CN104629255A - Preparation method of BN enhanced carbon fiber modified melamine formaldehyde resin material - Google Patents
Preparation method of BN enhanced carbon fiber modified melamine formaldehyde resin material Download PDFInfo
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- CN104629255A CN104629255A CN201510030260.8A CN201510030260A CN104629255A CN 104629255 A CN104629255 A CN 104629255A CN 201510030260 A CN201510030260 A CN 201510030260A CN 104629255 A CN104629255 A CN 104629255A
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Abstract
The invention discloses a preparation method of a BN enhanced carbon fiber modified melamine formaldehyde resin material. The preparation method comprises the following steps: putting carbon fibers, polyvinyl alcohol, boron trichloride and hexamethyldisilazane into a first reaction container for ultrasonic treatment to obtain a material A, drying the material A and then putting the material A into a second reaction container, fully filling the second reaction container with nitrogen, and then gradually heating and preserving heat to obtain BN enhanced carbon fibers; next, adding a silane coupling agent KH-791, microcrystalline wax and butyl stearate to the BN enhanced carbon fibers, stirring and then adding a melamine formaldehyde resin, an organic silicon resin and polyethylene, heating and further stirring, and finally adding dioctyl phthalate, epoxidized soybean oil, mica powder, talcum powder and zinc oxide, and stirring to obtain a mixture; shifting the mixture to a twin-screw extruder for melt extrusion, thereby obtaining the BN enhanced carbon fiber modified melamine formaldehyde resin material.
Description
Technical field
The present invention relates to terpolycyantoamino-formaldehyde resin field of material technology, particularly relate to a kind of preparation method of BN enhanced carbon fiber modified melamine-formaldehyde resin material.
Background technology
Terpolycyantoamino-formaldehyde resin is the thermosetting resin of a kind of excellent performance obtained by trimeric cyanamide and formaldehyde reaction, there is excellent stability, thermotolerance, electrical insulating property, self-extinguishing, arc resistance and good mechanical property, often be applied to cable processing industry, but, while having good material chemical property, its toughness, intensity are poor, can not meet the requirement to raw material high tenacity, high strength in cable processing industry.
Summary of the invention
Based on the technical problem that background technology exists, the present invention proposes a kind of preparation method of BN enhanced carbon fiber modified melamine-formaldehyde resin material, obtained terpolycyantoamino-formaldehyde resin toughness of material is good, intensity is high, can meet the demand of cable processing industry to raw material high tenacity, high strength.
The preparation method of a kind of BN enhanced carbon fiber modified melamine-formaldehyde resin material that the present invention proposes, comprises the following steps:
S1, by weight by 5-8 carbon fiber, 2-2.5 polyvinyl alcohol, 3-6 part boron trichloride, 3-6 part hexamethyldisilazane is put into the first reaction vessel and is carried out supersound process 25-30min and obtain material A, the frequency of supersound process is 35-38KHz, the power of supersound process is 1300-1500W, material A is taken out dry, dry temperature is 65-75 DEG C, then the second reaction vessel is put into, after second reaction vessel is full of nitrogen, the second reaction vessel and contents temperature thereof is raised to 720-750 DEG C by the heat-up rate of 5-7 DEG C/min, insulation 2-3h obtains BN enhanced carbon fiber,
S2,1.2-1.5 part silane coupling agent KH-791,0.2-0.5 part microcrystalline wax, 0.1-0.3 part butyl stearate are added in 13-16 part BN enhanced carbon fiber stir by weight, add 45-48 part terpolycyantoamino-formaldehyde resin, 21-24 part silicone resin, 13-15 part polyethylene again, be warming up to 140-145 DEG C, stir, add 2.2-2.5 part dioctyl phthalate (DOP), 1.1-1.4 part epoxy soybean oil, 6-9 part mica powder, 3-5 part talcum powder, 2-2.5 part zinc oxide again, after stirring, obtain mixture; Mixture is moved to twin screw extruder, BN enhanced carbon fiber modified melamine-formaldehyde resin material is obtained after melt extruding, district's temperature of extruding of twin screw extruder is respectively: 144-147 DEG C, 153-158 DEG C, 165-170 DEG C, 174-177 DEG C, 180-183 DEG C, head temperature is 192-202 DEG C, and twin screw extruder rotating speed is 280-310r/min.
Preferably, in S1, the PAN-based carbon fiber of carbon fiber to be Young's modulus be 230-250GPa.
Preferably, in S1, by weight by 6-7 carbon fiber, 2.2-2.4 polyvinyl alcohol, 4-5 part boron trichloride, 4-5 part hexamethyldisilazane is put into the first reaction vessel and is carried out supersound process 26-28min and obtain material A, the frequency of supersound process is 36-37KHz, the power of supersound process is 1380-1420W, material A is taken out dry, dry temperature is 68-72 DEG C, then the second reaction vessel is put into, after second reaction vessel is full of nitrogen, the second reaction vessel and contents temperature thereof is raised to 730-740 DEG C by the heat-up rate of 5.5-6 DEG C/min, insulation 2.2-2.5h obtains BN enhanced carbon fiber.
Preferably, in S1, the weight ratio of boron trichloride, hexamethyldisilazane is 1:1.
Preferably, in S2, the weight ratio of terpolycyantoamino-formaldehyde resin, silicone resin, polyethylene, BN enhanced carbon fiber is 46-47:22-23:13.5-14:14-15.
Preferably, in S2, by weight 1.3-1.4 part silane coupling agent KH-791,0.3-0.4 part microcrystalline wax, 0.15-0.2 part butyl stearate are added in 14-15 part BN enhanced carbon fiber and stir, add 46-47 part terpolycyantoamino-formaldehyde resin, 22-23 part silicone resin, 13.5-14 part polyethylene again, be warming up to 142-143 DEG C, stir, add 2.3-2.4 part dioctyl phthalate (DOP), 1.2-1.3 part epoxy soybean oil, 7-8 part mica powder, 3.5-4 part talcum powder, 2.2-2.4 part zinc oxide again, after stirring, obtain mixture; Mixture is moved to twin screw extruder, BN enhanced carbon fiber modified melamine-formaldehyde resin material is obtained after melt extruding, district's temperature of extruding of twin screw extruder is respectively: 145-146 DEG C, 154-156 DEG C, 166-168 DEG C, 175-176 DEG C, 181-182 DEG C, head temperature is 196-200 DEG C, and twin screw extruder rotating speed is 290-300r/min.
The present invention introduces silicone resin, polyethylene, BN enhanced carbon fiber modified melamine-formaldehyde resin, substantially increase toughness of the present invention, intensity and lear energy, wherein BN enhanced carbon fiber is that carbon fiber is through B, N enhancing obtains, carbon fiber strength is high, corrosion-resistant, modulus is high and to have stretching resistance strong, the features such as excellent in mechanical performance, but it is easily oxidized and have certain electroconductibility, in preparation process, boron trichloride, hexamethyldisilazane is attached to carbon fiber surface securely through supersound process under the effect of polyvinyl alcohol, BN coating is generated again by the pyroprocessing reaction under nitrogen protection, thus the BN coating with fabulous insulativity has been obtained at carbon fiber surface, and BN coating can with fabulous compatible of carbon fiber, substantially increase again the oxidation-resistance of carbon fiber, thus substantially increase toughness of the present invention, shock resistance, tear-resistant wear resisting property, the Plasticising system that dioctyl phthalate (DOP), butyl stearate, epoxy soybean oil are formed, improve plasticizing efficiency of the present invention, the present invention is made to have excellent heat-resisting, oil resistant, anti-swelling and resistance to migration energy, enhance toughness of the present invention, intensity and plasticity-, wherein butyl stearate can also coordinate as lubricant and releasing agent with microcrystalline wax, makes the present invention more be easy to processing, mica powder, talcum powder, zinc oxide, as the interpolation of reinforcing filler, substantially increase intensity of the present invention, wear resistant and impact resistant performance and electrical insulating property, and the interpolation of silane coupling agent KH-791, can be coated on the packing strengthening agent of BN enhanced carbon fiber and above-mentioned interpolation, make it be evenly distributed in the present invention, substantially increase intensity of the present invention, toughness and lear energy, meanwhile, plasticity-of the present invention is also enhanced.
Embodiment
Below, by specific embodiment, technical scheme of the present invention is described in detail.
Embodiment 1
The preparation method of a kind of BN enhanced carbon fiber modified melamine-formaldehyde resin material that the present invention proposes, comprises the following steps:
S1,8 carbon fibers, 2 polyvinyl alcohol, 3 parts of boron trichlorides, 3 parts of hexamethyldisilazanes are put into the first reaction vessel by weight and carry out supersound process 30min and obtain material A, the frequency of supersound process is 35KHz, the power of supersound process is 1500W, material A is taken out dry, dry temperature is 65 DEG C, then the second reaction vessel is put into, after second reaction vessel is full of nitrogen, raise the second reaction vessel and contents temperature to 720 DEG C thereof by the heat-up rate of 7 DEG C/min, insulation 3h obtains BN enhanced carbon fiber; Wherein, the PAN-based carbon fiber of carbon fiber to be Young's modulus be 230GPa;
S2,1.5 parts of silane coupling agent KH-791,0.2 part of microcrystalline wax, 0.3 part of butyl stearate are added in 13 parts of BN enhanced carbon fiber stir by weight, add 48 parts of terpolycyantoamino-formaldehyde resins, 21 parts of silicone resins, 15 parts of polyethylene again, be warming up to 140 DEG C, stir, add 2.5 parts of dioctyl phthalate (DOP)s, 1.1 parts of epoxy soybean oils, 9 parts of mica powders, 3 parts of talcum powder, 2.5 parts of zinc oxide again, after stirring, obtain mixture; Mixture is moved to twin screw extruder, BN enhanced carbon fiber modified melamine-formaldehyde resin material is obtained after melt extruding, district's temperature of extruding of twin screw extruder is respectively: 144 DEG C, 158 DEG C, 165 DEG C, 177 DEG C, 180 DEG C, head temperature is 202 DEG C, and twin screw extruder rotating speed is 280r/min.
Embodiment 2
The preparation method of a kind of BN enhanced carbon fiber modified melamine-formaldehyde resin material that the present invention proposes, comprises the following steps:
S1,5 carbon fibers, 2.5 polyvinyl alcohol, 6 parts of boron trichlorides, 6 parts of hexamethyldisilazanes are put into the first reaction vessel by weight and carry out supersound process 25min and obtain material A, the frequency of supersound process is 38KHz, the power of supersound process is 1300W, material A is taken out dry, dry temperature is 75 DEG C, then the second reaction vessel is put into, after second reaction vessel is full of nitrogen, raise the second reaction vessel and contents temperature to 750 DEG C thereof by the heat-up rate of 5 DEG C/min, insulation 2h obtains BN enhanced carbon fiber; Wherein, the PAN-based carbon fiber of carbon fiber to be Young's modulus be 250GPa;
S2,1.2 parts of silane coupling agent KH-791,0.5 part of microcrystalline wax, 0.1 part of butyl stearate are added in 16 parts of BN enhanced carbon fiber stir by weight, add 45 parts of terpolycyantoamino-formaldehyde resins, 24 parts of silicone resins, 13 parts of polyethylene again, be warming up to 145 DEG C, stir, add 2.2 parts of dioctyl phthalate (DOP)s, 1.4 parts of epoxy soybean oils, 6 parts of mica powders, 5 parts of talcum powder, 2 parts of zinc oxide again, after stirring, obtain mixture; Mixture is moved to twin screw extruder, BN enhanced carbon fiber modified melamine-formaldehyde resin material is obtained after melt extruding, district's temperature of extruding of twin screw extruder is respectively: 147 DEG C, 153 DEG C, 170 DEG C, 174 DEG C, 183 DEG C, head temperature is 192 DEG C, and twin screw extruder rotating speed is 310r/min.
Embodiment 3
The preparation method of a kind of BN enhanced carbon fiber modified melamine-formaldehyde resin material that the present invention proposes, comprises the following steps:
S1,7 carbon fibers, 2.2 polyvinyl alcohol, 4 parts of boron trichlorides, 4 parts of hexamethyldisilazanes are put into the first reaction vessel by weight and carry out supersound process 28min and obtain material A, the frequency of supersound process is 36KHz, the power of supersound process is 1420W, material A is taken out dry, dry temperature is 68 DEG C, then the second reaction vessel is put into, after second reaction vessel is full of nitrogen, raise the second reaction vessel and contents temperature to 730 DEG C thereof by the heat-up rate of 6 DEG C/min, insulation 2.5h obtains BN enhanced carbon fiber; Wherein, the PAN-based carbon fiber of carbon fiber to be Young's modulus be 230GPa;
S2,1.4 parts of silane coupling agent KH-791,0.3 part of microcrystalline wax, 0.2 part of butyl stearate are added in 14 parts of BN enhanced carbon fiber stir by weight, add 47 parts of terpolycyantoamino-formaldehyde resins, 22 parts of silicone resins, 14 parts of polyethylene again, be warming up to 142 DEG C, stir, add 2.4 parts of dioctyl phthalate (DOP)s, 1.2 parts of epoxy soybean oils, 8 parts of mica powders, 3.5 parts of talcum powder, 2.4 parts of zinc oxide again, after stirring, obtain mixture; Mixture is moved to twin screw extruder, BN enhanced carbon fiber modified melamine-formaldehyde resin material is obtained after melt extruding, district's temperature of extruding of twin screw extruder is respectively: 145 DEG C, 156 DEG C, 166 DEG C, 176 DEG C, 181 DEG C, head temperature is 200 DEG C, and twin screw extruder rotating speed is 290r/min.
Embodiment 4
The preparation method of a kind of BN enhanced carbon fiber modified melamine-formaldehyde resin material that the present invention proposes, comprises the following steps:
S1,6 carbon fibers, 2.4 polyvinyl alcohol, 5 parts of boron trichlorides, 5 parts of hexamethyldisilazanes are put into the first reaction vessel by weight and carry out supersound process 26min and obtain material A, the frequency of supersound process is 37KHz, the power of supersound process is 1380W, material A is taken out dry, dry temperature is 72 DEG C, then the second reaction vessel is put into, after second reaction vessel is full of nitrogen, raise the second reaction vessel and contents temperature to 740 DEG C thereof by the heat-up rate of 5.5 DEG C/min, insulation 2.2h obtains BN enhanced carbon fiber; Wherein, the PAN-based carbon fiber of carbon fiber to be Young's modulus be 250GPa;
S2,1.3 parts of silane coupling agent KH-791,0.4 part of microcrystalline wax, 0.15 part of butyl stearate are added in 15 parts of BN enhanced carbon fiber stir by weight, add 46 parts of terpolycyantoamino-formaldehyde resins, 23 parts of silicone resins, 13.5 parts of polyethylene again, be warming up to 143 DEG C, stir, add 2.3 parts of dioctyl phthalate (DOP)s, 1.3 parts of epoxy soybean oils, 7 parts of mica powders, 4 parts of talcum powder, 2.2 parts of zinc oxide again, after stirring, obtain mixture; Mixture is moved to twin screw extruder, BN enhanced carbon fiber modified melamine-formaldehyde resin material is obtained after melt extruding, district's temperature of extruding of twin screw extruder is respectively: 146 DEG C, 154 DEG C, 168 DEG C, 175 DEG C, 182 DEG C, head temperature is 196 DEG C, and twin screw extruder rotating speed is 300r/min.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (6)
1. a preparation method for BN enhanced carbon fiber modified melamine-formaldehyde resin material, is characterized in that, comprise the following steps:
S1, by weight by 5-8 carbon fiber, 2-2.5 polyvinyl alcohol, 3-6 part boron trichloride, 3-6 part hexamethyldisilazane is put into the first reaction vessel and is carried out supersound process 25-30min and obtain material A, the frequency of supersound process is 35-38KHz, the power of supersound process is 1300-1500W, material A is taken out dry, dry temperature is 65-75 DEG C, then the second reaction vessel is put into, after second reaction vessel is full of nitrogen, the second reaction vessel and contents temperature thereof is raised to 720-750 DEG C by the heat-up rate of 5-7 DEG C/min, insulation 2-3h obtains BN enhanced carbon fiber,
S2,1.2-1.5 part silane coupling agent KH-791,0.2-0.5 part microcrystalline wax, 0.1-0.3 part butyl stearate are added in 13-16 part BN enhanced carbon fiber stir by weight, add 45-48 part terpolycyantoamino-formaldehyde resin, 21-24 part silicone resin, 13-15 part polyethylene again, be warming up to 140-145 DEG C, stir, add 2.2-2.5 part dioctyl phthalate (DOP), 1.1-1.4 part epoxy soybean oil, 6-9 part mica powder, 3-5 part talcum powder, 2-2.5 part zinc oxide again, after stirring, obtain mixture; Mixture is moved to twin screw extruder, BN enhanced carbon fiber modified melamine-formaldehyde resin material is obtained after melt extruding, district's temperature of extruding of twin screw extruder is respectively: 144-147 DEG C, 153-158 DEG C, 165-170 DEG C, 174-177 DEG C, 180-183 DEG C, head temperature is 192-202 DEG C, and twin screw extruder rotating speed is 280-310r/min.
2. the preparation method of BN enhanced carbon fiber modified melamine-formaldehyde resin material according to claim 1, is characterized in that, in S1, and the PAN-based carbon fiber of carbon fiber to be Young's modulus be 230-250GPa.
3. the preparation method of BN enhanced carbon fiber modified melamine-formaldehyde resin material according to claim 1 or 2, it is characterized in that, in S1, by weight by 6-7 carbon fiber, 2.2-2.4 polyvinyl alcohol, 4-5 part boron trichloride, 4-5 part hexamethyldisilazane is put into the first reaction vessel and is carried out supersound process 26-28min and obtain material A, the frequency of supersound process is 36-37KHz, the power of supersound process is 1380-1420W, material A is taken out dry, dry temperature is 68-72 DEG C, then the second reaction vessel is put into, after second reaction vessel is full of nitrogen, the second reaction vessel and contents temperature thereof is raised to 730-740 DEG C by the heat-up rate of 5.5-6 DEG C/min, insulation 2.2-2.5h obtains BN enhanced carbon fiber.
4. the preparation method of BN enhanced carbon fiber modified melamine-formaldehyde resin material according to any one of claim 1-3, it is characterized in that, in S1, the weight ratio of boron trichloride, hexamethyldisilazane is 1:1.
5. the preparation method of BN enhanced carbon fiber modified melamine-formaldehyde resin material according to any one of claim 1-4, it is characterized in that, in S2, the weight ratio of terpolycyantoamino-formaldehyde resin, silicone resin, polyethylene, BN enhanced carbon fiber is 46-47:22-23:13.5-14:14-15.
6. the preparation method of BN enhanced carbon fiber modified melamine-formaldehyde resin material according to any one of claim 1-5, it is characterized in that, in S2, by weight by 1.3-1.4 part silane coupling agent KH-791, 0.3-0.4 part microcrystalline wax, 0.15-0.2 part butyl stearate adds in 14-15 part BN enhanced carbon fiber and stirs, add 46-47 part terpolycyantoamino-formaldehyde resin again, 22-23 part silicone resin, 13.5-14 part polyethylene, be warming up to 142-143 DEG C, stir, add 2.3-2.4 part dioctyl phthalate (DOP) again, 1.2-1.3 part epoxy soybean oil, 7-8 part mica powder, 3.5-4 part talcum powder, 2.2-2.4 part zinc oxide, mixture is obtained after stirring, mixture is moved to twin screw extruder, BN enhanced carbon fiber modified melamine-formaldehyde resin material is obtained after melt extruding, district's temperature of extruding of twin screw extruder is respectively: 145-146 DEG C, 154-156 DEG C, 166-168 DEG C, 175-176 DEG C, 181-182 DEG C, head temperature is 196-200 DEG C, and twin screw extruder rotating speed is 290-300r/min.
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Cited By (2)
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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 |
| CN114907790A (en) * | 2022-06-01 | 2022-08-16 | 上海库曜新材料有限公司 | Boron nitride-doped heat-conducting enhanced curing agent and application thereof |
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