CN105348867A - Modification method of nano aluminium oxide - Google Patents
Modification method of nano aluminium oxide Download PDFInfo
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- CN105348867A CN105348867A CN201510940729.1A CN201510940729A CN105348867A CN 105348867 A CN105348867 A CN 105348867A CN 201510940729 A CN201510940729 A CN 201510940729A CN 105348867 A CN105348867 A CN 105348867A
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- aluminium oxide
- nano aluminium
- silane coupling
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
- C09C1/407—Aluminium oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a modification method of nano aluminium oxide. According to the method, nano aluminium oxide is modified by using different silane coupling agents, then epoxy bonds of the silane coupling agents react with carboxyl or amino bonds react with semi-blocked isocyanate bonds so as to introduce double bonds, and the modified nano aluminium oxide can be dispersed in waterborne polyurethane well, and participates in reaction in the process of light curing, so that the nano aluminium oxide and a resin matrix can be combined well, and therefore, the thermal conductivity of coatings is excellent.
Description
Technical field
The present invention relates to a kind of method of modifying of nano aluminium oxide.
Background introduction
Nanotechnology fast development in recent years, nano material gains great popularity with its special process based prediction model.Now be widely used in fields such as microelectronics, chemical industry, national defence, space flight.Nanometer is a kind of novel high function fine inorganic material, and since obtained nano-alumina powder end, the understanding of people to this new high-tech material is constantly deepened, and finds its numerous characteristics.
In heat conductive filler, nanometer has higher thermal conductivity, excellent thermostability and resistance to chemical corrosion, good electrical insulating property, and cheap and wide material sources and being used widely.But because nano particle size is little, surface energy is high, be in thermodynamics unsteady state, very easily assemble agglomerating, thus have impact on the practical application effect of nano particle.So surface modification must be carried out to nano particle, to reduce surface energy, reduce the agglomeration power between nano particle, improve its dispersiveness in the base and dispersion stabilization, reduce two-phase interface tension force, improve wettability, bonding force and the consistency between nano particle and matrix resin, thus improve the over-all properties of matrix material.
The surface modifying method of nanometer mainly contains Physical and chemical method.Physically modified mainly adopts mechanical force to disperse and ultrasonic wave dispersion, the main object reaching particle dispersion by high-speed stirring and high speed ball milling of mechanical force dispersion.Ultrasonic wave dispersion be produce when utilizing ultrasonic cavitation localized hyperthermia, high pressure or strong shock wave and microjet etc., weaken the interaction energy between nanoparticle, prevent nanometer from reuniting and making it dispersion.Nanometer water-absorbent is strong, and therefore nanoparticle and water molecules form hydrogen bond and crosslinked together, and carry out modification with physical method to Nanosurface merely, obtain product dispersiveness poor, effect is not very desirable.
Chemical method mainly fingering row mechanical force dispersion while at other chemical group of alumina surface grafting.Add the larger dispersion medium of some polarity and can increase wetting power, reduce the free energy of liquid, liquid/solid interface, improve the dispersity of nano particle, other macromolecule dispersing agent can also increase sterically hindered effect by increasing polymer substance adsorbent layer thickness, to reach the object suppressing particle agglomeration.The modification of other chemical group of alumina surface grafting, can improve the range of application increasing aluminum oxide with the consistency of resin matrix.But the chemical process complex process of the surperficial modified nano-alumina of preparation at present, cost is higher.
Summary of the invention
The object of the present invention is to provide a kind of method of modifying of nano aluminium oxide.The method by modification to nano aluminium oxide, the while of making the nano aluminium oxide that obtains and aqueous polyurethane have a good consistency when photocuring and urethane resin produce chemical bond, thus improve the over-all properties of whole system.
Technical scheme of the present invention is:
A method of modifying for nano aluminium oxide, comprises the steps:
(1) nanometer a-Al2O3, silane coupling agent and dimethylbenzene are joined in there-necked flask, stirring reaction 3 ~ 5h in 110 ~ 120 DEG C of temperature ranges, the solution suction filtration obtained is gone out nano aluminium oxide, then be placed on dry 2 ~ 4h in the baking oven of 120 ~ 140 DEG C, obtain modified nano-alumina A;
(2) A obtained, dimethylbenzene, catalyzer and polycarboxylic acid to be joined in there-necked flask stirring reaction 3 ~ 5h in 90 ~ 110 DEG C of temperature ranges, the solution suction filtration obtained is gone out nano aluminium oxide, then be placed on dry 2 ~ 4h in the baking oven of 120 ~ 140 DEG C, obtain modified nano-alumina B;
(3) join in there-necked flask by vulcabond, stopper, hydroxyl one end, one end containing the photosensitive group compound of ultraviolet, acetone and catalyzer under nitrogen atmosphere, stirring reaction 2 ~ 4h in 30 ~ 50 DEG C of temperature ranges, obtains solution C;
(4) the C solution temperature obtained is increased to 40 ~ 70 DEG C, is then slowly added drop-wise in C by A, reaction 2 ~ 3h, obtains modified nano-alumina D.
Silane coupling agent described in step (1) is γ-methacryloxypropyl trimethoxy silane (KH-570), γ-glycidyl ether oxygen propyl trimethoxy silicane (KH-560) and γ-aminopropyl triethoxysilane (KH-550); The mass ratio of nano aluminium oxide and silane coupling agent is: (1 ~ 3): the volume fraction of 100 dimethylbenzene is 90 ~ 95%; The mass ratio of dimethylbenzene and silane coupling agent is (200 ~ 1000): 1; Stirring velocity is 400 ~ 600r/min;
Catalyzer in step (2) be cetyl trimethylammonium bromide, triphenylphosphine, triethylbenzyl brometo de amonio, Tetrabutyl amonium bromide, in the mixture of one or more; Polycarboxylic acid is the mixture of one or more in oxalic acid, succinic acid, hexanodioic acid, sebacic acid;
Vulcabond in step (3) is tolylene diisocyanate (TDI), different Buddhist diisocyanates (IPDI), hexamethylene diisocyanate (HDI), 4, the mixture of one or more in 4 '-diphenylmethanediisocyanate; Hydroxyl one end, one end is one or more mixture of pentaerythritol triacrylate (PETA) or hydroxyethyl methylacrylate (HEMA) or Hydroxyethyl acrylate (HEA) containing the photosensitive group compound of ultraviolet, stopper is Resorcinol and the mixture to one or more in methoxyl group phenol, and hydroxy acrylate with the amount ratio of diisocyanate species is: n (hydroxyl acrylic): n (having vulcabond)=1:(1 ~ 3); The massfraction of acetone add-on is 5 ~ 20%; Catalyzer is dibutyl tin laurate;
The invention has the beneficial effects as follows: by above reaction, synthesis obtains the situation that modified nano-alumina can overcome the agglomeration of nanoparticle in water and the describing property difference in urethane resin, utilize the photocuring under the ultraviolet lamp of double bond, make nano aluminium oxide can be good at being dispersed in resin, increase the heat conductivility of urethane.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but embodiment does not form the restriction to application claims protection domain:
The tolylene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate etc. of all uses in embodiment, and hydroxyethyl methylacrylate, Rocryl 410 are all through that underpressure distillation obtains, catalysts and solvents is by molecular sieve process.
Embodiment 1
(1) a-Al2O3,0.01g of nanometer 1.02g γ-methacryloxypropyl trimethoxy silane (KH-570) silane coupling agent, 0.01g are joined in there-necked flask to methoxyl group phenol and 20g dimethylbenzene, stirring reaction 3h in 110 DEG C of temperature ranges, the solution suction filtration obtained is gone out nano aluminium oxide, then be placed on dry 2h in the baking oven of 120 DEG C, obtain modified nano-alumina A;
(2) under nitrogen atmosphere 3g tolylene diisocyanate, 0.01g are joined in there-necked flask to methoxyl group phenol, 5.13g pentaerythritol triacrylate (PETA), 5g acetone and 0.02g catalyzer, stirring reaction 4h in 50 DEG C of temperature ranges, obtains solution C;
(3) the C solution temperature obtained is increased to 70 DEG C, is then slowly added drop-wise in C by A, reaction 3h, obtains modified nano-alumina D.
Embodiment 2
(1) by nanometer 3ga-Al
2o
3, 0.03g silane coupling agent γ-glycidyl ether oxygen propyl trimethoxy silicane (KH-560) and 70g dimethylbenzene joins in there-necked flask, stirring reaction 5h in 120 DEG C of temperature ranges, the solution suction filtration obtained is gone out nano aluminium oxide, then be placed on dry 4h in the baking oven of 140 DEG C, obtain modified nano-alumina A;
(2) A, 70g dimethylbenzene obtained, 0.04g cetyl trimethylammonium bromide and 0.06g oxalic acid to be joined in there-necked flask stirring reaction 3h in 90 DEG C of temperature ranges, the solution suction filtration obtained is gone out nano aluminium oxide, then be placed on dry 2h in the baking oven of 120 DEG C, obtain modified nano-alumina B;
Embodiment 3
(1) by nanometer 2ga-Al
2o
3, 0.02g silane coupling agent γ-aminopropyl triethoxysilane (KH-550) and 80g dimethylbenzene joins in there-necked flask, stirring reaction 4h in 130 DEG C of temperature ranges, the solution suction filtration obtained is gone out nano aluminium oxide, then be placed on dry 3h in the baking oven of 130 DEG C, obtain modified nano-alumina A.
Claims (1)
1. a method of modifying for nano aluminium oxide, comprises the steps:
(1) by nanometer α-Al
2o
3, silane coupling agent and dimethylbenzene joins in there-necked flask, stirring reaction 3 ~ 5h in 110 ~ 120 DEG C of temperature ranges, the solution suction filtration obtained is gone out nano aluminium oxide, is then placed on dry 2 ~ 4h in the baking oven of 120 ~ 140 DEG C, obtains modified nano-alumina A;
(2) A obtained, dimethylbenzene, catalyzer and polycarboxylic acid to be joined in there-necked flask stirring reaction 3 ~ 5h in 90 ~ 110 DEG C of temperature ranges, the solution suction filtration obtained is gone out nano aluminium oxide, then be placed on dry 2 ~ 4h in the baking oven of 120 ~ 140 DEG C, obtain modified nano-alumina B;
(3) join in there-necked flask by vulcabond, stopper, hydroxyl one end, one end containing the photosensitive group compound of ultraviolet, acetone and catalyzer under nitrogen atmosphere, stirring reaction 2 ~ 4h in 30 ~ 50 DEG C of temperature ranges, obtains solution C;
(4) the C solution temperature obtained is increased to 40 ~ 70 DEG C, is then slowly added drop-wise in C by A, reaction 2 ~ 3h, obtains modified nano-alumina D.
Silane coupling agent described in step (1) is γ-methacryloxypropyl trimethoxy silane (KH-570), γ-glycidyl ether oxygen propyl trimethoxy silicane (KH-560) and γ-aminopropyl triethoxysilane (KH-550); The mass ratio of nano aluminium oxide and silane coupling agent is: (1 ~ 3): the volume fraction of 100 dimethylbenzene is 90 ~ 95%; The mass ratio of dimethylbenzene and silane coupling agent is (200 ~ 1000): 1; Stirring velocity is 400 ~ 600r/min;
Catalyzer in step (2) be cetyl trimethylammonium bromide, triphenylphosphine, triethylbenzyl brometo de amonio, Tetrabutyl amonium bromide, in the mixture of one or more; Polycarboxylic acid is the mixture of one or more in oxalic acid, succinic acid, hexanodioic acid, sebacic acid;
Vulcabond in step (3) is tolylene diisocyanate (TDI), different Buddhist diisocyanates (IPDI), hexamethylene diisocyanate (HDI), 4, the mixture of one or more in 4 '-diphenylmethanediisocyanate; Hydroxyl one end, one end is one or more mixture of pentaerythritol triacrylate (PETA) or hydroxyethyl methylacrylate (HEMA) or Hydroxyethyl acrylate (HEA) containing the photosensitive group compound of ultraviolet, stopper is Resorcinol and the mixture to one or more in methoxyl group phenol, and hydroxy acrylate with the amount ratio of diisocyanate species is: n (hydroxyl acrylic): n (having vulcabond)=1:(1 ~ 3); The massfraction of acetone add-on is 5 ~ 20%; Catalyzer is dibutyl tin laurate.
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| CN105754379A (en) * | 2016-03-28 | 2016-07-13 | 江南大学 | Surface modification method for aluminum oxide abrasive powder |
| CN106009649A (en) * | 2016-07-12 | 2016-10-12 | 蚌埠高华电子股份有限公司 | Antibacterial nylon heat-conductive composite material for LED lamp and preparation method of material |
| CN106009646A (en) * | 2016-07-12 | 2016-10-12 | 蚌埠高华电子股份有限公司 | Aging-resistant aluminum oxide-nylon heat conducting composite material for LED lamps and preparation method of composite material |
| CN106009652A (en) * | 2016-07-12 | 2016-10-12 | 蚌埠高华电子股份有限公司 | Aluminum oxide-nylon heat conduction composite material for LED lamp and preparing method thereof |
| CN106009648A (en) * | 2016-07-12 | 2016-10-12 | 蚌埠高华电子股份有限公司 | Titanium dioxide-polyamide thermal conductive composite material for LED lamps and preparation method of material |
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| CN106046771A (en) * | 2016-07-12 | 2016-10-26 | 蚌埠高华电子股份有限公司 | Weather-resistance LED-lamp aluminum oxide-nylon heat-conduction composite and preparing method thereof |
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| CN106084761A (en) * | 2016-07-11 | 2016-11-09 | 铜陵日兴电子有限公司 | A kind of LED alumina silicate fibre nylon heat-conductive composite material and preparation method thereof |
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Application publication date: 20160224 |