CN106317714A - Method of modifying nano-aluminium oxide using cold plasma - Google Patents

Method of modifying nano-aluminium oxide using cold plasma Download PDF

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Publication number
CN106317714A
CN106317714A CN201610710813.9A CN201610710813A CN106317714A CN 106317714 A CN106317714 A CN 106317714A CN 201610710813 A CN201610710813 A CN 201610710813A CN 106317714 A CN106317714 A CN 106317714A
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nano
aluminium oxide
load
solvent
monomer
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CN106317714B (en
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于水利
刘建伟
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Tongji University
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Tongji University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/021—After-treatment of oxides or hydroxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/10—Encapsulated ingredients
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • 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
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • 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
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/16—Applications used for films

Abstract

The present invention provides a method of modifying the nano-aluminium oxide using cold plasma, including: (1) the selection of different monomer loading pattern, i.e., direct loading or solvent-assisted loading based on the load rate of the monomer to be grafted on the surface of nano-aluminium oxide particles; and (2) apply the cold plasma treatment to the nano-aluminium oxide particles whose surface receive the load of the monomer to be grafted, wherein, the treating power is 10 W -150 W, time is 0.1s - 3,600s, temperature 10 - 400oC, and the cold plasma induces the monomers on the surface of nano-aluminium oxide particles to polymerize thus modifies the surface of nano-aluminium oxide.

Description

The low-temperature plasma modified processing method of nano-aluminium oxide
Technical field
The invention belongs to the modified field of nano-aluminium oxide material, be specifically related to nano-aluminium oxide low temperature etc. from Daughter modification processing method.
Background technology
Nano-particle suffers from wide application prospect in many fields such as medicine, biology and environment.Doped nanoparticle Organic material be that a class has special mechanical performance, heat stability, optical property, rheological property, chemical property and urges Change the advanced composite material (ACM) of performance.In the exploitation of this type of composite, nano-aluminium oxide because of its excellence mechanical performance, Absorption property and catalytic performance and receive much concern.But nano-aluminium oxide specific grain surface is long-pending and surface can be big, self pole Easily reunite, bad dispersibility in the composite；On the other hand, the poor chemical stability of nano-aluminium oxide is strong at strong acid Easily peel off from material matrix under the effect of alkali, cause the reduction of composite property.Nano-aluminium oxide is carried out table Face modification is the important method solving above-mentioned two problems.
Traditional method of modifying utilizes the absorption property of aluminium sesquioxide or the hydroxyl on its surface, is connect by chemical action The specific monomer of branch thus realize the modification of nano-particle.This method relates to the use of chemical solvent, making of these solvents With on the one hand health being worked the mischief, water body, soil can be damaged during on the other hand solvent is exposed to environment.Separately Outward, the method applicability of chemical graft is poor, and selectable monomer type is limited.
Non-thermal plasma trap is a kind of eco-friendly powder surface treatment technology.Treat that grafted monomers is incorporated into reactor After, plasma atmosphere is formed molecular fragment, these molecular fragments regroup at powder surface, thus realize powder body Cladding.Alkane, alkene, alkynes and vinyl monomer, under the effect of low temperature plasma, all can occur above-mentioned reaction, from And make grafting optional monomer scope significantly widen.But in traditional plasma treatment procedure, monomer is at powder surface Polymerization there is randomness, thus the uniformity of grafting is difficult to ensure that.
Therefore, this area aoxidizes two in the urgent need to the nanometer three developing a kind of defect that can overcome above-mentioned prior art The method of modifying of aluminum.
Summary of the invention
The invention provides the low-temperature plasma modified processing method of nano-aluminium oxide of a kind of novelty, thus solve Problems of the prior art.
The invention provides a kind of low-temperature plasma modified processing method of nano-aluminium oxide, the method includes following Step:
(1) according to treating the grafted monomers load factor size at nano-aluminium oxide particle surface, different monomers is selected Mode of loading, it may be assumed that directly load or solvent assistant load；And
(2) area load is treated that the nano-aluminium oxide granule of grafted monomers carries out Low Temperature Plasma Treating, its In, processing power is 10W～150W, and the time is 0.1s～3600s, and temperature is 10-400 DEG C, low temperature plasma induction nanometer The monomer polymerization of aluminium sesquioxide particle surface, it is achieved the surface modification of nano-aluminium oxide.
In one preferred embodiment, in step (1), described direct load refers in monomer charge rate to be grafted In the case of 10%, directly by nano-aluminium oxide with treat that grafted monomers mixes, thus realize monomer at nano-particle The uniform load on surface；Described solvent assistant load refers in the case of monomer charge rate to be grafted is less than 10%, by waiting Branch monomer dispersion is in solvent, then mixes and get rid of solvent with nano-aluminium oxide, thus realizes monomer at nano-particle The uniform load on surface.
Another preferred embodiment in, described in treat that grafted monomers is methyl methacrylate, hydroxyethyl methacrylate Ethyl ester, ethylene glycol, Polyethylene Glycol, vinylpyrrolidone, polyvinylpyrrolidone, vinyl alcohol, polyvinyl alcohol, dopamine, polymerization Dopamine or their mixture.
Another preferred embodiment in, the solvent in described solvent assistant load be water, methanol, ethanol, acetone, N-N dimethyl acetylamide, N-N dimethylformamide, N-Methyl pyrrolidone, triethyl phosphate, dimethyl sulfoxide or they Mixing liquid.
Another preferred embodiment in, the particle diameter of described nano-aluminium oxide granule is 10nm～100nm.
Another preferred embodiment in, in the case of directly load, described in treat grafted monomers and nanometer three oxygen The weight ratio changing two alumina particles is 5:1 to 1:100.
Another preferred embodiment in, in the case of solvent assistant load, described in monomer dispersion to be grafted arrive Weight ratio in solvent is 1:10000 to 1:10.
Another preferred embodiment in, use purity be 99.99% argon, nitrogen, helium or they Combination gas produces plasma atmosphere.
Another preferred embodiment in, in the case of directly load, directly by nano-aluminium oxide with After grafted monomers mixes, it is fully ground the uniform load realizing monomer at nano grain surface.
Another preferred embodiment in, in the case of solvent assistant load, by centrifugation and drying Mode gets rid of solvent.
Accompanying drawing explanation
Fig. 1 shows the transmission electron microscope of the low-temperature plasma modified nano-particle obtained according to the embodiment of the present application 1 Figure.
Fig. 2 shows that the rear before modified nano-particle according to the embodiment of the present application 2 is dispersed in N,N-dimethylacetamide, Standing the photo after 24h, in figure, (a) represents before modified, and (b) represents modified.
Fig. 3 shows PVDF (the poly-inclined difluoro second that the modified sample according to the embodiment of the present application 3 is prepared as additive Alkene) composite membrane under acid solution effect, the situation that nano-particle therein runs off in time.
Fig. 4 shows that PVDF composite membrane that modified sample according to the embodiment of the present application 4 prepared as additive is at alkali liquor Under effect, the situation that nano-particle therein runs off in time.
After Fig. 5 shows that the modified sample according to the embodiment of the present application 5 disperses in water, the distribution situation of particle diameter.
Detailed description of the invention
Present inventor, through extensively in-depth study, holds for nano-aluminium oxide granule in prior art Easily reunite, and the defect that traditional plasma grafting uniformity is poor, it is proposed that by monomer with nano-particle in advance with necessarily Ratio is sufficiently mixed the method for modifying carrying out Cement Composite Treated by Plasma again, and is usually used in water process filter membrane modification for nano-particle Purposes, using a series of ultrafilter membrane organic additives as the surface modifying material of nano-particle.The method of the present invention is at low temperature etc. Carrying out simple pretreatment before gas ions effect, decrease the correlation module introducing monomer in mechanism, process controllability is strong, Environmental friendliness；In organic solvent, the dispersibility of modified particles significantly improves；Modified particles change in composite pvdf membrane Stability significantly improves.
The invention provides a kind of nano-aluminium oxide surface low-temperature plasma modification processing method, the method includes Following steps:
The first step: directly monomer to be grafted is mixed with certain volume/weight ratio with nano-aluminium oxide granule Uniformly (in the case of monomer charge rate is more than 10%)；Or by monomer dispersion to be grafted to water or organic solvent In, then nano-dispersing agent is mixed with nano-particle, and by the way of centrifugation and drying, remove water or organic solvent (in the case of monomer charge rate is less than 10%), thus realize the pretreatment of nano-aluminium oxide；
Second step: be placed in reaction of low temperature plasma device by pretreated nano-aluminium oxide granule, sets one Granule is processed by fixed plasma parameter；And
3rd step: collect the sample after Low Temperature Plasma Treating.
In the present invention, in the first step, treat described in that grafted monomers is methyl methacrylate, hydroxyethyl methacrylate second Ester, ethylene glycol, Polyethylene Glycol, vinylpyrrolidone, polyvinylpyrrolidone, vinyl alcohol, polyvinyl alcohol, dopamine, polymerization are many Bar amine or their mixture.
In the present invention, in the first step, the organic solvent of described dispersed monomer is methanol, ethanol, acetone, N-N diformazan Yl acetamide, N-N dimethylformamide, N-Methyl pyrrolidone, triethyl phosphate, dimethyl sulfoxide or their mixed liquor Body.
In the present invention, in the first step, the particle diameter of described aluminum oxide nanoparticles is 10nm-100nm.
In the present invention, in the first step, described monomer and (volume/weight) of nano-particle are than (mL monomer solution/g Nano-particle) it is 5:1～1:100.
In the present invention, in the first step, described monomer dispersion is to the weight ratio (monomer weight/weight of solvent) in solvent For 1:10000 to 1:10.
In the present invention, in second step, argon, helium, nitrogen or the combinations thereof using purity to be 99.99% Gas produces plasma atmosphere.
In the present invention, in second step, the plasma discharge power of employing is 10W～150W, processes time 0.1s ～3600s, temperature is 10-400 DEG C.
Main advantages of the present invention are:
The present invention, compared with traditional grafting method, has the advantage that
1, technological process is simple, and controllability is strong, environmental friendliness；
2, nanoparticle agglomerates alleviates, and surface coated functional group improves its chemical resistance；
3, the processing mode that monomer and aluminum oxide nanoparticles are pre-mixed makes the uniformity of grafting significantly improve.
Embodiment
The present invention is expanded on further below in conjunction with specific embodiment.It should be appreciated, however, that these embodiments are only used for The bright present invention and be not meant to limit the scope of the invention.The test method of unreceipted actual conditions in the following example, generally According to normal condition, or according to the condition proposed by manufacturer.Except as otherwise noted, all of percentage ratio and number are by weight Meter.
Embodiment 1:
Processing step:
By methyl methacrylate and the aluminium sesquioxide that particle diameter is 10nm by volume/weight ratio 0.6mL/1.0g uniformly mixes Close, obtain the nano-aluminium oxide granule of pretreatment.Above-mentioned granule is placed in reaction of low temperature plasma device (model: PDC- 32G-2, production firm: Harrick Plasma) in, at the low temperature plasma atmosphere that temperature is 380 DEG C, discharge power 15W And the surface carrying out nano-aluminium oxide under conditions of processing time 30min processes.
Experimental result:
The transmission electron microscope photo of the treated sample of gained is as shown in Figure 1.It will be seen from figure 1 that at Jing Guo The nano grain surface of reason has one layer of irregular covering, illustrates that polymer wrapped is at nano grain surface.
Embodiment 2:
Processing step:
By methyl methacrylate and the aluminium sesquioxide that particle diameter is 20nm by volume/weight ratio 0.1mL/1.0g uniformly mixes Close, obtain the nano-aluminium oxide granule of pretreatment.Above-mentioned granule is placed in reaction of low temperature plasma device, in temperature is Nano-aluminium oxide is carried out under conditions of the low temperature plasma atmosphere of 320 DEG C, discharge power 50W and process time 10min Surface process.
Experimental result:
The treated sample dispersion of gained is (mass concentration is 1%) in organic solvent N,N-dimethylacetamide, quiet Put the contrast experiment after 24h to scheme as shown in Figure 2.Figure it is seen that the nano-particle modified through surface keeps in a solvent Preferable stability, it is possible to long-time stable is suspended in solvent, undressed nano-particle is deposited to the most quickly Container bottom.
Embodiment 3:
Processing step:
By methyl methacrylate and the aluminium sesquioxide that particle diameter is 10nm by volume/weight ratio 0.6mL/1.0g uniformly mixes Close, obtain the nano-aluminium oxide granule of pretreatment.Above-mentioned granule is placed in reaction of low temperature plasma device, at 280 DEG C Low temperature plasma atmosphere, discharge power 15W and process the surface carrying out nano-aluminium oxide under conditions of time 30min Process.
Experimental result:
The treated sample of gained is the acid soak of 1.65 as additive, the PVDF composite membrane prepared at pH Under, its aluminium sesquioxide wastage in time is as it is shown on figure 3, comparative example is to the addition of the PVDF of unmodified aluminium sesquioxide Composite membrane.From figure 3, it can be seen that under the immersion of acid solution, the nano-particle turnover rate that surface is modified is significantly lower than unmodified Grain, modification enhances the ability that the resistance to acid solution of nano-particle corrodes.
Embodiment 4:
Processing step:
By methyl methacrylate and the aluminium sesquioxide that particle diameter is 10nm by volume/weight ratio 0.6mL/1.0g uniformly mixes Close, obtain the nano-aluminium oxide granule of pretreatment.Above-mentioned granule is placed in reaction of low temperature plasma device, at 240 DEG C Low temperature plasma atmosphere, discharge power 15W and process the surface carrying out nano-aluminium oxide under conditions of time 30min Process.
Experimental result:
The treated sample of gained is the dipping by lye of 12.23 as additive, the PVDF composite membrane prepared at pH Under, its aluminium sesquioxide such as Fig. 4 of wastage in time, comparative example is that the PVDF that with the addition of unmodified aluminium sesquioxide is combined Film.From fig. 4, it can be seen that under the action of soaking of alkali liquor, the nano-particle turnover rate that surface is modified is significantly lower than unmodified Grain, modification enhances the ability that the resistance to alkali liquor of nano-particle corrodes.
Embodiment 5:
Processing step:
By hydroxyethyl methylacrylate and the aluminium sesquioxide that particle diameter is 10nm by volume/weight ratio 0.6mL/1.0g is uniform Mixing, obtains the nano-aluminium oxide granule of pretreatment.Above-mentioned granule is placed in reaction of low temperature plasma device, 200 DEG C low temperature plasma atmosphere, discharge power 15W and process the table carrying out nano-aluminium oxide under conditions of time 30min Face processes.
Experimental result:
The treated sample dispersion of gained to the particle diameter distribution in water as it is shown in figure 5, wherein 0min be undressed Aluminium sesquioxide granule.From fig. 5, it can be seen that the distribution curve left shift of the nano particle diameter through modifying, particle diameter shows Write and reduce, illustrate that modified nanoparticle agglomerates effect alleviates..
Above-mentioned listed embodiment is only presently preferred embodiments of the present invention, is not used for limiting the enforcement model of the present invention Enclose.The most all equivalence changes made according to the content of scope of the present invention patent and modification, all should be the technology model of the present invention Farmland.
The all documents mentioned in the present invention are incorporated as reference the most in this application, just as each document by individually It is incorporated as with reference to like that.In addition, it is to be understood that after the above-mentioned teachings having read the present invention, those skilled in the art can To make various changes or modifications the present invention, these equivalent form of values fall within the model that the application appended claims is limited equally Enclose.

Claims (10)

1. the low-temperature plasma modified processing method of nano-aluminium oxide, the method comprises the following steps:
(1) according to treating the grafted monomers load factor size at nano-aluminium oxide particle surface, different monomer charge is selected Mode, it may be assumed that directly load or solvent assistant load；And
(2) area load being treated, the nano-aluminium oxide granule of grafted monomers carries out Low Temperature Plasma Treating, wherein, place Reason power is 10W～150W, and the time is 0.1s～3600s, and temperature is 10-400 DEG C, and low temperature plasma induction nanometer three aoxidizes The monomer polymerization on two alumina particles surfaces, it is achieved the surface modification of nano-aluminium oxide.
2. the method for claim 1, it is characterised in that in step (1), described direct load refers to treating that grafting is single Body load factor more than in the case of 10%, directly by nano-aluminium oxide with treat that grafted monomers mixes, thus realize monomer and exist The uniform load of nano grain surface；Described solvent assistant load refers to be less than the situation of 10% in monomer charge rate to be grafted Under, will monomer dispersion be grafted in solvent, then mix and get rid of solvent with nano-aluminium oxide, thus realize monomer and exist The uniform load of nano grain surface.
3. method as claimed in claim 1 or 2, it is characterised in that described in treat that grafted monomers is methyl methacrylate, methyl 2-(Acryloyloxy)ethanol, ethylene glycol, Polyethylene Glycol, vinylpyrrolidone, polyvinylpyrrolidone, vinyl alcohol, polyvinyl alcohol, DOPA Amine, polymerization dopamine or their mixture.
4. method as claimed in claim 1 or 2, it is characterised in that the solvent in described solvent assistant load be water, methanol, Ethanol, acetone, N-N dimethyl acetylamide, N-N dimethylformamide, N-Methyl pyrrolidone, triethyl phosphate, dimethyl are sub- Sulfone or their mixing liquid.
5. method as claimed in claim 1 or 2, it is characterised in that the particle diameter of described nano-aluminium oxide granule is 10nm ～100nm.
6. method as claimed in claim 2, it is characterised in that in the case of directly loading, described in treat grafted monomers and receive The weight ratio of rice aluminium sesquioxide granule is 5:1 to 1:100.
7. method as claimed in claim 2, it is characterised in that in the case of solvent assistant load, described in treat grafted monomers The weight ratio being distributed in solvent is 1:10000 to 1:10.
8. method as claimed in claim 1 or 2, it is characterised in that the argon that uses purity to be 99.99%, nitrogen, helium or Person's combinations thereof gas produces plasma atmosphere.
9. method as claimed in claim 2, it is characterised in that in the case of directly load, directly nanometer three is being aoxidized Two aluminum, with after grafted monomers mixes, are fully ground the uniform load realizing monomer at nano grain surface.
10. method as claimed in claim 2, it is characterised in that in the case of solvent assistant load, by centrifugation and The mode dried gets rid of solvent.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107325861A (en) * 2017-05-31 2017-11-07 江苏金基特钢有限公司 A kind of preparation method for the cutting fluid for improving corrosion resistance of magnesium alloy energy
CN110130102A (en) * 2019-05-09 2019-08-16 常州大学 A kind of carbon nano-fiber surface modification method
CN112980055A (en) * 2021-03-09 2021-06-18 常州熠光智能科技有限公司 Composite antistatic additive and preparation method and application thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101417789A (en) * 2008-11-05 2009-04-29 东华大学 Plasma modification processing method of metallic oxide nano powder at atmosphere pressure and normal temperature
CN101982502A (en) * 2010-10-22 2011-03-02 北京化工大学 Elastomer thermal interface material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101417789A (en) * 2008-11-05 2009-04-29 东华大学 Plasma modification processing method of metallic oxide nano powder at atmosphere pressure and normal temperature
CN101982502A (en) * 2010-10-22 2011-03-02 北京化工大学 Elastomer thermal interface material and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107325861A (en) * 2017-05-31 2017-11-07 江苏金基特钢有限公司 A kind of preparation method for the cutting fluid for improving corrosion resistance of magnesium alloy energy
CN107325861B (en) * 2017-05-31 2020-10-20 玉田县玉盛集装箱有限公司 Preparation method of cutting fluid for improving corrosion resistance of magnesium alloy
CN110130102A (en) * 2019-05-09 2019-08-16 常州大学 A kind of carbon nano-fiber surface modification method
CN112980055A (en) * 2021-03-09 2021-06-18 常州熠光智能科技有限公司 Composite antistatic additive and preparation method and application thereof

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