CN104629255B - A kind of BN strengthens the preparation method of carbon fiber modifying melamine resin material - Google Patents
A kind of BN strengthens the preparation method of carbon fiber modifying melamine resin material Download PDFInfo
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- CN104629255B CN104629255B CN201510030260.8A CN201510030260A CN104629255B CN 104629255 B CN104629255 B CN 104629255B CN 201510030260 A CN201510030260 A CN 201510030260A CN 104629255 B CN104629255 B CN 104629255B
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Abstract
The invention discloses the preparation method that a kind of BN strengthens carbon fiber modifying melamine resin material, comprise the following steps：Carbon fiber, polyvinyl alcohol, boron chloride, HMDS are put into the first reaction vessel and carry out ultrasonically treated obtaining material A, the second reaction vessel is put into after material A is dried, second reaction vessel is full of after nitrogen, gradually heating up and being incubated obtains BN enhancing carbon fibers；Silane coupler KH 791, microcrystalline wax, butyl stearate are added again and heat up and continue to stir after melamine resin, organic siliconresin, polyethylene to add after stirring in BN enhancing carbon fibers, stirring after dioctyl phthalate, epoxidized soybean oil, mica powder, talcum powder, zinc oxide is added and obtains mixed material；Mixed material is moved to BN enhancing carbon fiber modifying melamine resin materials are obtained after double screw extruder, melting extrusion.
Description
Technical field
The present invention relates to melamine resin field of material technology, more particularly to a kind of BN enhancing carbon fiber modifyings three
The preparation method of melamine-formaldehyde resin material.
Background technology
Melamine resin is a kind of thermosetting resin of excellent performance made from melamine and formaldehyde reaction,
With excellent stability, heat resistance, electrical insulating property, self-extinguishment, arc resistance and good mechanical property, electricity is often applied to
Cable processing industry, however, while good material chemical property is possessed, its toughness, intensity are poor, it is impossible to meet cable processing
To the requirement of raw material high tenacity, high intensity in industry.
The content of the invention
The technical problem existed based on background technology, the present invention proposes a kind of BN enhancings carbon fiber modifying melamine first
The preparation method of urea formaldehyde material, obtained melamine resin toughness of material is good, intensity is high, disclosure satisfy that cable is processed
Industry is to raw material high tenacity, the demand of high intensity.
A kind of preparation method of BN enhancings carbon fiber modifying melamine resin material proposed by the present invention, including with
Lower step：
S1, by weight by 5-8 carbon fibers, 2-2.5 polyvinyl alcohol, 3-6 parts of boron chlorides, the 3-6 parts of silicon nitrogen of hexamethyl two
Alkane, which is put into the first reaction vessel, to carry out ultrasonically treated 25-30min and obtains material A, and ultrasonically treated frequency is 35-38KHz, is surpassed
The power of sonication is 1300-1500W, material A is taken out into drying, dry temperature is 65-75 DEG C, is then placed in the second reaction
Container, the second reaction vessel is full of after nitrogen, and the second reaction vessel and its content are raised by 5-7 DEG C/min programming rate
Temperature is to 720-750 DEG C, and insulation 2-3h obtains BN enhancing carbon fibers；
S2, by weight by KH-791,0.2-0.5 parts of microcrystalline waxes of 1.2-1.5 parts of silane couplers, 0.1-0.3 parts it is hard
Resin acid butyl ester is added to stir in 13-16 parts of BN enhancing carbon fibers, adds 45-48 parts of melamine resins, 21-24
Part organic siliconresin, 13-15 parts of polyethylene, are warming up to 140-145 DEG C, stir, add 2.2-2.5 parts of phthalic acids
Dioctyl ester, 1.1-1.4 part epoxidized soybean oil, 6-9 parts of mica powders, 3-5 parts of talcum powder, 2-2.5 parts of zinc oxide, after stirring
To mixed material；Mixed material is moved to BN enhancing carbon fiber modifying melamines are obtained after double screw extruder, melting extrusion
Formaldehyde resin materials, the extrusion zone temperature of double screw extruder is respectively：144-147℃、153-158℃、165-170℃、
174-177 DEG C, 180-183 DEG C, head temperature is 192-202 DEG C, and double screw extruder rotating speed is 280-310r/min.
Preferably, in S1, carbon fiber is the polyacrylonitrile-based carbon fibre that modulus of elasticity is 230-250GPa.
Preferably, in S1, by weight by 6-7 carbon fibers, 2.2-2.4 polyvinyl alcohol, 4-5 parts of boron chlorides, 4-5 parts six
Methyl disilazane, which is put into the first reaction vessel, to carry out ultrasonically treated 26-28min and obtains material A, and ultrasonically treated frequency is
36-37KHz, ultrasonically treated power is 1380-1420W, and material A is taken out into drying, and dry temperature is 68-72 DEG C, then
The second reaction vessel is put into, the second reaction vessel is full of after nitrogen, is reacted by 5.5-6 DEG C/min programming rate rise second
Container and its contents temperature are to 730-740 DEG C, and insulation 2.2-2.5h obtains BN enhancing carbon fibers.
Preferably, in S1, boron chloride, the weight ratio of HMDS are 1:1.
Preferably, in S2, melamine resin, organic siliconresin, polyethylene, the weight ratio of BN enhancing carbon fibers are
46-47：22-23：13.5-14：14-15.
Preferably, in S2, by weight by KH-791,0.3-0.4 parts of microcrystalline waxes of 1.3-1.4 parts of silane couplers,
0.15-0.2 parts of butyl stearates are added to stir in 14-15 parts of BN enhancing carbon fibers, adds 46-47 parts of melamine first
Urea formaldehyde, 22-23 part organic siliconresin, 13.5-14 parts of polyethylene, are warming up to 142-143 DEG C, stir, add 2.3-
2.4 parts of dioctyl phthalates, 1.2-1.3 parts of epoxidized soybean oils, 7-8 parts of mica powders, 3.5-4 parts of talcum powder, 2.2-2.4 parts
Zinc oxide, mixed material is obtained after stirring；Mixed material is moved to BN enhancings are obtained after double screw extruder, melting extrusion
Carbon fiber modifying melamine resin material, the extrusion zone temperature of double screw extruder is respectively：145-146℃、154-
156 DEG C, 166-168 DEG C, 175-176 DEG C, 181-182 DEG C, head temperature is 196-200 DEG C, and double screw extruder rotating speed is
290-300r/min。
Present invention introduces organic siliconresin, polyethylene, BN enhancing carbon fiber modifying melamine resins, greatly improve
Toughness, intensity and the lear energy of the present invention, wherein BN enhancing carbon fiber is that carbon fiber is obtained through B, N enhancing, and carbon is fine
Tie up that intensity is high, corrosion-resistant, modulus is high and with stretching resistance is strong, excellent in mechanical performance the features such as, but it is oxidized easily and had
Have in certain electric conductivity, preparation process, boron chloride, HMDS are sonicated in the presence of polyvinyl alcohol
Carbon fiber surface is securely attached to, then by the high-temperature process reaction generation BN coatings under nitrogen protection, so that in carbon fiber
Surface has been made the BN coatings with fabulous insulating properties, and BN coatings can again be substantially increased with fabulous compatible of carbon fiber
The inoxidizability of carbon fiber, so as to substantially increase the toughness of the present invention, shock resistance, tear-resistant anti-wear performance；Phthalic acid
The Plasticising system that dioctyl ester, butyl stearate, epoxidized soybean oil are constituted, improves the plasticizing efficiency of the present invention so that the present invention
With excellent heat-resisting, oil resistant, anti-toughness, intensity and the plasticity for being swelled and resistance to migration energy, enhancing the present invention, wherein firmly
Resin acid butyl ester can also coordinate as lubricant and releasing agent with microcrystalline wax, the present invention is more easily processed；Mica powder, talcum
Powder, zinc oxide substantially increase intensity, wear resistant and impact resistant performance and the electric insulation of the present invention as the addition of reinforcing filler
Property；And on silane coupler KH-791 addition, the packing strengthening agent that BN enhancing carbon fibers and above-mentioned addition can be coated on, make it
It is evenly distributed in the present invention, substantially increases intensity, toughness and the lear energy of the present invention, meanwhile, also enhance this
The plasticity of invention.
Embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of BN enhancings carbon fiber modifying melamine resin material proposed by the present invention, including with
Lower step：
S1,8 carbon fibers, 2 polyvinyl alcohol, 3 parts of boron chlorides, 3 parts of HMDSs are put into first by weight
Ultrasonically treated 30min is carried out in reaction vessel and obtains material A, ultrasonically treated frequency is 35KHz, and ultrasonically treated power is
1500W, takes out drying, dry temperature is 65 DEG C, is then placed in the second reaction vessel, the second reaction vessel is filled by material A
After full nitrogen, the second reaction vessel and its contents temperature are raised to 720 DEG C by 7 DEG C/min programming rate, and insulation 3h is obtained
BN strengthens carbon fiber；Wherein, carbon fiber is the polyacrylonitrile-based carbon fibre that modulus of elasticity is 230GPa；
S2,1.5 parts of silane coupler KH-791,0.2 part of microcrystalline wax, 0.3 part of butyl stearate are added by weight
Stirred in 13 parts of BN enhancing carbon fibers, add 48 parts of melamine resins, 21 parts of organic siliconresins, 15 parts of poly- second
Alkene, is warming up to 140 DEG C, stirs, and adds 2.5 parts of dioctyl phthalates, 1.1 parts of epoxidized soybean oils, 9 parts of micas
Powder, 3 parts of talcum powder, 2.5 parts of zinc oxide, mixed material is obtained after stirring；Mixed material is moved into double screw extruder, melted
Melt and BN enhancing carbon fiber modifying melamine resin materials are obtained after extrusion, the extrusion zone temperature difference of double screw extruder
For：144 DEG C, 158 DEG C, 165 DEG C, 177 DEG C, 180 DEG C, head temperature is 202 DEG C, and double screw extruder rotating speed is 280r/min.
Embodiment 2
A kind of preparation method of BN enhancings carbon fiber modifying melamine resin material proposed by the present invention, including with
Lower step：
S1,5 carbon fibers, 2.5 polyvinyl alcohol, 6 parts of boron chlorides, 6 parts of HMDSs are put into by weight
Ultrasonically treated 25min is carried out in one reaction vessel and obtains material A, ultrasonically treated frequency is 38KHz, and ultrasonically treated power is
1300W, takes out drying, dry temperature is 75 DEG C, is then placed in the second reaction vessel, the second reaction vessel is filled by material A
After full nitrogen, the second reaction vessel and its contents temperature are raised to 750 DEG C by 5 DEG C/min programming rate, and insulation 2h is obtained
BN strengthens carbon fiber；Wherein, carbon fiber is the polyacrylonitrile-based carbon fibre that modulus of elasticity is 250GPa；
S2,1.2 parts of silane coupler KH-791,0.5 part of microcrystalline wax, 0.1 part of butyl stearate are added by weight
Stirred in 16 parts of BN enhancing carbon fibers, add 45 parts of melamine resins, 24 parts of organic siliconresins, 13 parts of poly- second
Alkene, is warming up to 145 DEG C, stirs, and adds 2.2 parts of dioctyl phthalates, 1.4 parts of epoxidized soybean oils, 6 parts of micas
Powder, 5 parts of talcum powder, 2 parts of zinc oxide, mixed material is obtained after stirring；Mixed material is moved into double screw extruder, melted
BN enhancing carbon fiber modifying melamine resin materials, the extrusion zone temperature difference of double screw extruder are obtained after extrusion
For：147 DEG C, 153 DEG C, 170 DEG C, 174 DEG C, 183 DEG C, head temperature is 192 DEG C, and double screw extruder rotating speed is 310r/min.
Embodiment 3
A kind of preparation method of BN enhancings carbon fiber modifying melamine resin material proposed by the present invention, including with
Lower step：
S1,7 carbon fibers, 2.2 polyvinyl alcohol, 4 parts of boron chlorides, 4 parts of HMDSs are put into by weight
Ultrasonically treated 28min is carried out in one reaction vessel and obtains material A, ultrasonically treated frequency is 36KHz, and ultrasonically treated power is
1420W, takes out drying, dry temperature is 68 DEG C, is then placed in the second reaction vessel, the second reaction vessel is filled by material A
After full nitrogen, the second reaction vessel and its contents temperature are raised to 730 DEG C by 6 DEG C/min programming rate, and insulation 2.5h is obtained
Strengthen carbon fiber to BN；Wherein, carbon fiber is the polyacrylonitrile-based carbon fibre that modulus of elasticity is 230GPa；
S2,1.4 parts of silane coupler KH-791,0.3 part of microcrystalline wax, 0.2 part of butyl stearate are added by weight
Stirred in 14 parts of BN enhancing carbon fibers, add 47 parts of melamine resins, 22 parts of organic siliconresins, 14 parts of poly- second
Alkene, is warming up to 142 DEG C, stirs, and adds 2.4 parts of dioctyl phthalates, 1.2 parts of epoxidized soybean oils, 8 parts of micas
Powder, 3.5 parts of talcum powder, 2.4 parts of zinc oxide, mixed material is obtained after stirring；Mixed material is moved into double screw extruder,
BN enhancing carbon fiber modifying melamine resin materials, the extrusion zone temperature point of double screw extruder are obtained after melting extrusion
It is not：145 DEG C, 156 DEG C, 166 DEG C, 176 DEG C, 181 DEG C, head temperature is 200 DEG C, and double screw extruder rotating speed is 290r/
min。
Embodiment 4
A kind of preparation method of BN enhancings carbon fiber modifying melamine resin material proposed by the present invention, including with
Lower step：
S1,6 carbon fibers, 2.4 polyvinyl alcohol, 5 parts of boron chlorides, 5 parts of HMDSs are put into by weight
Ultrasonically treated 26min is carried out in one reaction vessel and obtains material A, ultrasonically treated frequency is 37KHz, and ultrasonically treated power is
1380W, takes out drying, dry temperature is 72 DEG C, is then placed in the second reaction vessel, the second reaction vessel is filled by material A
After full nitrogen, the second reaction vessel and its contents temperature are raised to 740 DEG C by 5.5 DEG C/min programming rate, 2.2h is incubated
Obtain BN enhancing carbon fibers；Wherein, carbon fiber is the polyacrylonitrile-based carbon fibre that modulus of elasticity is 250GPa；
S2,1.3 parts of silane coupler KH-791,0.4 part of microcrystalline wax, 0.15 part of butyl stearate are added by weight
Is stirred in 15 parts of BN enhancing carbon fibers, add 46 parts of melamine resins, 23 parts of organic siliconresins, 13.5 parts gather
Ethene, is warming up to 143 DEG C, stirs, and adds 2.3 parts of dioctyl phthalates, 1.3 parts of epoxidized soybean oils, 7 parts of micas
Powder, 4 parts of talcum powder, 2.2 parts of zinc oxide, mixed material is obtained after stirring；Mixed material is moved into double screw extruder, melted
Melt and BN enhancing carbon fiber modifying melamine resin materials are obtained after extrusion, the extrusion zone temperature difference of double screw extruder
For：146 DEG C, 154 DEG C, 168 DEG C, 175 DEG C, 182 DEG C, head temperature is 196 DEG C, and double screw extruder rotating speed is 300r/min.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (6)
1. a kind of BN strengthens the preparation method of carbon fiber modifying melamine resin material, it is characterised in that including following
Step：
S1,5-8 carbon fibers, 2-2.5 polyvinyl alcohol, 3-6 parts of boron chlorides, 3-6 parts of HMDSs are put by weight
Enter to carry out ultrasonically treated 25-30min in the first reaction vessel and obtain material A, ultrasonically treated frequency is at 35-38KHz, ultrasound
The power of reason is 1300-1500W, material A is taken out into drying, dry temperature is 65-75 DEG C, is then placed in the second reaction appearance
Device, the second reaction vessel is full of after nitrogen, and the second reaction vessel and its content temperature are raised by 5-7 DEG C/min programming rate
Degree is to 720-750 DEG C, and insulation 2-3h obtains BN enhancing carbon fibers；
S2, by weight by KH-791,0.2-0.5 parts of microcrystalline waxes of 1.2-1.5 parts of silane couplers, 0.1-0.3 parts of stearic acid
Butyl ester, which adds 13-16 part BN, to be strengthened and is stirred in carbon fibers, add 45-48 parts of melamine resins, 21-24 parts have
Machine silicones, 13-15 part polyethylene, are warming up to 140-145 DEG C, stir, and add 2.2-2.5 parts of phthalic acids two pungent
Ester, 1.1-1.4 part epoxidized soybean oil, 6-9 parts of mica powders, 3-5 parts of talcum powder, 2-2.5 parts of zinc oxide, are mixed after stirring
Compound material；Mixed material is moved to BN enhancing carbon fiber modifying melamino-formaldehydes are obtained after double screw extruder, melting extrusion
Resin material, the extrusion zone temperature of double screw extruder is respectively：144-147℃、153-158℃、165-170℃、174-177
DEG C, 180-183 DEG C, head temperature be 192-202 DEG C, double screw extruder rotating speed be 280-310r/min.
2. BN strengthens the preparation method of carbon fiber modifying melamine resin material, its feature according to claim 1
It is, in S1, carbon fiber is the polyacrylonitrile-based carbon fibre that modulus of elasticity is 230-250GPa.
3. BN according to claim 1 or claim 2 strengthens the preparation method of carbon fiber modifying melamine resin material, it is special
Levy and be, in S1, by weight by 6-7 carbon fibers, 2.2-2.4 polyvinyl alcohol, 4-5 parts of boron chlorides, the 4-5 parts of silicon of hexamethyl two
Azane, which is put into the first reaction vessel, to carry out ultrasonically treated 26-28min and obtains material A, and ultrasonically treated frequency is 36-37KHz,
Ultrasonically treated power is 1380-1420W, material A is taken out into drying, dry temperature is 68-72 DEG C, is then placed in second anti-
Container is answered, the second reaction vessel is full of after nitrogen, the second reaction vessel is raised and its interior by 5.5-6 DEG C/min programming rate
Tolerant temperature is to 730-740 DEG C, and insulation 2.2-2.5h obtains BN enhancing carbon fibers.
4. BN according to claim 1 or claim 2 strengthens the preparation method of carbon fiber modifying melamine resin material, it is special
Levy and be, in S1, boron chloride, the weight ratio of HMDS are 1:1.
5. BN according to claim 1 or claim 2 strengthens the preparation method of carbon fiber modifying melamine resin material, it is special
Levy and be, in S2, melamine resin, organic siliconresin, polyethylene, the weight ratio of BN enhancing carbon fibers are 46-47：
22-23：13.5-14：14-15.
6. BN according to claim 1 or claim 2 strengthens the preparation method of carbon fiber modifying melamine resin material, it is special
Levy and be, in S2, by weight by KH-791,0.3-0.4 parts of microcrystalline waxes of 1.3-1.4 parts of silane couplers, 0.15-0.2 parts
Butyl stearate is added to stir in 14-15 parts of BN enhancing carbon fibers, adds 46-47 parts of melamine resins, 22-
23 parts of organic siliconresins, 13.5-14 parts of polyethylene, are warming up to 142-143 DEG C, stir, and add 2.3-2.4 parts of adjacent benzene two
Formic acid dioctyl ester, 1.2-1.3 part epoxidized soybean oil, 7-8 parts of mica powders, 3.5-4 parts of talcum powder, 2.2-2.4 parts of zinc oxide, stirring
Mixed material is obtained after uniform；Mixed material is moved to BN enhancing carbon fiber modifyings are obtained after double screw extruder, melting extrusion
Melamine resin material, the extrusion zone temperature of double screw extruder is respectively：145-146℃、154-156℃、166-
168 DEG C, 175-176 DEG C, 181-182 DEG C, head temperature is 196-200 DEG C, and double screw extruder rotating speed is 290-300r/min.
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| CN110372992A (en) * | 2019-07-23 | 2019-10-25 | 安徽升隆电气有限公司 | A kind of detector for fire alarm system potent flameproof case material and preparation method thereof |
| CN114907790B (en) * | 2022-06-01 | 2023-11-03 | 上海库曜新材料有限公司 | Boron nitride doped heat conduction enhanced curing agent and application thereof |
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| CN102418090A (en) * | 2011-11-07 | 2012-04-18 | 深圳市欣天科技有限公司 | Method for surface metallization of resin-based composite material compressed by mold |
| CN104231605A (en) * | 2014-09-25 | 2014-12-24 | 丹阳丹金航空材料科技有限公司 | Rare earth modified carbon fiber reinforced composite material and preparation method thereof |
| CN104532551A (en) * | 2014-12-12 | 2015-04-22 | 哈尔滨工业大学 | Method for in-situ preparing silicon-boron-carbon-nitrogen ceramic coating on surface of carbon fiber |
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2015
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102418090A (en) * | 2011-11-07 | 2012-04-18 | 深圳市欣天科技有限公司 | Method for surface metallization of resin-based composite material compressed by mold |
| CN104231605A (en) * | 2014-09-25 | 2014-12-24 | 丹阳丹金航空材料科技有限公司 | Rare earth modified carbon fiber reinforced composite material and preparation method thereof |
| CN104532551A (en) * | 2014-12-12 | 2015-04-22 | 哈尔滨工业大学 | Method for in-situ preparing silicon-boron-carbon-nitrogen ceramic coating on surface of carbon fiber |
Non-Patent Citations (1)
| Title |
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| Carbon Fiber Reinforced Melamine-Formaldehyde;B. VOIGT et al.;《POLYMER COMPOSITES》;20030630;第24卷(第3期);全文 * |
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