CN104559136B - Aluminum oxide/polyurethane/epoxy resin heat-conductive composite material and preparation method thereof - Google Patents
Aluminum oxide/polyurethane/epoxy resin heat-conductive composite material and preparation method thereof Download PDFInfo
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- CN104559136B CN104559136B CN201410728340.6A CN201410728340A CN104559136B CN 104559136 B CN104559136 B CN 104559136B CN 201410728340 A CN201410728340 A CN 201410728340A CN 104559136 B CN104559136 B CN 104559136B
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Abstract
The present invention relates to aluminum oxide/polyurethane/epoxy resin heat-conductive composite material and preparation method thereof.Under the catalytic action of dibutyl tin laurate, reacted by IPDI and macromolecule dihydric alcohol, and using small molecular alcohol compounds as end-capping reagent, aliphatic polyurethane performed polymer is made, then mixed successively with epoxy resin and curing agent, by being heating and curing, aluminum oxide/polyurethane/epoxy resin heat-conductive composite material is prepared.Aluminum oxide/polyurethane/epoxy resin heat-conductive composite material prepared by the present invention has good heat conductivility and mechanical property concurrently, and being especially single use the epoxy resin disadvantage big as the fragility caused by heat conduction substrate can be obviously improved.
Description
Technical field
The present invention relates to heat-conductive composite material field, more particularly to a kind of aluminum oxide/polyurethane/epoxy resin heat conduction is compound
The preparation method of material.
Technical background
In recent years, based on the communication such as the active demand to convenience, mobile phone, tablet personal computer, digital camera and recreation apparatus
Material just gradually develops to the direction of miniaturization, and the thermal diffusivity of such electronic component just seems most important.Epoxy resin has
Good mechanical property, electrical property, adhesive property, heat endurance etc., are filled out by adding the heat conduction such as copper powder, aluminum oxide, aluminium nitride
Material, can prepare the epoxy resin-base composite material with Thermal conductivity.But epoxy resin divides in the curing process
Lack slip between subchain, easily form 3 D stereo network structure, crosslink density is big, therefore internal stress to be present big, crisp for solidified resin
The shortcomings of property is big, easy to crack, largely limits the further expansion of such composite application.
It is an effective method to carry out toughness reinforcing to epoxy resin based thermal conductive composite.Cao et al. is by nano oxygen
Change aluminium to be dispersed in polyester phase, then again with epoxy blend, be prepared for having the nano aluminium oxide of high rigidity and high tenacity/
Polyester/epoxy resin composite material, and electric conductivity and fine heat-resisting performance.But the prior art do not study nano aluminium oxide with
And influence (Cao Y M, Sun J, Yu D H.Preparation and of the polyester to composite heat conductivility
properties of nano‐Al2O3 particles/polyester/epoxy resin ternary composites
[J].Journal of Applied Polymer Science,2002,83(1):70‐77).Ban Jianfeng et al. is gathered using liquid crystal
Urethane is prepared for epoxy resin liquid crystal polyurethane/Al as modifying agent2O3/ epoxy resin composite material, although composite
Heat endurance increases, but fragility is not improved (the poly- ammonia of Ban Jianfeng, Qin Liqin, Pang Qi, Liang Chunjie, Tao Ping virtue liquid crystal
Ester/Al2O3Research [J] Yulin Teachers College's journals (natural science) of/epoxy resin composite material electrical property, 2011,32
(5):73‐77).There is document report recently, it is epoxy resin toughened using the hycar of carboxy blocking, can be with
Make yield strength, Young's modulus and impact strength that 2.7%, 5.5% and 20.9% (Zhou H S, Song X X, Xu be respectively increased
S A.Mechanical and thermal properties of novel rubber‐toughened epoxy blend
prepared by in situ pre‐crosslinking[J].Journal of Applied Polymer Science,
2014,131(22),DOI:10.1002/app.41110).But in system, heat filling is not added.
In summary, although having some at present on improving the brittle documents and materials of epoxy resin based thermal conductive composite,
But significant effect is not obtained also.
The content of the invention
It is an object of the invention to improve the shortcomings that epoxy resin based thermal conductive composite fragility is larger, there is provided one kind maintains
While heat conductivility and tensile strength, it was demonstrated that the elongation at break of material fragility is significantly improved aluminum oxide/polyurethane/ring
Oxygen tree fat heat-conductive composite material and preparation method thereof.
The present invention is first in the presence of initiator dibutyl tin laurate, with IPDI and big point
Sub- dihydric alcohol is reaction monomers, and small molecular alcohol compounds are end-capping reagent, and aliphatic polyurethane performed polymer is made；Then in pre-polymerization
Epoxy resin, aluminum oxide and curing agent are sequentially added in body, by being heating and curing, aluminum oxide/polyurethane/epoxy resin is made and leads
Hot composite.
The object of the invention is achieved through the following technical solutions：
The preparation method of aluminum oxide/polyurethane/epoxy resin heat-conductive composite material, comprises the following steps：
(1) in terms of mass fraction, will control temperature after the water removal of 20-40 part macromolecule dihydric alcohols compound as to 30-50 DEG C,
6-12 parts IPDI and the dibutyl tin laurate of 0.0025-0.25 parts are added, after being well mixed, heating
To 65-80 DEG C and react 1-4h；0.5-3.0 part small molecular alcohol compounds are added, continues to react 0.5-1h, is down to room temperature, obtains
Aliphatic polyurethane performed polymer；Described macromolecule dihydric alcohol compound is polyether Glycols or polyester diol, and molecular weight is
500‐2000；
(2) in terms of mass fraction, the liquid epoxies of 50-150 parts, heating are added in aliphatic polyurethane performed polymer
To 35-50 DEG C, 60-80 DEG C is warming up under stirring condition, vacuumizes and is stirred with 80-120rpm/min speed；Then add
The modified aluminas of 30-200 parts, stirred with 120-180rpm/min speed, be then cooled to 30-40 DEG C；Add 12-36 parts
Modified amine curing agent, after being stirred with 30-60rpm/min speed, pour the mixture into stainless steel mould,
After standing 5-10min in 60-65 DEG C of drying box, plus die cover, it is put into drying box in 60-80 DEG C and 110-130 DEG C of temperature
Solidify 2-3h in degree respectively, naturally cool to room temperature, open mould, obtain aluminum oxide/polyurethane/epoxy resin heat conduction composite wood
Material；Described modified amine curing agent is that phenol aldehyde modified aminated compounds (T31 curing agent), diethylenetriamines and butyl shrink
In the addition product (593 curing agent) or m-phenylene diamine (MPD) of glycerin ether and the condensation reaction thing (590 curing agent) of expoxy propane phenyl ether
One kind.
Preferably, the water removal is carried out in the condition that temperature is 100-120 DEG C and vacuum is 0.09-0.1MPa.Institute
The time for stating water removal is preferably 2-4h.
Described small molecular alcohol compounds are the one or more in ethanol, propyl alcohol and butanol.
The viscosity of described liquid epoxies is 2000-15000mPas.
The particle diameter of described aluminum oxide is 1-5 μm.
The time that 60-80 DEG C of stirring is warming up under the stirring condition is 10-60min.
The time that the speed using 80-120rpm/min stirs is 10-30min；With 120-180rpm/min speed
The time of stirring is 0.5-2h；The time stirred using 30-60rpm/min speed is 5-20min.
The present invention compared with prior art, has the following advantages that：
(1) aliphatic polyurethane performed polymer is used as flexible modifying agent, acid amides not only active in its molecular structure
Group, but also flexible C-C chains and C-O-C chains, have good compatibility with epoxy resin, can significantly improve asphalt mixtures modified by epoxy resin
The elongation at break of aliphatic radical heat-conductive composite material, so as to improve its fragility, further expand its use range.
(2) a small amount of NCO remained on aliphatic polyurethane performed polymer, can be with the epoxy radicals on epoxy resin
Chemically react, make between the two by formation of chemical bond inierpeneirating network structure, advantageously carrying in its elongation at break
It is high.
Embodiment
To more fully understand the present invention, with reference to embodiment, the present invention is further illustrated, but the reality of the present invention
It is unlimited so to apply mode.
Thermal conductivity in the present invention is according to GB/T 11205-2009 standard tests：By the survey that size is 180 × 180 × 2mm
After sample of having a try is placed on flat board, pressure as defined in application.Stable temperature is added in the one side of sample, heat will be by inputting temperature
The one side (hot face) of degree is delivered to another side (huyashi-chuuka (cold chinese-style noodles)), the measurement hot-fluid transmission capacity after stable, then calculates thermal conductivity through following formula：
λ=(QD)/[S (K1‐K2)]
In formula：λ-thermal conductivity, Wm‐1·K‐1；Q- hot-fluid transmission capacities, W；D- sample thickness, m；The surface of S- samples
Product, m2；K1- sample hot-face temperature, K；K2- sample coldface temperature, K.
Tensile strength and elongation at break in the present invention are tested according to ISO 0527, rate of extension 5mm/min.
Embodiment 1
Adding the polyether Glycols that 20g molecular weight is 2000 in the reactor, (trade mark N220, Sinopec's share have
Limit company Shanghai Gaoqiao Petrochemical Company), under conditions of 100 DEG C and vacuum are 0.09MPa, 50 DEG C are down to after removing water 3h；By 8g
IPDI and 0.05g dibutyl tin laurate are added in reactor, after being well mixed, are warming up to 70 DEG C
And react 3h；Finally, 0.5g ethanol is added in reactor, continues to react 1h, be down to room temperature, produce aliphatic polyurethane pre-polymerization
Body.Added in aliphatic polyurethane performed polymer liquid epoxies that 100g viscosity is 12000mPas (trade mark CYD-128,
Balin Branch Corp. SINOPEC), 40 DEG C are heated to, stirs 30min；60 DEG C are continuously heating to, is taken out true
Empty and with 100rpm/min speed stirs 30min；Then the aluminum oxide that 80g particle diameters are 5 μm is added, with 120rpm/min speed
Degree stirring 1h, is then cooled to 40 DEG C；28g 593 curing agent are added, will be mixed after 40rpm/min speed stirring 10min
Compound is poured into stainless steel mould, after standing 10min in 60 DEG C of drying box, plus die cover, is put into drying box in 80
DEG C and 120 DEG C solidify 2h respectively, naturally cool to room temperature, open mould, produce aluminum oxide/polyurethane/epoxy resin heat conduction and answer
Condensation material, its thermal conductivity, tensile strength and elongation at break are as shown in table 1.
Embodiment 2
Adding the polyether Glycols that 30g molecular weight is 1000 in the reactor, (trade mark N210, Sinopec's share have
Limit company Shanghai Gaoqiao Petrochemical Company), under conditions of 120 DEG C and vacuum are 0.1MPa, 40 DEG C are down to after removing water 2h；By 10g
IPDI and 0.005g dibutyl tin laurate are added in reactor, after being well mixed, are warming up to 80
DEG C and react 1h；Finally, 1g propyl alcohol is added in reactor, continues to react 0.5h, be down to room temperature, it is pre- to produce aliphatic polyurethane
Aggressiveness.Liquid epoxies (the trade mark CYD- that 150g viscosity is 8000mPas is added in aliphatic polyurethane performed polymer
127, Balin Branch Corp. SINOPEC), 50 DEG C are heated to, stirs 20min, makes it well mixed；After
It is continuous to be warming up to 70 DEG C, vacuumize and 10min is stirred with 120rpm/min speed；Then the oxidation that 100g particle diameters are 2 μm is added
Aluminium, 0.5h is stirred with 160rpm/min speed, is then cooled to 30 DEG C；32g T31 curing agent is added, with 30rpm/min's
After speed stirring 20min, pour the mixture into stainless steel mould, after standing 5min in 60 DEG C of drying box, plus mould
Lid, is put into drying box and solidifies 2h respectively in 60 DEG C and 130 DEG C, naturally cools to room temperature, opens mould, produces aluminum oxide/gather
Urethane/epoxy resin heat conduction composite, its thermal conductivity, tensile strength and elongation at break are as shown in table 1.
Embodiment 3
Polyester diol (trade mark SC-2000, the Yantai Hua Da chemistry work that 40g molecular weight is 2000 are added in the reactor
Industry Co., Ltd), under conditions of 110 DEG C and vacuum are 0.1MPa, 50 DEG C are down to after removing water 3h；By 12g isophorones two
Isocyanates and 0.1g dibutyl tin laurate are added in reactor, after being well mixed, are warming up to 65 DEG C and are reacted 3h；Most
Afterwards, 3g butanol is added in reactor, continues to react 0.5h, be down to room temperature, produce aliphatic polyurethane performed polymer.In aliphatic
Liquid epoxies (trade mark CYD-115C, the CNPC that 120g viscosity is 15000mPas are added in base polyurethane prepolymer for use as
Ba Ling branch companies of work limited company), 50oC is heated to, stirs 60min, makes it well mixed；80 DEG C are continuously heating to, is taken out
Vacuum simultaneously stirs 30min with 80rpm/min speed；Then the aluminum oxide that 200g particle diameters are 1 μm is added, with 180rpm/min's
Speed stirs 1h, is then cooled to 40 DEG C；20g 590 curing agent are added, will after 60rpm/min speed stirring 10min
Mixture is poured into stainless steel mould, after standing 10min in 60 DEG C of drying box, plus die cover, be put into drying box in
80 DEG C and 130 DEG C solidify 1h respectively, naturally cool to room temperature, open mould, produce aluminum oxide/polyurethane/epoxy resin heat conduction
Composite, its thermal conductivity, tensile strength and elongation at break are as shown in table 1.
Embodiment 4
Adding the polyether Glycols that 25g molecular weight is 400 in the reactor, (trade mark N210, Sinopec's share have
Limit company Shanghai Gaoqiao Petrochemical Company), under conditions of 120 DEG C and vacuum are 0.01MPa, 30 DEG C are down to after removing water 4h；By 12g
IPDI and 0.05g dibutyl tin laurate are added in reactor, after being well mixed, are warming up to 75 DEG C
And react 2h；Finally, 0.5g ethanol is added in reactor, continues to react 1h, be down to room temperature, produce aliphatic polyurethane pre-polymerization
Body.Added in aliphatic polyurethane performed polymer liquid epoxies that 140g viscosity is 1100mPas (trade mark CYD-115,
Balin Branch Corp. SINOPEC), 35 DEG C are heated to, stirs 10min, makes it well mixed；Continue to rise
Temperature vacuumizes to 70 DEG C and stirs 30min with 110rpm/min speed；Then the aluminum oxide that 150g particle diameters are 3 μm is added, with
150rpm/min speed stirring 1h, is then cooled to 35 DEG C；18g 593 curing agent are added, are stirred with 50rpm/min speed
After mixing 10min, pour the mixture into stainless steel mould, after standing 10min in 60 DEG C of drying box, plus die cover, put
Enter in drying box and solidify 2h respectively in 70 DEG C and 130 DEG C, naturally cool to room temperature, open mould, produce aluminum oxide/polyurethane/
Epoxy resin heat conduction composite, its thermal conductivity, tensile strength and elongation at break are as shown in table 1.
Comparative example 1
Liquid epoxies (trade mark CYD-128, the Chinese stone that 110g viscosity is 12000mPas are added in the reactor
Oily chemical inc Ba Ling branch companies), 40 DEG C are heated to, stirs 30min；Be continuously heating to 60 DEG C, vacuumize and with
100rpm/min speed stirring 30min；Then 80g aluminum oxide is added, 1h is stirred with 150rpm/min speed, then dropped
Temperature is to 40 DEG C；24g 593 curing agent are added, after 40rpm/min speed stirring 10min, pour the mixture into stainless steel mold
In tool, after standing 10min in 60oC drying box, plus die cover, it is put into drying box and solidifies respectively in 80 DEG C and 120 DEG C
2h, room temperature is naturally cooled to, open mould, produce aluminum oxide/epoxy resin heat conduction composite, its thermal conductivity, tensile strength
It is as shown in table 1 with elongation at break.
The thermal conductivity of aluminum oxide/polyurethane/epoxy resin heat-conductive composite material prepared by the embodiment of the present invention, stretching are strong
Degree and elongation at break are as shown in table 1.As it can be seen from table 1 compared with comparative example 1, the aluminum oxide/poly- ammonia of the invention prepared
While preferable heat conductivility and tensile strength is kept, its elongation at break also obtains ester/epoxy resin heat conduction composite
To significantly improving, i.e., fragility is effectively improved.
Table 1
| Sample | Thermal conductivity (Wm‐1·K‐1) | Tensile strength (MPa) | Elongation at break (%) |
| Embodiment 1 | 0.61 | 25 | 3.3 |
| Embodiment 2 | 0.65 | 34 | 4.3 |
| Embodiment 3 | 0.94 | 33 | 5.1 |
| Embodiment 4 | 0.86 | 38 | 2.8 |
| Comparative example 1 | 0.64 | 26 | 1.9 |
Claims (6)
1. the preparation method of aluminum oxide/polyurethane/epoxy resin heat-conductive composite material, it is characterised in that comprise the following steps：
(1) in terms of mass fraction, it is to 30-50 DEG C that temperature is controlled after 20-40 part macromolecule dihydric alcohols compound is removed water, and is added
6-12 parts IPDI and the dibutyl tin laurate of 0.0025-0.25 parts, after being well mixed, it is warming up to
65-80 DEG C and react 1-4h；0.5-3.0 part small molecular alcohol compounds are added, continues to react 0.5-1h, is down to room temperature, must contain
The aliphatic polyurethane performed polymer of isocyanate group；Described macromolecule dihydric alcohol compound is polyether Glycols or polyester binary
Alcohol, molecular weight 500-2000；
(2) in terms of mass fraction, the liquid epoxy of 50-150 parts is added in the aliphatic polyurethane performed polymer of isocyanato group containing
Resin, 35-50 DEG C is heated to, 60-80 DEG C is warming up under stirring condition, vacuumized and stirred with 80-120rpm/min speed；
Then the modified aluminas of 30-200 parts is added, is stirred with 120-180rpm/min speed, is then cooled to 30-40 DEG C；Add
Enter the modified amine curing agent of 12-36 parts, after being stirred with 30-60rpm/min speed, pour the mixture into stainless steel mold
In tool, after standing 5-10min in 60-65 DEG C of drying box, plus die cover, it is put into drying box in 60-80 DEG C and 110-
Solidify 2-3h respectively in 130 DEG C of temperature, naturally cool to room temperature, open mould, obtain aluminum oxide/polyurethane/epoxy resin heat conduction
Composite；Described modified amine curing agent is phenol aldehyde modified aminated compounds, diethylenetriamines and butyl glycidyl
The addition product or m-phenylene diamine (MPD) of ether and one kind in the condensation reaction thing of expoxy propane phenyl ether；
The water removal is carried out in the condition that temperature is 100-120 DEG C and vacuum is 0.09-0.1MPa；The time of the water removal
For 2-4h.
2. the preparation method of aluminum oxide according to claim 1/polyurethane/epoxy resin heat-conductive composite material, its feature
It is：Described small molecular alcohol compounds are the one or more in ethanol, propyl alcohol and butanol.
3. the preparation method of aluminum oxide according to claim 1/polyurethane/epoxy resin heat-conductive composite material, its feature
It is：The viscosity of described liquid epoxies is 2000-15000mPas.
4. the preparation method of aluminum oxide according to claim 1/polyurethane/epoxy resin heat-conductive composite material, its feature
It is：The particle diameter of described aluminum oxide is 1-5 μm.
5. the preparation method of aluminum oxide according to claim 1/polyurethane/epoxy resin heat-conductive composite material, its feature
It is：The time that 60-80 DEG C of stirring is warming up under the stirring condition is 10-60min.
6. the preparation method of aluminum oxide according to claim 1/polyurethane/epoxy resin heat-conductive composite material, its feature
It is：The time that the speed using 80-120rpm/min stirs is 10-30min；Stirred with 120-180rpm/min speed
Time be 0.5-2h；The time stirred using 30-60rpm/min speed is 5-20min.
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| CN110229521A (en) * | 2019-06-28 | 2019-09-13 | 青岛云路聚能电气有限公司 | A kind of Heat Conduction Material and the preparation method and application thereof |
| CN113604007B (en) * | 2021-08-05 | 2023-01-10 | 宁夏清研高分子新材料有限公司 | LCPU modified epoxy resin-based heat-conducting composite material and preparation method and application thereof |
| CN115044192B (en) * | 2021-11-30 | 2024-02-13 | 广东金戈新材料股份有限公司 | High-filling heat-conducting master batch applied to polyester plastics and preparation method thereof |
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