared into phenolic resin film, then phenolic resin film and fibre reinforcement material are carried out compound, described hot melt process resol preimpregnation material can be obtained, preparation method is simple, and practicality is stronger.In addition, the matrix material adopting hot melt process resol preimpregnation material of the present invention to be prepared from, has excellent resistance toheat and mechanical property, can meet the application in the national defence such as aircraft, spacecraft and yacht and civil area.
Embodiment
Being described in further detail the present invention below in conjunction with specific embodiment, is below explanation of the invention instead of restriction.
Hot melt process resol preimpregnation material of the present invention by fibre reinforcement material and by mass fraction be the heat-reactive phenolic resin of 50 ~ 100 parts, being prepared from containing boron additive of the membrane-forming agent of 1 ~ 10 part and 1 ~ 10 part, wherein, the mass ratio of fibre reinforcement material and heat-reactive phenolic resin is 1 ~ 3:1.
Described heat-reactive phenolic resin is one or more mixtures mixed in any proportion in ba phenolic resin, Mo-phenolic resin, W-phenolic resin, ammonia resol, phosphorous-containing phenolic resin, phenol cyanate resin and benzoxazine colophony.
Described membrane-forming agent is one or more mixtures mixed in any proportion in PAUR, polyether(poly)urethane, aliphatic polyurethane, acroleic acid polyurethane, aromatic urethane, end amido liquid acrylonitrile butadiene rubber, hydroxyl terminated butyl nitrile (HTBN) rubber, epoxy terminated paracril, nbr carboxyl terminal, polyethersulfone, polysulfones, poly ether imide, polyketone ether, polyphenylene oxide and polyaryletherketone.
Described is inorganic compounds of boron boric acid containing boron additive, boron oxide, borax, Sodium Tetraborate, phenyl-boron dihydroxide, diphenyl-borinic acids, naphthalene boronic acids, luxuriant and rich with fragrance boric acid, anthracene boric acid, benzyloxy phenylo boric acid, hydroxybenzene boric acid, methylol phenylo boric acid, isopropylphenylboronic acid, phenetole boric acid, dibromobenzene boric acid, dichlorobenzene boric acid, ethylbenzene boric acid, Carboxybenzeneboronic acid, aryl boron bakelite resin, one or more mixtures mixed in any proportion of thermosetting boron-containing phenolic resin and thermoplasticity boron bakelite resin.
Described fibre reinforcement material is by a kind of plain weave of braiding in high-strength glass fibre, high-elastic glass fibre, aromatic polyamide fibre, carbon fiber, boron fibre, aramid fiber, high molecular weight polyethylene fiber, human relations fiber difficult to understand and basalt fibre or the woven fiber glass of twill or carbon cloth.
Embodiment one
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) woven fiber glass of the plain weave of high-strength glass fibre braiding is taken, ba phenolic resin, acroleic acid polyurethane and inorganic compounds of boron boric acid, ba phenolic resin is added in reaction flask, and be heated to 65 DEG C and make ba phenolic resin melting, wherein, acroleic acid polyurethane and inorganic compounds of boron boric acid is added in heat-processed, constant temperature stirs 120 minutes again, the rotating speed of ba phenolic resin in reaction flask is made to be 400 revs/min, obtain phenolic resin blend, then phenolic resin blend described in freezing, wherein, ba phenolic resin, the mass fraction of acroleic acid polyurethane and inorganic compounds of boron boric acid is respectively 100 parts, 4 parts and 4.5 parts, the woven fiber glass of plain weave and the mass ratio of ba phenolic resin of high-strength glass fibre braiding are 2:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 60 DEG C places 20 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 70 DEG C, film forming linear velocity is 2 ms/min, cold plate temperature is 20 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) woven fiber glass of plain weave that weaves of the phenolic resin film of Resin film infusion that obtains and high-strength glass fibre carries out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 80 DEG C, the linear velocity of hot-rolling is 2 ms/min, and the temperature of cold roller is 10 DEG C.
Embodiment two
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) carbon cloth of the plain weave of carbon fiber knit is taken, ba phenolic resin, polyether(poly)urethane and Carboxybenzeneboronic acid, ba phenolic resin is added in reaction flask, and be heated to 65 DEG C and make Mo-phenolic resin melting, wherein, polyether(poly)urethane and Carboxybenzeneboronic acid is added in heat-processed, constant temperature stirs 90 minutes again, the rotating speed of ba phenolic resin in reaction flask is made to be 380 revs/min, obtain phenolic resin blend, then phenolic resin blend described in freezing, wherein, ba phenolic resin, polyether(poly)urethane and be respectively 100 parts containing the mass fraction of Carboxybenzeneboronic acid, 8 parts and 6.5 parts, the carbon cloth of the plain weave of carbon fiber knit and the mass ratio of ba phenolic resin are 1:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 60 DEG C places 25 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 65 DEG C, film forming linear velocity is 1 m/min, cold plate temperature is 15 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) carbon cloth of the phenolic resin film of Resin film infusion that obtains and the plain weave of carbon fiber knit carries out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 75 DEG C, the linear velocity of hot-rolling is 1 m/min, and the temperature of cold roller is 10 DEG C.
Embodiment three
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) woven fiber glass of the plain weave of aromatic polyamide fibre braiding is taken, W-phenolic resin, PAUR and boron oxide, W-phenolic resin is added in reaction flask, and be heated to 60 DEG C and make W-phenolic resin melting, wherein, PAUR and boron oxide is added in heat-processed, constant temperature stirs 80 minutes again, the rotating speed of W-phenolic resin in reaction flask is made to be 100 revs/min, obtain phenolic resin blend, then phenolic resin blend described in freezing, wherein, W-phenolic resin, the mass fraction of PAUR and boron oxide is respectively 50 parts, 1 part and 1 part, the woven fiber glass of plain weave and the mass ratio of W-phenolic resin of aromatic polyamide fibre braiding are 1:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 90 DEG C places 50 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 95 DEG C, film forming linear velocity is 3 ms/min, cold plate temperature is 20 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) woven fiber glass of plain weave that weaves of the phenolic resin film of Resin film infusion that obtains and aromatic polyamide fibre carries out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 70 DEG C, the linear velocity of hot-rolling is 1 m/min, and the temperature of cold roller is 10 DEG C.
Embodiment four
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) woven fiber glass of the plain weave of carbon fiber knit is taken, ammonia resol, aliphatic polyurethane and borax, ammonia resol is added in reaction flask, and be heated to 90 DEG C and make the melting of ammonia resol, wherein, aliphatic polyurethane and borax is added in heat-processed, constant temperature stirs 240 minutes again, the rotating speed of ammonia resol in reaction flask is made to be 500 revs/min, obtain phenolic resin blend, then phenolic resin blend described in freezing, wherein, ammonia resol, the mass fraction of aliphatic polyurethane and borax is respectively 100 parts, 10 parts and 10 parts, the woven fiber glass of the plain weave of carbon fiber knit and the mass ratio of ammonia resol are 3:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 60 DEG C places 20 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 60 DEG C, film forming linear velocity is 1 m/min, cold plate temperature is 10 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) woven fiber glass of the phenolic resin film of Resin film infusion that obtains and the plain weave of carbon fiber knit carries out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 105 DEG C, the linear velocity of hot-rolling is 3 ms/min, and the temperature of cold roller is 20 DEG C.
Embodiment five
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) woven fiber glass of the plain weave of boron fibre braiding is taken, phosphorous-containing phenolic resin, aromatic urethane and Sodium Tetraborate, phosphorous-containing phenolic resin is added in reaction flask, and be heated to 65 DEG C and make phosphorous-containing phenolic resin melting, wherein, aromatic urethane and Sodium Tetraborate is added in heat-processed, constant temperature stirs 90 minutes again, the rotating speed of phosphorous-containing phenolic resin in reaction flask is made to be 150 revs/min, obtain phenolic resin blend, then phenolic resin blend described in freezing, wherein, phosphorous-containing phenolic resin, the mass fraction of aromatic urethane and Sodium Tetraborate is respectively 60 parts, 2 parts and 3 parts, the woven fiber glass of plain weave and the mass ratio of phosphorous-containing phenolic resin of boron fibre braiding are 1.2:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 65 DEG C places 25 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 63 DEG C, film forming linear velocity is 1.2 ms/min, cold plate temperature is 12 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) woven fiber glass of plain weave that weaves of the phenolic resin film of Resin film infusion that obtains and boron fibre carries out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 75 DEG C, the linear velocity of hot-rolling is 1.3 ms/min, and the temperature of cold roller is 15 DEG C.
Embodiment six
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) the twill woven fiber glass of aramid fiber braiding is taken, phenol cyanate resin, end amido liquid acrylonitrile butadiene rubber and phenyl-boron dihydroxide, phenol cyanate resin is added in reaction flask, and be heated to 70 DEG C and make the melting of phenol cyanate resin, wherein, end amido liquid acrylonitrile butadiene rubber and phenyl-boron dihydroxide is added in heat-processed, constant temperature stirs 90 minutes again, the rotating speed of phenol cyanate resin in reaction flask is made to be 150 revs/min, obtain phenolic resin blend, then phenolic resin blend described in freezing, wherein, phenol cyanate resin, the mass fraction of end amido liquid acrylonitrile butadiene rubber and phenyl-boron dihydroxide is respectively 70 parts, 3 parts and 10 parts, the twill woven fiber glass of aramid fiber braiding and the mass ratio of phenol cyanate resin are 1.5:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 70 DEG C places 30 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 70 DEG C, film forming linear velocity is 1.5 ms/min, cold plate temperature is 15 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) the twill woven fiber glass that weaves of the phenolic resin film of Resin film infusion that obtains and aramid fiber carries out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 80 DEG C, the linear velocity of hot-rolling is 2 ms/min, and the temperature of cold roller is 12 DEG C.
Embodiment seven
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) the twill woven fiber glass of high molecular weight polyethylene fiber braiding is taken, benzoxazine colophony, hydroxyl terminated butyl nitrile (HTBN) rubber and diphenyl-borinic acids, benzoxazine colophony is added in reaction flask, and be heated to 75 DEG C and make benzoxazine colophony melting, wherein, hydroxyl terminated butyl nitrile (HTBN) rubber and diphenyl-borinic acids is added in heat-processed, constant temperature stirs 100 minutes again, the rotating speed of benzoxazine colophony in reaction flask is made to be 150 revs/min, obtain phenolic resin blend, then phenolic resin blend described in freezing, wherein, benzoxazine colophony, the mass fraction of hydroxyl terminated butyl nitrile (HTBN) rubber and diphenyl-borinic acids is respectively 100 parts, 3 parts and 5 parts, the twill woven fiber glass of high molecular weight polyethylene fiber braiding and the mass ratio of heat-reactive phenolic resin are 2:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 80 DEG C places 30 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 80 DEG C, film forming linear velocity is 2.5 ms/min, cold plate temperature is 12 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) the twill woven fiber glass that weaves of the phenolic resin film of Resin film infusion that obtains and high molecular weight polyethylene fiber carries out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 85 DEG C, the linear velocity of hot-rolling is 2 ms/min, and the temperature of cold roller is 16 DEG C.
Embodiment eight
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) the twill woven fiber glass of human relations fibrage difficult to understand is taken, benzoxazine and ba phenolic resin mixture in any proportion, epoxy terminated paracril and naphthalene boronic acids, benzoxazine and ba phenolic resin mixture are in any proportion added in reaction flask, and be heated to 85 DEG C and make the mixture melting in any proportion of benzoxazine and ba phenolic resin, wherein, epoxy terminated paracril and naphthalene boronic acids is added in heat-processed, constant temperature stirs 180 minutes again, the rotating speed of benzoxazine and ba phenolic resin mixture in any proportion in reaction flask is made to be 300 revs/min, obtain phenolic resin blend, then phenolic resin blend described in freezing, wherein, benzoxazine and ba phenolic resin, the mass fraction of epoxy terminated paracril and naphthalene boronic acids is respectively 50 parts, 10 parts and 10 parts, the twill woven fiber glass of human relations fibrage difficult to understand and the mass ratio of PAUR and polyether(poly)urethane mixture are in any proportion 3:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 85 DEG C places 45 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 85 DEG C, film forming linear velocity is 2.5 ms/min, cold plate temperature is 18 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) phenolic resin film of Resin film infusion that obtains and the twill woven fiber glass of human relations fibrage difficult to understand carry out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 90 DEG C, the linear velocity of hot-rolling is 2.5 ms/min, and the temperature of cold roller is 18 DEG C.
Embodiment nine
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) the twill carbon cloth of basalt fibre braiding is taken, the mixture that ba phenolic resin mixes in any proportion with Mo-phenolic resin and W-phenolic resin, nbr carboxyl terminal and luxuriant and rich with fragrance boric acid, by ba phenolic resin, the mixture that Mo-phenolic resin and W-phenolic resin mix in any proportion adds in reaction flask, and be heated to 80 DEG C and make ba phenolic resin, the mixture melting that Mo-phenolic resin and W-phenolic resin mix in any proportion, wherein, nbr carboxyl terminal and luxuriant and rich with fragrance boric acid is added in heat-processed, constant temperature stirs 200 minutes again, make ba phenolic resin in reaction flask, the rotating speed of the mixture that Mo-phenolic resin and W-phenolic resin mix in any proportion is 350 revs/min, obtain phenolic resin blend, then phenolic resin blend described in freezing, wherein, the mixture that ba phenolic resin mixes in any proportion with Mo-phenolic resin and W-phenolic resin, the mass fraction of nbr carboxyl terminal and luxuriant and rich with fragrance boric acid is respectively 70 parts, 8 parts and 8 parts, the twill carbon cloth of basalt fibre braiding and ba phenolic resin, the mass ratio of the mixture that Mo-phenolic resin and W-phenolic resin mix in any proportion is 2.5:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 85 DEG C places 45 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 90 DEG C, film forming linear velocity is 2.8 ms/min, cold plate temperature is 18 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) the capable compound of twill carbon cloth that weaves of the phenolic resin film of Resin film infusion that obtains and basalt fibre, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 100 DEG C, the linear velocity of hot-rolling is 2.5 ms/min, and the temperature of cold roller is 18 DEG C.
Embodiment ten
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) the twill carbon cloth of basalt fibre braiding is taken, ba phenolic resin and Mo-phenolic resin, the mixture that W-phenolic resin and ammonia resol mix in any proportion, polysulfones and anthracene boric acid, by ba phenolic resin, Mo-phenolic resin, the mixture that W-phenolic resin and ammonia resol mix in any proportion adds in reaction flask, and is heated to 90 DEG C and makes ba phenolic resin, Mo-phenolic resin, the mixture melting that W-phenolic resin and ammonia resol mix in any proportion, wherein, add polysulfones and anthracene boric acid, then constant temperature stirs 230 minutes, make ba phenolic resin in reaction flask in heat-processed, Mo-phenolic resin, the rotating speed of the mixture that W-phenolic resin and ammonia resol mix in any proportion is 450 revs/min, obtains phenolic resin blend, then phenolic resin blend described in freezing, wherein, and ba phenolic resin, Mo-phenolic resin, the mixture that W-phenolic resin and ammonia resol mix in any proportion, the mass fraction of polysulfones and anthracene boric acid is respectively 50 parts, 1 part and 9 parts, the twill carbon cloth of basalt fibre braiding and ba phenolic resin, Mo-phenolic resin, the mass ratio of the mixture that W-phenolic resin and ammonia resol mix in any proportion is 3:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 60 DEG C places 50 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 95 DEG C, film forming linear velocity is 2.8 ms/min, cold plate temperature is 18 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) the twill carbon cloth that weaves of the phenolic resin film of Resin film infusion that obtains and basalt fibre carries out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 105 DEG C, the linear velocity of hot-rolling is 2.8 ms/min, and the temperature of cold roller is 20 DEG C.
Embodiment 11
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) the twill carbon cloth of basalt fibre braiding is taken, ba phenolic resin and Mo-phenolic resin, W-phenolic resin, the mixture that ammonia resol and phosphorous-containing phenolic resin mix in any proportion, poly ether imide and benzyloxy phenylo boric acid, by ba phenolic resin, Mo-phenolic resin, W-phenolic resin, the mixture that ammonia resol and phosphorous-containing phenolic resin mix in any proportion adds in reaction flask, and is heated to 75 DEG C and makes ba phenolic resin, Mo-phenolic resin, W-phenolic resin, the mixture melting that ammonia resol and phosphorous-containing phenolic resin mix in any proportion, wherein, add poly ether imide and benzyloxy phenylo boric acid, then constant temperature stirs 220 minutes, make ba phenolic resin in reaction flask in heat-processed, Mo-phenolic resin, W-phenolic resin, the rotating speed of the mixture that ammonia resol and phosphorous-containing phenolic resin mix in any proportion is 350 revs/min, obtains phenolic resin blend, then phenolic resin blend described in freezing, wherein, and ba phenolic resin, Mo-phenolic resin, W-phenolic resin, the mixture that ammonia resol and phosphorous-containing phenolic resin mix in any proportion, the mass fraction of poly ether imide and benzyloxy phenylo boric acid is respectively 100 parts, 2 parts and 2 parts, the twill carbon cloth of basalt fibre braiding and ba phenolic resin, Mo-phenolic resin, W-phenolic resin, the mass ratio of the mixture that ammonia resol and phosphorous-containing phenolic resin mix in any proportion is 3:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 75 DEG C places 35 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 90 DEG C, film forming linear velocity is 1.5 ms/min, cold plate temperature is 18 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) the twill carbon cloth that weaves of the phenolic resin film of Resin film infusion that obtains and basalt fibre carries out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 90 DEG C, the linear velocity of hot-rolling is 2.6 ms/min, and the temperature of cold roller is 12 DEG C.
Embodiment 12
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) the plain weave glass cloth of human relations fibrage difficult to understand is taken, ba phenolic resin and Mo-phenolic resin, W-phenolic resin, ammonia resol, the mixture that phosphorous-containing phenolic resin and phenol cyanate resin mix in any proportion, polyketone ether and hydroxybenzene boric acid, by ba phenolic resin, Mo-phenolic resin, W-phenolic resin, ammonia resol, the mixture that phosphorous-containing phenolic resin and phenol cyanate resin mix in any proportion adds in reaction flask, and is heated to 63 DEG C and makes ba phenolic resin, Mo-phenolic resin, W-phenolic resin, ammonia resol, the mixture melting that phosphorous-containing phenolic resin and phenol cyanate resin mix in any proportion, wherein, add polyketone ether and hydroxybenzene boric acid, then constant temperature stirs 85 minutes, make ba phenolic resin in reaction flask in heat-processed, Mo-phenolic resin, W-phenolic resin, ammonia resol, the rotating speed of the mixture that phosphorous-containing phenolic resin and phenol cyanate resin mix in any proportion is 180 revs/min, obtains phenolic resin blend, then phenolic resin blend described in freezing, wherein, and ba phenolic resin and Mo-phenolic resin, W-phenolic resin, ammonia resol, the mixture that phosphorous-containing phenolic resin and phenol cyanate resin mix in any proportion, the mass fraction of polyketone ether and hydroxybenzene boric acid is respectively 50 parts, 6 parts and 9 parts, the plain weave glass cloth of human relations fibrage difficult to understand and ba phenolic resin, Mo-phenolic resin, W-phenolic resin, ammonia resol, the mass ratio of the mixture that phosphorous-containing phenolic resin and phenol cyanate resin mix in any proportion is 3:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 75 DEG C places 25 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 65 DEG C, film forming linear velocity is 1.6 ms/min, cold plate temperature is 11 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) phenolic resin film of Resin film infusion that obtains and the plain weave glass cloth of human relations fibrage difficult to understand carries out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 75 DEG C, the linear velocity of hot-rolling is 3 ms/min, and the temperature of cold roller is 18 DEG C.
Embodiment 13
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) high-elastic fiberglass braided plain weave glass cloth is taken, ba phenolic resin and Mo-phenolic resin, W-phenolic resin, ammonia resol, phosphorous-containing phenolic resin, the mixture that phenol cyanate resin and benzoxazine colophony mix in any proportion, polyphenylene oxide and isopropylphenylboronic acid, by ba phenolic resin, Mo-phenolic resin, W-phenolic resin, ammonia resol, phosphorous-containing phenolic resin, the mixture that phenol cyanate resin and benzoxazine colophony mix in any proportion adds in reaction flask, and is heated to 89 DEG C and makes ba phenolic resin, Mo-phenolic resin, W-phenolic resin, ammonia resol, phosphorous-containing phenolic resin, the mixture melting that phenol cyanate resin and benzoxazine colophony mix in any proportion, wherein, add polyphenylene oxide and isopropylphenylboronic acid in heat-processed, then constant temperature stirs 85 minutes, makes ba phenolic resin in reaction flask, Mo-phenolic resin, W-phenolic resin, ammonia resol, phosphorous-containing phenolic resin, the rotating speed of the mixture that phenol cyanate resin and benzoxazine colophony mix in any proportion is 260 revs/min, obtains phenolic resin blend, then phenolic resin blend described in freezing, wherein, and ba phenolic resin and Mo-phenolic resin, W-phenolic resin, ammonia resol, phosphorous-containing phenolic resin, the mixture that phenol cyanate resin and benzoxazine colophony mix in any proportion, the mass fraction of polyphenylene oxide and isopropylphenylboronic acid is respectively 50 parts, 9 parts and 9 parts, high-elastic fiberglass braided plain weave glass cloth and ba phenolic resin, Mo-phenolic resin, W-phenolic resin, ammonia resol, phosphorous-containing phenolic resin, the mass ratio of the mixture that phenol cyanate resin and benzoxazine colophony mix in any proportion is 1.8:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 65 DEG C places 25 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 78 DEG C, film forming linear velocity is 1.9 ms/min, cold plate temperature is 14 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) phenolic resin film of Resin film infusion that obtains and high-elastic fiberglass braided plain weave glass cloth carries out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 74 DEG C, the linear velocity of hot-rolling is 1.9 ms/min, and the temperature of cold roller is 15 DEG C.
Embodiment 14
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) the plain weave glass cloth of carbon fiber knit is taken, Mo-phenolic resin, polyaryletherketone and isopropylphenylboronic acid, Mo-phenolic resin is added in reaction flask, and be heated to 65 DEG C and make Mo-phenolic resin melting, wherein, polyaryletherketone and isopropylphenylboronic acid is added in heat-processed, constant temperature stirs 89 minutes again, the rotating speed of Mo-phenolic resin in reaction flask is made to be 480 revs/min, obtain phenolic resin blend, then phenolic resin blend described in freezing, wherein, Mo-phenolic resin, the mass fraction of polyaryletherketone and isopropylphenylboronic acid is respectively 60 parts, 10 parts and 10 parts, the plain weave glass cloth of carbon fiber knit and the mass ratio of Mo-phenolic resin are 3:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 65 DEG C places 36 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 86 DEG C, film forming linear velocity is 1 m/min, cold plate temperature is 20 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) phenolic resin film of Resin film infusion that obtains and the plain weave glass cloth of carbon fiber knit carries out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 100 DEG C, the linear velocity of hot-rolling is 1 m/min, and the temperature of cold roller is 12 DEG C.
Embodiment 15
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) the plain weave glass cloth of aramid fiber braiding is taken, phenol cyanate resin, the mixture that PAUR and polyether(poly)urethane mix in any proportion and phenetole boric acid, phenol cyanate resin is added in reaction flask, and be heated to 78 DEG C and make the melting of phenol cyanate resin, wherein, mixture and phenetole boric acid that PAUR and polyether(poly)urethane mix in any proportion is added in heat-processed, constant temperature stirs 85 minutes again, the rotating speed of phenol cyanate resin in reaction flask is made to be 200 revs/min, obtain phenolic resin blend, then phenolic resin blend described in freezing, wherein, phenol cyanate resin, the mass fraction of the mixture that PAUR and polyether(poly)urethane mix in any proportion and phenetole boric acid is respectively 100 parts, 1 part and 1 part, the plain weave glass cloth of aramid fiber braiding and the mass ratio of phenol cyanate resin are 1:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 3 DEG C places 20 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 60 DEG C, film forming linear velocity is 1 m/min, cold plate temperature is 20 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) the plain weave glass cloth that weaves of the phenolic resin film of Resin film infusion that obtains and aramid fiber carries out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 105 DEG C, the linear velocity of hot-rolling is 1 m/min, and the temperature of cold roller is 15 DEG C.
Embodiment 16
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) the plain weave glass cloth of human relations fibrage difficult to understand is taken, phenol cyanate resin, poly ether imide and polyketone ether, the mixture that polyphenylene oxide and polyaryletherketone mix in any proportion and phenetole boric acid, dibromobenzene boric acid, dichlorobenzene boric acid, ethylbenzene boric acid, Carboxybenzeneboronic acid, aryl boron bakelite resin, the mixture that thermosetting boron-containing phenolic resin and thermoplasticity boron bakelite resin mix in any proportion, adds phenol cyanate resin in reaction flask, and is heated to 86 DEG C and makes the melting of phenol cyanate resin, wherein, in heat-processed, adds poly ether imide, polyketone ether, the mixture that polyphenylene oxide and polyaryletherketone mix in any proportion and phenetole boric acid, dibromobenzene boric acid, dichlorobenzene boric acid, ethylbenzene boric acid, Carboxybenzeneboronic acid, aryl boron bakelite resin, the mixture that thermosetting boron-containing phenolic resin and thermoplasticity boron bakelite resin mix in any proportion, then constant temperature stirs 85 minutes, makes the rotating speed of phenol cyanate resin in reaction flask be 100 revs/min, obtain phenolic resin blend, then phenolic resin blend described in freezing, wherein, phenol cyanate resin, the mixture that poly ether imide and polyketone ether and polyphenylene oxide and polyaryletherketone mix in any proportion and phenetole boric acid, dibromobenzene boric acid, dichlorobenzene boric acid, ethylbenzene boric acid, Carboxybenzeneboronic acid, aryl boron bakelite resin, the mass fraction of the mixture that thermosetting boron-containing phenolic resin and thermoplasticity boron bakelite resin mix in any proportion is respectively 50 parts, 10 parts and 10 parts, the plain weave glass cloth of human relations fibrage difficult to understand and the mass ratio of phenol cyanate resin are 3:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 80 DEG C places 30 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 80 DEG C, film forming linear velocity is 2 ms/min, cold plate temperature is 15 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) phenolic resin film of Resin film infusion that obtains and the plain weave glass cloth of human relations fibrage difficult to understand carries out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 105 DEG C, the linear velocity of hot-rolling is 1 m/min, and the temperature of cold roller is 20 DEG C.
Embodiment 17
The preparation method of hot melt process resol preimpregnation material of the present invention comprises the following steps:
1) the plain weave carbon cloth of human relations fibrage difficult to understand is claimed, benzoxazine colophony, the mixture that PAUR and polyether(poly)urethane mix in any proportion and the mixture that methylol phenylo boric acid mixes in any proportion with isopropylphenylboronic acid, benzoxazine colophony is added in reaction flask, and be heated to 75 DEG C and make benzoxazine colophony melting, wherein, mixture that PAUR and polyether(poly)urethane mix in any proportion and the mixture that methylol phenylo boric acid mixes in any proportion with isopropylphenylboronic acid is added in heat-processed, constant temperature stirs 100 minutes again, the rotating speed of benzoxazine colophony in reaction flask is made to be 500 revs/min, obtain phenolic resin blend, then phenolic resin blend described in freezing, wherein, benzoxazine colophony, the mass fraction of the mixture that PAUR and polyether(poly)urethane mix in any proportion and the mixture that methylol phenylo boric acid mixes in any proportion with isopropylphenylboronic acid is respectively 50 parts, 8 parts and 8 parts, the plain weave carbon cloth of human relations fibrage difficult to understand and the mass ratio of benzoxazine colophony are 2:1,
2) by step 1) phenolic resin blend that the obtains convection oven that is placed in 80 DEG C places 30 minutes, then pour in sweat connecting machine and make resin molding, wherein, the temperature of sweat connecting machine is 80 DEG C, film forming linear velocity is 2 ms/min, cold plate temperature is 15 DEG C, then is cooled to room temperature, obtains the phenolic resin film of Resin film infusion;
3) by step 2) phenolic resin film of Resin film infusion that obtains and the plain weave carbon cloth of human relations fibrage difficult to understand carry out compound, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 80 DEG C, the linear velocity of hot-rolling is 2 ms/min, and the temperature of cold roller is 15 DEG C.
In embodiment one, the performance perameter of tego film and hot melt process resol preimpregnation material is as shown in table 1:
Table 1
In embodiment two, the performance perameter of tego film and hot melt process resol preimpregnation material is as shown in table 2:
Table 2
Claims (10)
1. a hot melt process resol preimpregnation material, it is characterized in that, by fibre reinforcement material and by mass fraction be the heat-reactive phenolic resin of 50 ~ 100 parts, being prepared from containing boron additive of the membrane-forming agent of 1 ~ 10 part and 1 ~ 10 part, wherein, the mass ratio of fibre reinforcement material and heat-reactive phenolic resin is 1 ~ 3:1.
2. hot melt process resol preimpregnation material according to claim 1, it is characterized in that, described heat-reactive phenolic resin is one or more mixtures mixed in any proportion in ba phenolic resin, Mo-phenolic resin, W-phenolic resin, ammonia resol, phosphorous-containing phenolic resin, phenol cyanate resin and benzoxazine colophony.
3. hot melt process resol preimpregnation material according to claim 1, it is characterized in that, described membrane-forming agent is one or more mixtures mixed in any proportion in PAUR, polyether(poly)urethane, aliphatic polyurethane, acroleic acid polyurethane, aromatic urethane, end amido liquid acrylonitrile butadiene rubber, hydroxyl terminated butyl nitrile (HTBN) rubber, epoxy terminated paracril, nbr carboxyl terminal, polyethersulfone, polysulfones, poly ether imide, polyketone ether, polyphenylene oxide and polyaryletherketone.
4. hot melt process resol preimpregnation material according to claim 1, it is characterized in that, described is inorganic compounds of boron boric acid containing boron additive, boron oxide, borax, Sodium Tetraborate, phenyl-boron dihydroxide, diphenyl-borinic acids, naphthalene boronic acids, luxuriant and rich with fragrance boric acid, anthracene boric acid, benzyloxy phenylo boric acid, hydroxybenzene boric acid, methylol phenylo boric acid, isopropylphenylboronic acid, phenetole boric acid, dibromobenzene boric acid, dichlorobenzene boric acid, ethylbenzene boric acid, Carboxybenzeneboronic acid, aryl boron bakelite resin, one or more mixtures mixed in any proportion of thermosetting boron-containing phenolic resin and thermoplasticity boron bakelite resin.
5. hot melt process resol preimpregnation material according to claim 1, it is characterized in that, described fibre reinforcement material is by a kind of plain weave of braiding in high-strength glass fibre, high-elastic glass fibre, aromatic polyamide fibre, carbon fiber, boron fibre, aramid fiber, high molecular weight polyethylene fiber, human relations fiber difficult to understand and basalt fibre or the woven fiber glass of twill or carbon cloth.
6. a preparation method for hot melt process resol preimpregnation material, is characterized in that, comprise the following steps:
1) take fibre reinforcement material, heat-reactive phenolic resin, membrane-forming agent by claim 1 and contain boron additive, heat-reactive phenolic resin is joined in reaction flask, and be heated to molten state, wherein, in heat-processed, add membrane-forming agent and contain boron additive, constant temperature stirs again, obtains phenolic resin blend, then phenolic resin blend described in freezing;
2) by step 1) phenolic resin blend that obtains dries, then pours in sweat connecting machine and make resin molding, then be cooled to room temperature, obtain the phenolic resin film of Resin film infusion;
3) by step 2) phenolic resin film of Resin film infusion that obtains and fibre reinforcement material carry out compound, obtains hot melt process resol preimpregnation material.
7. the preparation method of hot melt process resol preimpregnation material according to claim 6, is characterized in that,
Step 1) in heat-reactive phenolic resin is added in reaction flask, and the concrete operations being heated to molten state are: added in reaction flask by heat-reactive phenolic resin, and are heated to 60 ~ 90 DEG C and make heat-reactive phenolic resin melting;
Step 1) in the process that stirs of constant temperature in reaction flask the rotating speed of heat-reactive phenolic resin be 100 ~ 500 revs/min, the time that constant temperature stirs is 80 ~ 240 minutes.
8. the preparation method of hot melt process resol preimpregnation material according to claim 6, it is characterized in that, by step 1) phenolic resin blend that obtains dries, then the temperature pouring sweat connecting machine in the process making resin molding in sweat connecting machine into is 60 ~ 95 DEG C, film forming linear velocity is 1 ~ 3 m/min, and cold plate temperature is 10 ~ 20 DEG C.
9. the preparation method of hot melt process resol preimpregnation material according to claim 6, it is characterized in that, step 2) in by step 1) concrete operations of drying of the phenolic resin blend that obtains are: by step 1) phenolic resin blend that the obtains convection oven that is placed in 60 ~ 90 DEG C places 20 ~ 50 minutes.
10. the preparation method of hot melt process resol preimpregnation material according to claim 6, it is characterized in that, step 3) concrete operations be: by step 2) phenolic resin film of Resin film infusion that obtains carries out compound with fibre reinforcement material after four hot-rollings heating, and then rolling, obtain hot melt process resol preimpregnation material, wherein, in recombination process, the temperature of hot-rolling is 70 ~ 105 DEG C, the linear velocity of hot-rolling is 1 ~ 3 m/min, and the temperature of cold roller is 10 ~ 20 DEG C.
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