CN109608865A - A kind of thermally conductive foam with heat-conductive characteristic - Google Patents
A kind of thermally conductive foam with heat-conductive characteristic Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/06—Polyethene
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Abstract
The invention discloses a kind of thermally conductive foam with heat-conductive characteristic, by include following parts by weight raw material mixing after be prepared through oscillation, foaming, drying: 30-50 parts of polyurethane, 20-30 parts of polyethylene, 4-6 parts of dispersing agent, 2-3 parts of fire retardant, 1-3 parts of antiaging agent, 15-20 parts of modified carbon fiber, 2-4 parts of foaming agent, 3-5 parts of plasticizer, 5-7 parts of curing agent, 1-2 parts of surfactant.Thermally conductive foam prepared by the present invention, under the synergistic effect of each component, foam has excellent tensile property, heat resistance, the stability of anti-flammability and structure, and frothing percentage height, thermal coefficient are high inside foam, it is at low cost simultaneously, it is readily produced, is with a wide range of applications.
Description
Technical field
The invention belongs to thermally conductive foam technical fields, and in particular to a kind of thermally conductive foam with heat-conductive characteristic.
Background technique
Heat transfer be in medium without macroscopic motion when phenomenon of Heat, can occur in solid, liquids and gases,
But for stringent, it is only only pure heat transfer in solids, and fluid is even at stationary state, wherein also due to temperature
It spends density contrast caused by gradient and generates free convection, therefore, thermal convection occurs simultaneously with heat transfer in a fluid.In electronics
In industrial circle, heat transfer is always an important process in electronics industry, and the operating temperature of component is often reliability
Important evidence.The especially assembling of microelectronics increasingly densification, working environment is sharply to high temperature direction change.According to aobvious
Show, electronic component temperature is every to increase 2 DEG C, and reliability decrease 10%, service life at 50 DEG C only has 1/6 at 25 DEG C, thermal conductivity
Can improve usually along with the optimization of heat dissipation performance, therefore, Heat-conductive gap interface material more and more attention has been paid to.
Foam is a kind of quality material with buffering, damping, sound-absorbing, obdurability and other effects, existing rubber, polyurethane,
The antistatic foams such as polyethylene, polyethers, conducting foam.Although having had already appeared several foams with heat-conduction effect at present
Material, but its inner cell is uneven, frothing percentage is low, thermal coefficient is low, has big control difficulty, high production cost, molding difficult
The disadvantages of.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of thermally conductive foam with heat-conductive characteristic is provided.
The present invention is achieved by the following technical solutions:
A kind of thermally conductive foam with heat-conductive characteristic, by weight component are as follows: 30-50 parts of polyurethane, polyethylene 20-30
Part, 4-6 parts of dispersing agent, 2-3 parts of fire retardant, 1-3 parts of antiaging agent, 15-20 parts of modified carbon fiber, 2-4 parts of foaming agent, plasticizer
3-5 parts, 5-7 parts of curing agent, 1-2 parts of surfactant.
Preferably, a kind of thermally conductive foam with heat-conductive characteristic, wherein the dispersing agent is fatty acid, aliphatic
One or both of amides, esters, the fire retardant are magnalium flame retardant, in nitrogenated flame retardant, organic silicon fibre retardant
One or two, the antiaging agent be 2-mercaptobenzimidazole or 2,2,4- trimethyl -1,2- dihyaroquinoline condensates,
The foaming agent is one or both of normal butane, pentane, n-hexane, and the plasticizer is that citric acid ester type or epoxy are big
Soya-bean oil, the curing agent are formic acid or acetic acid, and the surfactant is neopelex or lauryl sodium sulfate.
Preferably, a kind of thermally conductive foam with heat-conductive characteristic, wherein modified carbon fiber the preparation method is as follows:
1) it adds chitosan into glacial acetic acid/aqueous solution, is heated to 45-55 DEG C, stirring is completely dissolved to form shell to chitosan
Then ammonium persulfate is added in glycan solution, sodium hydroxide solution and vinyl pyrrolidone, heating is added after keeping the temperature 10-15min
To 65-70 DEG C, isothermal reaction 2-3h, modification of chitosan solution is made
2) will formalin and chloroformic solution mix after be added in container, adding triethylamine and adjusting pH is 9-10, then plus
Enter diethylenetriamine, 1-2h is reacted at 5-10 DEG C, then adds parahydroxyben-zaldehyde, is warming up to 80-90 DEG C, the reaction was continued
1-2h, to after reaction, be cooled to room temperature, benzoxazine is made in vacuum distillation removal solvent；
3) paraformaldehyde, sodium hydroxide solution are added in the there-necked flask for being equipped with blender and condensation reflux unit, are then risen
Temperature is cooled to 50-55 DEG C after paraformaldehyde dissolution, adds Bisphenol F and toluene solution, add after mixing to 70-80 DEG C
Enter aniline, be warming up to 85-90 DEG C, flow back 4-5h, after product stratification, separates lower-layer resin solution and at 80-85 DEG C
20-25min is rotated, then then moves to and is heated to 70-80 DEG C in vacuum drying oven, Bisphenol F-aniline type benzo is made in dry 3-5h
Oxazines；
4) Bisphenol F-aniline type benzoxazine is added in n,N-Dimethylformamide solution, carbon fiber is added after stirring and dissolving
Dimension, the vibrating dispersion 40-60min under 500-800W ultrasonic wave form dispersion liquid, then add benzoxazine and modified shell is poly-
Sugar juice is warming up to 70-80 DEG C, isothermal reaction 20-23h after mixing evenly, is then dried in vacuo 8-10h at 70-75 DEG C and goes
It except solvent, then moves in Muffle furnace, is heated to 200-240 DEG C, solidify 1-2h, then squeezed through extruder, can be prepared by being modified
Carbon fiber.
Preferably, a kind of thermally conductive foam with heat-conductive characteristic, wherein modified carbon fiber preparation step 1) in, the shell
The mass volume ratio of glycan and glacial acetic acid/aqueous solution, sodium hydroxide solution, vinyl pyrrolidone solution is 1g:15-20ml:
4-6ml:5-7ml, glacial acetic acid content is 20-25% in the glacial acetic acid/aqueous solution, remaining is distilled water, and the sodium hydroxide is molten
The concentration of liquid be 3-5mol/L, the chitosan, ammonium persulfate mass ratio be 1:0.2-0.3.
Preferably, a kind of thermally conductive foam with heat-conductive characteristic, wherein modified carbon fiber preparation step 2) in, the first
Aldehyde, chloroform, diethylenetriamine and parahydroxyben-zaldehyde volume ratio be 25-30:20-25:3-5:4-7, the concentration of the formaldehyde
For 35-38%.
Preferably, a kind of thermally conductive foam with heat-conductive characteristic, wherein modified carbon fiber preparation step 3) in, it is described more
Polyformaldehyde, sodium hydroxide solution, toluene solution and aniline mass volume ratio be 1g:2-3ml:1-1.5ml:1.2-1.6ml, institute
The mass ratio for stating paraformaldehyde and Bisphenol F is 1:1.2-1.5, and the concentration of the sodium hydroxide solution is 5-8%.
Preferably, a kind of thermally conductive foam with heat-conductive characteristic, wherein modified carbon fiber preparation step 4) in, it is described double
Phenol F- aniline type benzoxazine, N,N-dimethylformamide solution, modification of chitosan solution mass volume ratio be 1g:8-
10ml:3-4ml, the Bisphenol F-aniline type benzoxazine, carbon fiber and benzoxazine mass ratio are 1:1-2:0.5-0.8,
The screw diameter of the extruder is 60-90mm, draw ratio 1:24-30, revolving speed 20-90r/min, head pressure 15-
25MPa。
Preferably, a kind of thermally conductive foam with heat-conductive characteristic, wherein the thermally conductive foam with heat-conductive characteristic
The preparation method is as follows: by polyurethane, polyethylene, dispersing agent, fire retardant, antiaging agent, modified carbon fiber, foaming agent, plasticising
In the case where power is 400-600W ultrasonic wave, vibrating dispersion 30-40min, formation are blended after agent, curing agent, surfactant mixing
Liquid, then by blended liquid in the foaming furnace that frequency is 2400-2600MHz, power is 2-5kW microwave foam 3-5min, then
1-2h is dried in 200-260 DEG C of baking oven, can be prepared by required foam.
The present invention has the advantage that thermally conductive foam prepared by the present invention compared with prior art, makees in the collaboration of each component
Under, foam has excellent tensile property, heat resistance, the stability of anti-flammability and structure, and frothing percentage inside foam
High, thermal coefficient height, at the same it is at low cost, it is readily produced.Modified carbon fiber in the thermally conductive foam is by Bisphenol F-aniline type benzene
And the compound that oxazines, carbon fiber and benzoxazine are formed under the adhesive effect of modification of chitosan solution, firstly, modified shell is poly-
Sugar is to be graft-polymerized under the action of vinyl pyrrolidone and initiator to chitosan, to improve the glutinous of chitosan
Conjunction property；Secondly, being introduced into Bisphenol F-aniline type benzoxazine and carbon fiber complex system using benzoxazine as interface modifier
In, under the adhesive effect of modification of chitosan, benzoxazine is adhered to Bisphenol F-aniline type benzoxazine and carbon fiber surface, can
To enhance interface cohesion of the Bisphenol F-between aniline type benzoxazine and carbon fiber, reduce interface resistance between the two, so that
That one-dimensional plane may be implemented is height-oriented by extruding for carbon fiber, so that modified carbon fiber takes with plane originally
In the case where on solid space have it is height-oriented so that modified carbon fiber have higher thermal conductivity.
Specific embodiment
Below with reference to specific implementation method, the present invention is described further.
Embodiment 1
A kind of thermally conductive foam with heat-conductive characteristic, by weight component are as follows: 30 parts of polyurethane, 20 parts of polyethylene, dispersion
4 parts of agent, 2 parts of fire retardant, 1 part of antiaging agent, 15 parts of modified carbon fiber, 2 parts of foaming agent, 3 parts of plasticizer, 5 parts of curing agent, surface
1 part of activating agent.
Preferably, wherein, the dispersing agent is one or both of fatty acid, aliphatic amide type, esters, institute
Stating fire retardant is one or both of magnalium flame retardant, nitrogenated flame retardant, organic silicon fibre retardant, and the antiaging agent is 2-
Mercaptobenzimidazole or 2,2,4- trimethyl -1,2- dihyaroquinoline condensates, the foaming agent are normal butane, pentane, just
One or both of hexane, the plasticizer be citric acid ester type or epoxidized soybean oil, the curing agent be formic acid or acetic acid,
The surfactant is neopelex or lauryl sodium sulfate.
Preferably, wherein, modified carbon fiber the preparation method is as follows:
1) it adds chitosan into glacial acetic acid/aqueous solution, is heated to 45 DEG C, stirring is completely dissolved to form chitosan to chitosan
Then ammonium persulfate is added in solution, sodium hydroxide solution and vinyl pyrrolidone is added after keeping the temperature 15min, is warming up to 65 DEG C,
Modification of chitosan solution is made in isothermal reaction 3h
2) it is added in container after mixing formalin and chloroformic solution, adding triethylamine and adjusting pH is 9, is then added two
Ethylene triamine reacts 2h at 5 DEG C, then adds parahydroxyben-zaldehyde, is warming up to 80 DEG C, the reaction was continued 2h, wait react knot
Shu Hou is cooled to room temperature, and benzoxazine is made in vacuum distillation removal solvent；
3) paraformaldehyde, sodium hydroxide solution are added in the there-necked flask for being equipped with blender and condensation reflux unit, are then risen
Temperature is cooled to 50 DEG C after paraformaldehyde dissolution, adds Bisphenol F and toluene solution, aniline is added after mixing to 70 DEG C,
85 DEG C are warming up to, flow back 5h, after product stratification, separates lower-layer resin solution and rotates 25min at 80 DEG C, then again
It moves in vacuum drying oven and is heated to 70 DEG C, Bisphenol F-aniline type benzoxazine is made in dry 5h；
4) Bisphenol F-aniline type benzoxazine is added in n,N-Dimethylformamide solution, carbon fiber is added after stirring and dissolving
Dimension, the vibrating dispersion 60min under 500W ultrasonic wave form dispersion liquid, then add benzoxazine and modification of chitosan solution,
It is warming up to 70 DEG C, isothermal reaction 23h after mixing evenly, is then dried in vacuo 10h at 70 DEG C and removes solvent, then move to Muffle furnace
In, 200 DEG C are heated to, solidifies 2h, is then squeezed through extruder, modified carbon fiber is made.
Preferably, wherein modified carbon fiber preparation step 1) in, the chitosan and glacial acetic acid/aqueous solution, hydroxide
Sodium solution, vinyl pyrrolidone solution mass volume ratio be 1g:15ml:4ml:5ml, ice in the glacial acetic acid/aqueous solution
Acetic acid content is 20%, remaining is distilled water, and the concentration of the sodium hydroxide solution is 3mol/L, the chitosan, ammonium persulfate
Mass ratio be 1:0.2.
Preferably, wherein modified carbon fiber preparation step 2) in, the formaldehyde, chloroform, diethylenetriamine and to hydroxyl
The volume ratio of benzaldehyde is 25:20:3:4, and the concentration of the formaldehyde is 35%.
Preferably, wherein modified carbon fiber preparation step 3) in, the paraformaldehyde, sodium hydroxide solution, toluene are molten
The mass volume ratio of liquid and aniline is 1g:2ml:1ml:1.2ml, and the mass ratio of the paraformaldehyde and Bisphenol F is 1:1.2, institute
The concentration for stating sodium hydroxide solution is 5%.
Preferably, wherein modified carbon fiber preparation step 4) in, the Bisphenol F-aniline type benzoxazine, N, N- diformazan
Base formamide solution, modification of chitosan solution mass volume ratio be 1g:8ml:3ml, the Bisphenol F-aniline type benzoxazine,
The mass ratio of carbon fiber and benzoxazine is 1:1:0.5, and the screw diameter of the extruder is 60mm, draw ratio 1:24, is turned
Speed is 20r/min, head pressure 15MPa.
Preferably, wherein, the thermally conductive foam with heat-conductive characteristic the preparation method is as follows: by polyurethane, poly-
After ethylene, dispersing agent, fire retardant, antiaging agent, modified carbon fiber, foaming agent, plasticizer, curing agent, surfactant mixing
The vibrating dispersion 40min in the case where power is 400W ultrasonic wave, forms blended liquid, is then 2400MHz, power in frequency by blended liquid
For microwave foaming 5min in the foaming furnace of 2kW, 2h then is dried in 200 DEG C of baking ovens, can be prepared by required foam.
Embodiment 2
A kind of thermally conductive foam with heat-conductive characteristic, by weight component are as follows: 40 parts of polyurethane, 25 parts of polyethylene, dispersion
5 parts of agent, 2.5 parts of fire retardant, 2 parts of antiaging agent, 17 parts of modified carbon fiber, 3 parts of foaming agent, 4 parts of plasticizer, 6 parts of curing agent, table
1.5 parts of face activating agent.
Preferably, wherein, the dispersing agent is one or both of fatty acid, aliphatic amide type, esters, institute
Stating fire retardant is one or both of magnalium flame retardant, nitrogenated flame retardant, organic silicon fibre retardant, and the antiaging agent is 2-
Mercaptobenzimidazole or 2,2,4- trimethyl -1,2- dihyaroquinoline condensates, the foaming agent are normal butane, pentane, just
One or both of hexane, the plasticizer be citric acid ester type or epoxidized soybean oil, the curing agent be formic acid or acetic acid,
The surfactant is neopelex or lauryl sodium sulfate.
Preferably, wherein, modified carbon fiber the preparation method is as follows:
1) it adds chitosan into glacial acetic acid/aqueous solution, is heated to 50 DEG C, stirring is completely dissolved to form chitosan to chitosan
Then ammonium persulfate is added in solution, sodium hydroxide solution and vinyl pyrrolidone is added after keeping the temperature 13min, is warming up to 68 DEG C,
Modification of chitosan solution is made in isothermal reaction 2.5h
2) it is added in container after mixing formalin and chloroformic solution, adding triethylamine and adjusting pH is 9.5, is then added
Diethylenetriamine reacts 1.5h at 7 DEG C, then adds parahydroxyben-zaldehyde, is warming up to 85 DEG C, the reaction was continued 1.5h, to
After reaction, it is cooled to room temperature, benzoxazine is made in vacuum distillation removal solvent；
3) paraformaldehyde, sodium hydroxide solution are added in the there-necked flask for being equipped with blender and condensation reflux unit, are then risen
Temperature is cooled to 53 DEG C after paraformaldehyde dissolution, adds Bisphenol F and toluene solution, aniline is added after mixing to 75 DEG C,
87 DEG C are warming up to, flow back 4.5h, after product stratification, separates lower-layer resin solution and rotates 23min at 82 DEG C, then
It then moves in vacuum drying oven and is heated to 75 DEG C, Bisphenol F-aniline type benzoxazine is made in dry 4h；
4) Bisphenol F-aniline type benzoxazine is added in n,N-Dimethylformamide solution, carbon fiber is added after stirring and dissolving
Dimension, the vibrating dispersion 500min under 700W ultrasonic wave form dispersion liquid, then add benzoxazine and modification of chitosan is molten
Liquid is warming up to 75 DEG C, isothermal reaction 21h after mixing evenly, is then dried in vacuo 9h at 72 DEG C and removes solvent, then moves to Muffle
In furnace, 230 DEG C are heated to, solidifies 1.5h, is then squeezed through extruder, modified carbon fiber is made.
Preferably, wherein modified carbon fiber preparation step 1) in, the chitosan and glacial acetic acid/aqueous solution, hydroxide
Sodium solution, vinyl pyrrolidone solution mass volume ratio be 1g:17ml:5ml:6ml, ice in the glacial acetic acid/aqueous solution
Acetic acid content is 23%, remaining is distilled water, and the concentration of the sodium hydroxide solution is 4mol/L, the chitosan, ammonium persulfate
Mass ratio be 1:0.25.
Preferably, wherein modified carbon fiber preparation step 2) in, the formaldehyde, chloroform, diethylenetriamine and to hydroxyl
The volume ratio of benzaldehyde is 27:23:4:5, and the concentration of the formaldehyde is 36%.
Preferably, wherein modified carbon fiber preparation step 3) in, the paraformaldehyde, sodium hydroxide solution, toluene are molten
The mass volume ratio of liquid and aniline is 1g:2.5ml:1.3ml:1.5ml, and the mass ratio of the paraformaldehyde and Bisphenol F is 1:
1.3, the concentration of the sodium hydroxide solution is 6%.
Preferably, wherein modified carbon fiber preparation step 4) in, the Bisphenol F-aniline type benzoxazine, N, N- diformazan
Base formamide solution, modification of chitosan solution mass volume ratio be 1g:9ml:3.5l, the Bisphenol F-aniline type benzo is disliked
The mass ratio of piperazine, carbon fiber and benzoxazine is 1:1.5:0.6, and the screw diameter of the extruder is 60mm, draw ratio 1:
30, revolving speed 50r/min, head pressure 20MPa.
Preferably, wherein, the thermally conductive foam with heat-conductive characteristic the preparation method is as follows: by polyurethane, poly-
After ethylene, dispersing agent, fire retardant, antiaging agent, modified carbon fiber, foaming agent, plasticizer, curing agent, surfactant mixing
The vibrating dispersion 35min in the case where power is 500W ultrasonic wave, forms blended liquid, is then 2500MHz, power in frequency by blended liquid
For microwave foaming 4min in the foaming furnace of 3kW, 1.52h then is dried in 240 DEG C of baking ovens, can be prepared by required foam.
Embodiment 3
A kind of thermally conductive foam with heat-conductive characteristic, by weight component are as follows: 50 parts of polyurethane, 30 parts of polyethylene, dispersion
6 parts of agent, 3 parts of fire retardant, 3 parts of antiaging agent, 20 parts of modified carbon fiber, 4 parts of foaming agent, 5 parts of plasticizer, 7 parts of curing agent, surface
2 parts of activating agent.
Preferably, wherein, the dispersing agent is one or both of fatty acid, aliphatic amide type, esters, institute
Stating fire retardant is one or both of magnalium flame retardant, nitrogenated flame retardant, organic silicon fibre retardant, and the antiaging agent is 2-
Mercaptobenzimidazole or 2,2,4- trimethyl -1,2- dihyaroquinoline condensates, the foaming agent are normal butane, pentane, just
One or both of hexane, the plasticizer be citric acid ester type or epoxidized soybean oil, the curing agent be formic acid or acetic acid,
The surfactant is neopelex or lauryl sodium sulfate.
Preferably, wherein, modified carbon fiber the preparation method is as follows:
1) it adds chitosan into glacial acetic acid/aqueous solution, is heated to 55 DEG C, stirring is completely dissolved to form chitosan to chitosan
Then ammonium persulfate is added in solution, sodium hydroxide solution and vinyl pyrrolidone is added after keeping the temperature 10min, is warming up to 70 DEG C,
Modification of chitosan solution is made in isothermal reaction 2h
2) it is added in container after mixing formalin and chloroformic solution, adding triethylamine and adjusting pH is 10, is then added
Diethylenetriamine reacts 1h at 10 DEG C, then adds parahydroxyben-zaldehyde, is warming up to 90 DEG C, the reaction was continued 1h, wait react
After, it is cooled to room temperature, benzoxazine is made in vacuum distillation removal solvent；
3) paraformaldehyde, sodium hydroxide solution are added in the there-necked flask for being equipped with blender and condensation reflux unit, are then risen
Temperature is cooled to 55 DEG C after paraformaldehyde dissolution, adds Bisphenol F and toluene solution, aniline is added after mixing to 80 DEG C,
90 DEG C are warming up to, flow back 4h, after product stratification, separates lower-layer resin solution and rotates 20min at 85 DEG C, then again
It moves in vacuum drying oven and is heated to 80 DEG C, Bisphenol F-aniline type benzoxazine is made in dry 3h；
4) Bisphenol F-aniline type benzoxazine is added in n,N-Dimethylformamide solution, carbon fiber is added after stirring and dissolving
Dimension, the vibrating dispersion 40min under 800W ultrasonic wave form dispersion liquid, then add benzoxazine and modification of chitosan solution,
It is warming up to 80 DEG C, isothermal reaction 20h after mixing evenly, is then dried in vacuo 8h at 75 DEG C and removes solvent, then move to Muffle furnace
In, 240 DEG C are heated to, solidifies 1 h, is then squeezed through extruder, modified carbon fiber is made.
Preferably, wherein modified carbon fiber preparation step 1) in, the chitosan and glacial acetic acid/aqueous solution, hydroxide
Sodium solution, vinyl pyrrolidone solution mass volume ratio be 1g:20ml:6ml:7ml, ice in the glacial acetic acid/aqueous solution
Acetic acid content is 25%, remaining is distilled water, and the concentration of the sodium hydroxide solution is 5mol/L, the chitosan, ammonium persulfate
Mass ratio be 1:0.3.
Preferably, wherein modified carbon fiber preparation step 2) in, the formaldehyde, chloroform, diethylenetriamine and to hydroxyl
The volume ratio of benzaldehyde is 30:25:5:7, and the concentration of the formaldehyde is 38%.
Preferably, wherein modified carbon fiber preparation step 3) in, the paraformaldehyde, sodium hydroxide solution, toluene are molten
The mass volume ratio of liquid and aniline is 1g:3ml:1.5ml:1.6ml, and the mass ratio of the paraformaldehyde and Bisphenol F is 1:1.5,
The concentration of the sodium hydroxide solution is 8%.
Preferably, wherein modified carbon fiber preparation step 4) in, the Bisphenol F-aniline type benzoxazine, N, N- diformazan
Base formamide solution, modification of chitosan solution mass volume ratio be 1g:10ml:4ml, the Bisphenol F-aniline type benzo is disliked
The mass ratio of piperazine, carbon fiber and benzoxazine is 1:2:0.8, and the screw diameter of the extruder is 90mm, draw ratio 1:30,
Revolving speed is 90r/min, head pressure 25MPa.
Preferably, wherein, the thermally conductive foam with heat-conductive characteristic the preparation method is as follows: by polyurethane, poly-
After ethylene, dispersing agent, fire retardant, antiaging agent, modified carbon fiber, foaming agent, plasticizer, curing agent, surfactant mixing
The vibrating dispersion 30min in the case where power is 600W ultrasonic wave, forms blended liquid, is then 2600MHz, power in frequency by blended liquid
For microwave foaming 3min in the foaming furnace of 5kW, 1h then is dried in 260 DEG C of baking ovens, can be prepared by required foam.
Comparative example 1: removal modified carbon fiber preparation step 1) in vinyl pyrrolidone, remaining is same as Example 1.
Comparative example 2: modified carbon fiber preparation step 2) in pH be adjusted to 8-9, remaining is same as Example 1.
Comparative example 3: removal modified carbon fiber preparation step 3) in paraformaldehyde dissolve cooling treatment, remaining and embodiment
1 is identical.
Comparative example 4: removal modified carbon fiber preparation step 4) in Muffle furnace calcining, remaining is same as Example 1.
Comparative example 5: removal modified carbon fiber preparation step 4) in extruder squeeze, remaining is same as Example 1.
Comparative example 6: common carbon fibers are selected to replace modified carbon fiber, remaining is same as Example 1.
Test example: testing embodiment 1-3 and comparative example the 1-6 thermally conductive foam provided, and control group is without containing changing
The common foam of property carbon fiber, test result are as shown in Table 1:
Table one
As can be seen from Table I, thermally conductive foam provided by the invention not only has good mechanical property, but also has excellent
Thermal conductivity.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
It transforms or replaces, should be covered by the scope of protection of the present invention without what creative work was expected.
Claims (8)
1. a kind of thermally conductive foam with heat-conductive characteristic, which is characterized in that component is as follows by weight: 30-50 parts of polyurethane,
20-30 parts of polyethylene, 4-6 parts of dispersing agent, 2-3 parts of fire retardant, 1-3 parts of antiaging agent, 15-20 parts of modified carbon fiber, foaming agent
2-4 parts, 3-5 parts of plasticizer, 5-7 parts of curing agent, 1-2 parts of surfactant.
2. a kind of thermally conductive foam with heat-conductive characteristic as described in claim 1, which is characterized in that the dispersing agent is rouge
One or both of fat acids, aliphatic amide type, esters, the fire retardant are magnalium flame retardant, nitrogenated flame retardant, have
One or both of machine silicon fire retardant, the antiaging agent are 2-mercaptobenzimidazole or 2,2,4- trimethyl -1,2- dihydros
Change quinoline condensate, the foaming agent is one or both of normal butane, pentane, n-hexane, and the plasticizer is lemon
Esters of gallic acid or epoxidized soybean oil, the curing agent be formic acid or acetic acid, the surfactant be neopelex or
Lauryl sodium sulfate.
3. a kind of thermally conductive foam with heat-conductive characteristic as described in claim 1, which is characterized in that modified carbon fiber
The preparation method is as follows:
1) it adds chitosan into glacial acetic acid/aqueous solution, is heated to 45-55 DEG C, stirring is completely dissolved to form shell to chitosan
Then ammonium persulfate is added in glycan solution, sodium hydroxide solution and vinyl pyrrolidone, heating is added after keeping the temperature 10-15min
To 65-70 DEG C, isothermal reaction 2-3h, modification of chitosan solution is made
2) will formalin and chloroformic solution mix after be added in container, adding triethylamine and adjusting pH is 9-10, then plus
Enter diethylenetriamine, 1-2h is reacted at 5-10 DEG C, then adds parahydroxyben-zaldehyde, is warming up to 80-90 DEG C, the reaction was continued
1-2h, to after reaction, be cooled to room temperature, benzoxazine is made in vacuum distillation removal solvent；
3) paraformaldehyde, sodium hydroxide solution are added in the there-necked flask for being equipped with blender and condensation reflux unit, are then risen
Temperature is cooled to 50-55 DEG C after paraformaldehyde dissolution, adds Bisphenol F and toluene solution, add after mixing to 70-80 DEG C
Enter aniline, be warming up to 85-90 DEG C, flow back 4-5h, after product stratification, separates lower-layer resin solution and at 80-85 DEG C
20-25min is rotated, then then moves to and is heated to 70-80 DEG C in vacuum drying oven, Bisphenol F-aniline type benzo is made in dry 3-5h
Oxazines；
4) Bisphenol F-aniline type benzoxazine is added in n,N-Dimethylformamide solution, carbon fiber is added after stirring and dissolving
Dimension, the vibrating dispersion 40-60min under 500-800W ultrasonic wave form dispersion liquid, then add benzoxazine and modified shell is poly-
Sugar juice is warming up to 70-80 DEG C, isothermal reaction 20-23h after mixing evenly, is then dried in vacuo 8-10h at 70-75 DEG C and goes
It except solvent, then moves in Muffle furnace, is heated to 200-240 DEG C, solidify 1-2h, then squeezed through extruder, can be prepared by being modified
Carbon fiber.
4. a kind of thermally conductive foam with heat-conductive characteristic as claimed in claim 3, wherein modified carbon fiber preparation step 1)
In, the mass volume ratio of the chitosan and glacial acetic acid/aqueous solution, sodium hydroxide solution, vinyl pyrrolidone solution is 1g:
15-20ml:4-6ml:5-7ml, glacial acetic acid content is 20-25% in the glacial acetic acid/aqueous solution, remaining is distilled water, the hydrogen
The concentration of sodium hydroxide solution be 3-5mol/L, the chitosan, ammonium persulfate mass ratio be 1:0.2-0.3.
5. a kind of thermally conductive foam with heat-conductive characteristic as claimed in claim 3, wherein modified carbon fiber preparation step 2)
In, the formaldehyde, chloroform, diethylenetriamine and parahydroxyben-zaldehyde volume ratio be 25-30:20-25:3-5:4-7, the first
The concentration of aldehyde is 35-38%.
6. a kind of thermally conductive foam with heat-conductive characteristic as claimed in claim 3, wherein modified carbon fiber preparation step 3)
In, the paraformaldehyde, sodium hydroxide solution, toluene solution and aniline mass volume ratio be 1g:2-3ml:1-1.5ml:
The mass ratio of 1.2-1.6ml, the paraformaldehyde and Bisphenol F is 1:1.2-1.5, and the concentration of the sodium hydroxide solution is 5-
8%。
7. a kind of thermally conductive foam with heat-conductive characteristic as claimed in claim 3, wherein modified carbon fiber preparation step 4)
In, the Bisphenol F-aniline type benzoxazine, n,N-Dimethylformamide solution, modification of chitosan solution mass volume ratio be
1g:8-10ml:3-4ml, the Bisphenol F-aniline type benzoxazine, carbon fiber and benzoxazine mass ratio are 1:1-2:0.5-
0.8, the screw diameter of the extruder is 60-90mm, draw ratio 1:24-30, revolving speed 20-90r/min, and head pressure is
15-25MPa。
8. a kind of thermally conductive foam with heat-conductive characteristic as described in Arbitrary Term in claim 1-3, which is characterized in that described
Thermally conductive foam with heat-conductive characteristic the preparation method is as follows: by polyurethane, polyethylene, dispersing agent, fire retardant, anti-aging
It shakes after agent, modified carbon fiber, foaming agent, plasticizer, curing agent, surfactant mixing in the case where power is 400-600W ultrasonic wave
Dispersion 30-40min is swung, blended liquid is formed, then by blended liquid in the foaming that frequency is 2400-2600MHz, power is 2-5kW
Microwave foaming 3-5min, then dries 1-2h in 200-260 DEG C of baking oven, can be prepared by required foam in furnace.
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| CN201811315885.9A CN109608865A (en) | 2018-11-07 | 2018-11-07 | A kind of thermally conductive foam with heat-conductive characteristic |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111548621A (en) * | 2019-12-31 | 2020-08-18 | 江西宏柏新材料股份有限公司 | Organic silicon resin flame-retardant polyurethane foam heat-insulating material and preparation method thereof |
| CN113652076A (en) * | 2021-05-26 | 2021-11-16 | 袁望平 | Dustproof sound insulation plate with buffering function and preparation method thereof |
-
2018
- 2018-11-07 CN CN201811315885.9A patent/CN109608865A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111548621A (en) * | 2019-12-31 | 2020-08-18 | 江西宏柏新材料股份有限公司 | Organic silicon resin flame-retardant polyurethane foam heat-insulating material and preparation method thereof |
| CN113652076A (en) * | 2021-05-26 | 2021-11-16 | 袁望平 | Dustproof sound insulation plate with buffering function and preparation method thereof |
| CN114806138A (en) * | 2021-05-26 | 2022-07-29 | 袁望平 | Dustproof acoustic celotex board with buffer function |
| CN113652076B (en) * | 2021-05-26 | 2022-12-27 | 苏州鱼得水电气科技有限公司 | Dustproof sound insulation plate with buffering function and preparation method thereof |
| CN114806138B (en) * | 2021-05-26 | 2024-02-02 | 广州市五羊艺冠声学材料有限公司 | Dustproof acoustic baffle with buffer function |
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