CN105255086B - A kind of heat conduction blended polymer material and its preparation technology - Google Patents
A kind of heat conduction blended polymer material and its preparation technology Download PDFInfo
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- CN105255086B CN105255086B CN201510763187.5A CN201510763187A CN105255086B CN 105255086 B CN105255086 B CN 105255086B CN 201510763187 A CN201510763187 A CN 201510763187A CN 105255086 B CN105255086 B CN 105255086B
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- benzenesulfonic acid
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Abstract
A kind of heat conduction blended polymer material and preparation method thereof, poly- N acryloylpiperidines solution is mixed to vinyl benzenesulfonic acid solution with poly- so that poly- N acryloylpiperidines are (50 55) % with the poly- mass percent to vinyl benzenesulfonic acid：(45 50) %, mix homogeneously obtain mixing polymer blend solution；Polymer blend solution coating will be mixed on substrate, after solvent volatilization, repetition continues above-mentioned coating process, until it reaches the thickness of needs；Then peel off from substrate, dry, annealing obtains heat conduction blended polymer material.The present invention simply uses the polymer of the low heat conduction of 2 classes, the high heat conductance of polymer blend is realized using its intermolecular hydrogen bonding and chain structure, thermal conductivity reaches 0.5 0.6W/ (mK), and system still has high electrical insulating property and breakdown strength, excellent machinability.The invention has process is simple, low for equipment requirements, and easy processing molding characteristic, processing cost are low.
Description
Technical field
The invention belongs to technical field of chemical product manufacture, is related to a kind of heat conduction blended polymer material and its prepares work
Skill.
Background technology
At present heat-conducting polymer material mainly using the inorganic particulate with Thermal conductivity for example aluminium oxide, aluminium nitride,
The filled polymers such as silicon nitride, due to the thermal conductivity of polymer itself it is extremely low, about 0.12-0.23W/m K, therefore generally require heat conduction
Inorganic particulate consumption reaches the thermal conductivity of more than 50-70wt% systems and is just significantly higher.Meanwhile, raise simultaneously in thermal conductivity
Excessive inorganic particulate causes the mechanical properties decrease of material, impact flexibility seriously to reduce, and electrical insulating property and breakdown strength glide.This
Outward, system viscosity is big, causes poor processability.
For the problem that presently, there are, generally carry out super drawing and can improve its draw direction leading to bulk polymer
Hot property, defines aligning for strand mainly due to the direction, reduces phonon transmission thermal resistance, therefore one-way heat conduction performance
Improve.But the method high cost of super drawing and commercial production cannot be realized, only reside within the experimental stage at present.And it is right
Have not been reported in the preparation and research of heat conduction polymer blend.
The content of the invention
It is an object of the invention to overcome the shortcoming that current thermal conductive polymer is present, there is provided a kind of heat conduction polymer blend material
Material and its preparation technology, the polymeric material that the preparation technology is obtained have high insulation, higher heat-conductivity, good mechanical strength and
The Intrinsical polymer of toughness, and the advantage of low cost processing.
For achieving the above object, the present invention is employed the following technical solutions：
A kind of heat conduction blended polymer material, based on quality percentage, including 50-55% poly- N- acryloylpiperidines with
And 45-50%'s is poly- to vinyl benzenesulfonic acid.
The weight average molecular weight of the poly- N- acryloylpiperidines is 7000-9000.
The poly- weight average molecular weight to vinyl benzenesulfonic acid is 12-15 ten thousand.
A kind of preparation technology of heat conduction blended polymer material, comprises the following steps：
1) prepared by polymer blend solution：
Poly- N- acryloylpiperidines are dissolved in into N-N, in dimethyl formamide solution, poly- N- acryloylpiperidines is made into molten
Liquid；N-N is dissolved in vinyl benzenesulfonic acid by poly-, in dimethyl formamide solution, is made into poly- to vinyl benzenesulfonic acid solution；By poly- N-
Acryloylpiperidine solution mixes to vinyl benzenesulfonic acid solution with poly- so that poly- N- acryloylpiperidines are with poly- to Ethenylbenzene sulphur
The mass percent of acid is (50-55) %：(45-50) %, mix homogeneously obtain mixing polymer blend solution；
2) rotary coating masking：
Polymer blend solution coating will be mixed on substrate, after solvent volatilization, repetition continues above-mentioned coating process, directly
To the thickness for reaching needs；Coating is finished, and after standing, peels off, obtain film sample from substrate；
3) it is dried and anneals：
Film sample is placed under nitrogen atmosphere and is dried, after making annealing treatment under nitrogen atmosphere, naturally cool to room
Temperature, obtains heat conduction blended polymer material.
The step 1) in poly- N- acryloylpiperidines weight average molecular weight be 7000-9000；Gather to vinyl benzenesulfonic acid
Weight average molecular weight is 12-15 ten thousand..
The step 1) in poly- N- acryloylpiperidines solution mass concentration be 1-3%；Gather to vinyl benzenesulfonic acid solution
Mass concentration be 0.6-1.0%.
The step 1) in mix homogeneously be first pass through ultrasonic 0.5-1h, then under room temperature, mechanical agitation 1-2h reaches.
The step 2) in coating rotating speed be 1200-1500rpm, the time is 15-25s.
The step 2) in stand time be 12-16h.
The step 3) in be dried temperature be 120-130 DEG C, the time is 1-2h；The temperature of annealing is 150-160
DEG C, the time is 0.2-0.3h.
Compared with prior art, the invention has the advantages that：
The present invention adopts a kind of totally new kind of design, prepares heat conduction polymer blend.Using two kinds of different molecular weights
And the polymer A and polymer B of strand compliance, polymer A belong to low-molecular-weight rigidity link structure polymer, i.e.,
Poly- N- acryloylpiperidines, polymer B are the poly- to vinyl benzenesulfonic acid polymer with flexible chain structure of high molecular.Profit
Intermolecular force, reinforcing blending effect, by hydrogen bond action and just are improved with the hydrogen bond action existed between polymer molecular weight
The template effect of property short chain polymer A so that the strand of long-chain flexible polymer B spread apart by random tangled structure
Come, arranged finally along the rigid chain of polymer A.Cooperative effect based on hydrogen bond and to each other so that long-chain polymer B
Define the structure with local order being adapted with A.By means of the dipole-dipole force of spinning apparatus so that polymer blend
Strand is further orientated, and the high temperature anneal under final nitrogen so that blending structure strand it is orderly
Structure increases, and finally realizes microcosmic local order structure in intrinsic silicon so that phonon is carried out along hydrogen bond and ordered structure
Transmission, effectively reduces interface resistance, and system thermal conductivity is significantly improved.The present invention is micro- to system based on molecule interchain hydrogen bond action
The regulation and control of structure are seen, local order structure is set up inside polymer blend, reduced the thermal resistance of phonon transmission, improve blending polymerization
Thing heat conductivility.
The present invention does not use heat conduction inorganic particulate, simply uses the polymer of the low heat conduction of 2 classes, using its intermolecular hydrogen bonding and
Realizing the high heat conductance of polymer blend, thermal conductivity reaches 0.5-0.6W/ (mK) to chain structure, and system still has high electricity
Insulating properties and breakdown strength, excellent machinability.Overcome mechanics, electricity and the processing characteristics deterioration of filling thermal conductive polymer
Many defect problems.The heat conduction blending polymeric system of the present invention is two-component polymer, does not use any inorganic particulate to fill out
Material, belongs to Intrinsical polymer, therefore system mechanical strength is high, and impact flexibility is good.Super drawing with intrinsic polymer system and
Electrostatic spinning is compared, and the invention has process is simple, low for equipment requirements, and easy processing molding characteristic, processing cost are low.The present invention
The heat conduction polymer blend of making and have high electrical insulating properties, low-k and dielectric loss factor, high-breakdown-voltage, be suitable for
Use in high insulating heat-conductive occasion.Heat conduction blended polymer material prepared by the present invention is in high performance copper clad laminate, solar energy, LED
The radiating occasion of the electronic equipments such as illumination, automotive electronics, computer, Switching Power Supply has extensive use
Description of the drawings
Fig. 1 heat conduction polymer blend interior microscopic local order structure schematic diagrams obtained in the present invention.
Specific embodiment
Below by specific embodiment, the present invention is described in detail.
Embodiment 1
1) mix polymer blend solution to prepare：
By the poly- N- acryloylpiperidines (poly (N- that weight average molecular weight is 7000-9000
Acryloylpiperidine N-N is dissolved in)), in dimethyl formamide solution, the poly- N- acryloyls that mass concentration is 1% is made into
Phenylpiperidines solution；Weight average molecular weight is dissolved in into N-N for the poly- of 12-15 ten thousand to vinyl benzenesulfonic acid, in dimethyl formamide solution, is matched somebody with somebody
Into mass concentration be 1.0% it is poly- to vinyl benzenesulfonic acid solution；By poly- N- acryloylpiperidines solution with poly- to vinyl benzenesulfonic acid
Solution mixes so that poly- N- acryloylpiperidines are 55% with the poly- mass percent to vinyl benzenesulfonic acid：45%, ultrasonic 1h,
Then mechanical agitation 2h under room temperature, obtains mixing polymer blend solution after mix homogeneously；
2) rotary coating masking：
Polymer blend solution coating will be mixed on spinning apparatus on substrate, the rotating speed of coating is 1200rpm,
Time is 20s, and after solvent volatilization, repetition continues above-mentioned coating process 5 times, until it reaches the thickness of needs；Coating is finished, quiet
14h is put, is treated that solvent volatilization is finished, is peeled off from substrate, obtain film sample.Film sample has certain thickness.
3) it is dried and anneals：
Film sample is placed under nitrogen atmosphere and 2h is dried at 120 DEG C, annealed under nitrogen atmosphere at 150 DEG C
After processing 0.3h, room temperature is naturally cooled to, heat conduction blended polymer material is obtained.
Embodiment 2
1) mix polymer blend solution to prepare：
The poly- N- acryloylpiperidines that weight average molecular weight is 7000 are dissolved in into N-N, in dimethyl formamide solution, are made into
Mass concentration is 2% poly- N- acryloylpiperidines solution；It is that 120,000 poly- is dissolved in N- to vinyl benzenesulfonic acid by weight average molecular weight
N, in dimethyl formamide solution, be made into mass concentration be 0.6% it is poly- to vinyl benzenesulfonic acid solution；By poly- N- acryloyl groups
Piperidine solution mixes to vinyl benzenesulfonic acid solution with poly- so that poly- N- acryloylpiperidines and the poly- quality to vinyl benzenesulfonic acid
Percentage ratio is 50%：50%, ultrasonic 0.5h, then mechanical agitation 1h under room temperature, obtains mixing polymer blend after mix homogeneously
Solution；
2) rotary coating masking：
Polymer blend solution coating will be mixed on spinning apparatus on substrate, the rotating speed of coating is 1500rpm,
Time is 15s, and after solvent volatilization, repetition continues above-mentioned coating process 4 times, until it reaches the thickness of needs；Coating is finished, quiet
12h is put, is treated that solvent volatilization is finished, is obtained with certain thickness film sample；
3) it is dried and anneals：
Film sample is placed under nitrogen atmosphere and 2h is dried at 125 DEG C, annealed under nitrogen atmosphere at 152 DEG C
After processing 0.3h, room temperature is naturally cooled to, thin film is peeled off from substrate, obtain heat conduction blended polymer material.
Embodiment 3
1) mix polymer blend solution to prepare：
The poly- N- acryloylpiperidines that weight average molecular weight is 9000 are dissolved in into N-N, in dimethyl formamide solution, are made into
Mass concentration is 3% poly- N- acryloylpiperidines solution；It is that 130,000 poly- is dissolved in N- to vinyl benzenesulfonic acid by weight average molecular weight
N, in dimethyl formamide solution, be made into mass concentration be 0.7% it is poly- to vinyl benzenesulfonic acid solution；By poly- N- acryloyl groups
Piperidine solution mixes to vinyl benzenesulfonic acid solution with poly- so that poly- N- acryloylpiperidines and the poly- quality to vinyl benzenesulfonic acid
Percentage ratio is 52%：48%, ultrasonic 0.6h, then mechanical agitation 2h under room temperature, obtains mixing polymer blend after mix homogeneously
Solution；
2) rotary coating masking：
Polymer blend solution coating will be mixed on spinning apparatus on substrate, the rotating speed of coating is 1300rpm,
Time is 17s, and after solvent volatilization, repetition continues above-mentioned coating process 5 times, until it reaches the thickness of needs；Coating is finished, quiet
13h is put, is treated that solvent volatilization is finished, is obtained with certain thickness film sample；
3) it is dried and anneals：
Film sample is placed under nitrogen atmosphere and 1h is dried at 130 DEG C, annealed under nitrogen atmosphere at 155 DEG C
After processing 0.3h, room temperature is naturally cooled to, thin film is peeled off from substrate, obtain heat conduction blended polymer material.
Embodiment 4
1) mix polymer blend solution to prepare：
The poly- N- acryloylpiperidines that weight average molecular weight is 8000 are dissolved in into N-N, in dimethyl formamide solution, are made into
Mass concentration is 1.5% poly- N- acryloylpiperidines solution；It is that 150,000 poly- is dissolved in vinyl benzenesulfonic acid by weight average molecular weight
N-N, in dimethyl formamide solution, be made into mass concentration be 0.8% it is poly- to vinyl benzenesulfonic acid solution；By poly- N- acryloyls
Phenylpiperidines solution mixes to vinyl benzenesulfonic acid solution with poly- so that poly- N- acryloylpiperidines and the poly- matter to vinyl benzenesulfonic acid
Amount percentage ratio is 55%：45%, ultrasonic 0.8h, then mechanical agitation 1.5h under room temperature, obtains mixing blending poly- after mix homogeneously
Polymer solution；
2) rotary coating masking：
Polymer blend solution coating will be mixed on spinning apparatus on substrate, the rotating speed of coating is 1400rpm,
Time is 20s, and after solvent volatilization, repetition continues above-mentioned coating process 6 times, until it reaches the thickness of needs；Coating is finished, quiet
15h is put, is treated that solvent volatilization is finished, is obtained with certain thickness film sample；
3) it is dried and anneals：
Film sample is placed under nitrogen atmosphere and 1.5h is dried at 120 DEG C, moved back under nitrogen atmosphere at 158 DEG C
After fire processes 0.25h, room temperature is naturally cooled to, thin film is peeled off from substrate, obtain heat conduction blended polymer material.
Embodiment 5
1) mix polymer blend solution to prepare：
Poly- N- acryloylpiperidine of the weight average molecular weight for 7000-9000 is dissolved in into N-N, in dimethyl formamide solution,
It is made into the poly- N- acryloylpiperidines solution that mass concentration is 2.5%；It is the poly- to Ethenylbenzene of 12-15 ten thousand by weight average molecular weight
Sulfonic acid is dissolved in N-N, in dimethyl formamide solution, be made into mass concentration be 0.9% it is poly- to vinyl benzenesulfonic acid solution；Will be poly-
N- acryloylpiperidines solution mixes to vinyl benzenesulfonic acid solution with poly- so that poly- N- acryloylpiperidines are with poly- to Ethenylbenzene
The mass percent of sulfonic acid is 53%：47%, ultrasonic 1h, then mechanical agitation 1h under room temperature, obtains mixing altogether after mix homogeneously
Mixed polymer solution；
2) rotary coating masking：
Polymer blend solution coating will be mixed on spinning apparatus on substrate, the rotating speed of coating is 1500rpm,
Time is 16s, and after solvent volatilization, repetition continues above-mentioned coating process 5 times, until it reaches the thickness of needs；Coating is finished, quiet
16h is put, is treated that solvent volatilization is finished, is obtained with certain thickness film sample；
3) it is dried and anneals：
Film sample is placed under nitrogen atmosphere and 1h is dried at 130 DEG C, annealed under nitrogen atmosphere at 160 DEG C
After processing 0.2h, room temperature is naturally cooled to, thin film is peeled off from substrate, obtain heat conduction blended polymer material.
The physical property contrast of 1 polymer blend of table and filling thermal conductive polymer
Fig. 1 heat conduction polymer blend interior microscopic local order structure schematic diagrams obtained in the present invention, in figure, long-chain gathers
Connected by hydrogen bond between compound and short chain polymer, referring to Fig. 1.The present invention is acted on poly- to improve blending based on intermolecular hydrogen bonding
Compound heat conductivility, gathers the vinyl benzenesulfonic acid to different molecular weight, poly- N- acryloylpiperidines Jing solution altogether by primary raw material
Under the coating of mixed, multiple rotary, nitrogen atmosphere, the process such as dry is prepared from.The invention is based on molecule interchain hydrogen bond action to system
The regulation and control of microstructure, set up local order structure so that hot-fluid flows through blending polymerization along hydrogen bond inside polymer blend
Thing interface, rather than through being conducted heat with the weak interface of van der Waals interaction, therefore, the thermal resistance of phonon transmission is effectively reduced, is changed
Kind polymer blend heat conductivility.The new blended polymer material that the present invention makes has higher heat-conductivity and high electric insulation
Property, with filled-type thermally conductive polymer phase ratio, the preparation technology relative ease of the heat conduction blended polymer material, mechanical strength and punching
Hit toughness good, performance comparison is shown in Table 1.Additionally, also having the characteristics such as the good, low cost of processing characteristics, it is expected to realize criticizing
Quantify commercial production.Heat conduction blended polymer material prepared by the invention is in high performance copper clad laminate, solar energy, LED illumination, automobile
The radiating occasion of the electronic equipments such as electronics, computer, Switching Power Supply has extensive use.
Claims (7)
1. a kind of heat conduction blended polymer material, it is characterised in that based on quality percentage, including the poly- N- acryloyls of 50-55%
Phenylpiperidines and 45-50%'s is poly- to vinyl benzenesulfonic acid；
The weight average molecular weight of the poly- N- acryloylpiperidines is 7000-9000；
The poly- weight average molecular weight to vinyl benzenesulfonic acid is 12-15 ten thousand；
It is obtained especially by procedure below：
1) prepared by polymer blend solution：
Poly- N- acryloylpiperidines are dissolved in into N-N, in dimethyl formamide solution, poly- N- acryloylpiperidines solution is made into；
N-N is dissolved in vinyl benzenesulfonic acid by poly-, in dimethyl formamide solution, is made into poly- to vinyl benzenesulfonic acid solution；By poly- N- propylene
Acylpiperidine solution mixes to vinyl benzenesulfonic acid solution with poly- so that poly- N- acryloylpiperidines are with poly- to vinyl benzenesulfonic acid
Mass percent is (50-55) %：(45-50) %, mix homogeneously obtain mixing polymer blend solution；
2) rotary coating masking：
Polymer blend solution coating will be mixed on substrate, after solvent volatilization, repetition continues above-mentioned coating process, until reaching
To the thickness for needing；Coating is finished, and after standing, peels off, obtain film sample from substrate；
3) it is dried and anneals：
Film sample is placed under nitrogen atmosphere and is dried, after making annealing treatment under nitrogen atmosphere, naturally cooled to room temperature, obtain
To heat conduction blended polymer material.
2. a kind of preparation technology of heat conduction blended polymer material, it is characterised in that comprise the following steps：
1) prepared by polymer blend solution：
Poly- N- acryloylpiperidines are dissolved in into N-N, in dimethyl formamide solution, poly- N- acryloylpiperidines solution is made into；
N-N is dissolved in vinyl benzenesulfonic acid by poly-, in dimethyl formamide solution, is made into poly- to vinyl benzenesulfonic acid solution；By poly- N- propylene
Acylpiperidine solution mixes to vinyl benzenesulfonic acid solution with poly- so that poly- N- acryloylpiperidines are with poly- to vinyl benzenesulfonic acid
Mass percent is (50-55) %：(45-50) %, mix homogeneously obtain mixing polymer blend solution；
2) rotary coating masking：
Polymer blend solution coating will be mixed on substrate, after solvent volatilization, repetition continues above-mentioned coating process, until reaching
To the thickness for needing；Coating is finished, and after standing, peels off, obtain film sample from substrate；
3) it is dried and anneals：
Film sample is placed under nitrogen atmosphere and is dried, after making annealing treatment under nitrogen atmosphere, naturally cooled to room temperature, obtain
To heat conduction blended polymer material；
Wherein, the step 1) in poly- N- acryloylpiperidines weight average molecular weight be 7000-9000；Gather to vinyl benzenesulfonic acid
Weight average molecular weight be 12-15 ten thousand.
3. a kind of preparation technology of heat conduction blended polymer material according to claim 2, it is characterised in that the step
1) in, the mass concentration of poly- N- acryloylpiperidines solution is 1-3%；The poly- mass concentration to vinyl benzenesulfonic acid solution is 0.6-
1.0%.
4. a kind of preparation technology of heat conduction blended polymer material according to claim 2, it is characterised in that the step
1) in, mix homogeneously is to first pass through ultrasonic 0.5-1h, and then under room temperature, mechanical agitation 1-2h reaches.
5. a kind of preparation technology of heat conduction blended polymer material according to claim 2, it is characterised in that the step
2) in, the rotating speed of coating is 1200-1500rpm, and the time is 15-25s.
6. a kind of preparation technology of heat conduction blended polymer material according to claim 2, it is characterised in that the step
2) time stood in is 12-16h.
7. a kind of preparation technology of heat conduction blended polymer material according to claim 2, it is characterised in that the step
3) temperature being dried in is 120-130 DEG C, and the time is 1-2h；The temperature of annealing is 150-160 DEG C, and the time is 0.2-
0.3h。
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| CN116496437A (en) * | 2023-05-15 | 2023-07-28 | 清华大学深圳国际研究生院 | Polymer material with high intrinsic thermal conductivity and preparation method thereof |
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