CN102675547A - Janus particle with double properties and preparation method thereof - Google Patents
Janus particle with double properties and preparation method thereof Download PDFInfo
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- CN102675547A CN102675547A CN2011100564778A CN201110056477A CN102675547A CN 102675547 A CN102675547 A CN 102675547A CN 2011100564778 A CN2011100564778 A CN 2011100564778A CN 201110056477 A CN201110056477 A CN 201110056477A CN 102675547 A CN102675547 A CN 102675547A
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Abstract
The invention discloses a Janus particle with double properties and a preparation method thereof. By employing cross-linked polymer colloidal particles as seeds and through a seed emulsion polymerization method, Janus particles with double properties are obtained on the basis of a phase separation mechanism; inorganic, metal and metal oxide compounded Janus particles with electrical, magnetic, optical properties are obtained through functional group modification and composition of function materials and can be used for the material field. The Janus particles have an emulsifying property in organic, inorganic dispersed phases or different organic dispersed phases and meanwhile the Janus particles have a great application prospect in the aspects of self-assembly, superhydrophobicity, nanomotor and the like. The preparation method provided by the invention is easy to operate, has the feasibility of mass production and can adapt to different needs by modification and composition of function materials.
Description
Technical field
The invention belongs to the material technology field, particularly one type has Janus particle of double properties and preparation method thereof.
Background technology
Janus is former to be meant the two-sided god in Rome; Since famous scientist de.Gennes in 1991 in its Nobel's comment, describe (P.G.De Gennes, Rev.Mod.Phys. behind the particle with double properties with Janus one speech; 1992; 64,645-648), the Janus particle has just caused that people study interest greatly.This is the research field of a cross discipline, relates to pharmacy, biological chemistry, many subjects such as physics and colloid chemistry; This is a field that is full of boundless vital force, at emulsifying agent, and catalyzer, transmitter; Many aspects such as indicating meter and nanometer motor exist great application prospect (A.Walther, M.Hoffmann and A.H.E.M ü ller, Angew.Chem., Int.Ed.; 2008,47,711-714; J.Choi, Y.Zhao, D.Zhang, S.Chien and Y.H.Lo, Nano Lett., 2003,3,995-1000; T.Nisisako, T.Torii, T.Takahashi and Y.Takizawa, Adv.Mater., 2006,18,1152-1156; R.Golestanian, T.B.Liverpool and A.Ajdari, Phys.Rev.Lett., 2005,94,220801; L.F.Valadares, Y.G.Tao, N.S.Zacharia, V.Kitaev, F.Galembeck, R.Kapral, G.A.Ozin, Small2010,6,565.)
Being used for preparing Janus particulate main method at present has: 1) optionally finishing method (V.N.Paunov, O.J.Cayre, Adv.Mater., 2004,16,788-791.).This method is suggested the earliest, simultaneously also is the simplest direct a kind of method, but the characteristics that are based on two dimensional surface make this method can not be used for mass preparation Janus particle.Recently, Granick etc. have proposed Pickering emulsion method (L.Hong, S.Jiang on the basis of this method; S.Granick, Langmuir, 2006; 22; 9495-9499.), make productive rate be greatly improved based on three-dimensional ball-type surface, but the use of a large amount of paraffin and organic solvent and remove and become restrictive factor.2) based on the emulsion polymerization that is separated (J.W.Kim, R.J.Larsen, D.A.Weitz, J.Am.Chem.Soc., 2006,128,14374-14377.).Because letex polymerization, this method are the most possible methods that realizes batch process.But the Janus particle for preparing in this way at present all can not deserve to be called Janus particle truly, and this is not thorough owing to being separated, and has polymer B in the polymer A all the time.Secondly, also have limited construction from part (Yin, Y.Lu, B.Gates, Y.Xia, J.Am.Chem.Soc.; 2001,123,8718-8729), microfluid method (Z.Nie, W.Li, M.Seo; S.Xu, E.Kumacheva, J Am.Chem.Soc., 2006,128,9408-9412.); The self-assembly method of segmented copolymer (R.Erhardt, M.Zhang, A.
H.Zettl, C.Abetz, P.Frederik, G.Krausch; V.Abetz, A.H.E.M ü ller, J.Am.Chem.Soc., 2003,125,3260-3267.) with (S.Reculusa such as surface nucleation method; C.Poncet-Legrand, A.Perro, E.Duguet, E.Bourgeat-Lami, C.Mingotaud; S.Ravaine, Chem.Mater., 2005,17,3338-3344.).Generally speaking; The Janus particulate prepares the critical problem that the aspect mainly exists two aspects at present: A) pure Janus particulate preparation, because the asymmetry on the chemical property has more tangible research and using value than the asymmetry on the appearance structure.B) Janus particulate batch preparations, this is the basis that the potential application of Janus particulate is achieved.Therefore, proposition is a kind of can the pure Janus particulate of batch preparations method seem most important.
Summary of the invention
The purpose of this invention is to provide a kind of Janus particle and preparation method thereof with double properties.
A kind of batch preparations Janus particulate method provided by the invention; After comprising the steps: crosslinked polymeric colloid particles dispersed obtained seed solution in water; Emulsion system is added drop-wise in the said seed solution reacts, reaction finishes and obtains said Janus particle; Wherein, said emulsion system is obtained by monomer, linking agent, emulsifying agent, initiator and water mixing and emulsifying.
In this method, said crosslinked polymeric colloid particle is selected from least a in polyacrylonitrile and the polyacrylic ester, and degree of crosslinking is 10-80%; Preferred 50%, said crosslinked polymeric colloid particulate diameter is 10nm-100 μ m, preferred 400nm-1 μ m; Said crosslinked polymeric colloid particle is hollow or solid polymeric colloid particle; In the said hollow crosslinked polymeric colloid particle, shell thickness is 1nm-10um, preferred 100nm-1um;
Said monomer is selected from least a in the alkene that the total number of carbon atoms is 4-24, optimization styrene; Said linking agent is selected from least a in Vinylstyrene and the ethylene glycol dimethacrylate; Said initiator is selected from least a in Potassium Persulphate, ammonium persulphate, Sodium Persulfate and the hydrogen peroxide; Said emulsifying agent is selected from least a in sodium laurylsulfonate and the sodium lauryl sulphate.The mass percentage concentration of said seed solution is 0.1-30%, specifically can be 3.2%, preferred 1-10%; The mass percentage concentration of said monomer in said emulsion system is 0.1-20%, is specially 1.5%, preferred 1-10%; The mass percentage concentration of said linking agent in said emulsion system is 0.1-20%, specifically can be 4.4%, preferred 1-10%; The mass percentage concentration of said emulsifying agent in said emulsion system is 0.01-5%, is specially 2.9%, preferred 0.1-3%; The mass percentage concentration of said initiator in said emulsion system is 0.01-1%, is specially 0.03%, preferred 0.01-0.1%; The weight of said emulsion system is 0.1-20 times of said seed solution weight, and preferred 10-20 doubly; In the said dropping step, rate of addition is 0.01-5ml/ minute, preferred 0.1-0.5ml/ minute; In the said reactions step, temperature is 60-90 ℃, specifically can be 80 ℃, and preferred 75-85 ℃, the time is 2-10 hour, preferred 6-8 hour.
Method for preparing and the Janus particle also belong to protection scope of the present invention.This Janus particulate diameter is 10nm-100 μ m, preferred 400nm-1 μ m.
Preparation modification Janus particulate method provided by the invention comprises the steps: said Janus particles dispersed is carried out back flow reaction in basic soln, and reaction finishes and with acidic solution reaction system transferred to neutrality again, obtains the Janus particle of said modification.
In this method, said basic soln is selected from least a in the aqueous solution of the aqueous solution and Pottasium Hydroxide of sodium hydroxide, and the mass percentage concentration of said basic soln is 0.05-20%, specifically can be 5%, preferred 1-10%; Said acidic solution is selected from least a in hydrochloric acid and the acetic acid, and the mass percentage concentration of said acidic solution is 0.05-30%, preferred 1-10%; The mass percentage concentration of said Janus particle in reaction system is 0.1-60%, specifically can be 1%, preferred 1-20%; In the said reactions step, the time is 1-24 hour, preferred 12-24 hour.
Method for preparing and the Janus particle of modification, also belong to protection scope of the present invention.This Janus particulate diameter is 10nm-100 μ m, preferred 400nm-1 μ m.
Preparation nano particle compound Janus particulate method provided by the invention; Comprise the steps: that Janus particles dispersed with said modification is in water; Add the nanoparticles solution that has opposite charges and adsorb, obtain said nano particle compound Janus particle (also promptly utilizing electrostatic adsorption to prepare nano particle compound Janus particle);
Wherein, the said nano particle that has opposite charges is selected from SiO
2, Fe
3O
4, TiO
2, Au, Ag, Fe, Pd, Pt, FeO, Fe
3O
4, Fe
2O
3, Al
2O
3, SnO
2, Eu
2O
3, MnO
2, CaCO
3, in CoO, NiO, ZnO and the CdTe nano particle any one, preferred Au, Ag, Pd and Fe
3O
4In any one; The said particle diameter that has the nano particle of opposite charges is 1-50nm, specifically can be 2-4nm, 2-8nm or 4-8nm, preferred 2-10nm; The mass percentage concentration of the Janus particle of said modification in the system of being made up of the Janus particle and the water of said modification is 0.1-40%, specifically can be 9%, preferred 5-20%; In the said adsorption step, temperature is 20-40 ℃, specifically can be 25 ℃, and preferred 20-30 ℃, the time is 1-24 hour, specifically can be 5 hours, preferred 12-24 hour.
Method for preparing and nano particle compound Janus particle, also belong to protection scope of the present invention.This Janus particulate diameter is 10nm-100 μ m, preferred 400nm-1 μ m.
The Janus particulate method of preparation metal composite provided by the invention; Comprise the steps: the Janus particle of said modification is immersed in the aqueous solution of metal cation salt; The aqueous solution that adds reductive agent again after immersion finishes reacts, the Janus particle (also promptly utilizing in-situ reducing to prepare the Janus particle of metal composite) that reaction finishes and obtains said metal composite.
In this method, in the aqueous solution of said metal cation salt, said metal cation salt is any one in the soluble salt of following metals ion: Au
3+, Ag
+, Pt
2+, Pd
2+, Fe
2+, Fe
3+, Zn
2+, Mn
2+, Co
2+, Ni
2+, Cu
2+And Mg
2+, any one in preferred perchlorate, muriate, nitrate salt and the vitriol; Said reductive agent is selected from NaBH
4, LiB (C
2H
5)
3H and N
2H
4In any one;
The mass percentage concentration of the aqueous solution of said metal cation salt is 0.01-60%, specifically can be 1%, preferred 1-20%; The mass percentage concentration of said Janus particle in the aqueous solution of metal cation salt is 0.1-40%, preferred 10-30%; The mass percentage concentration of the aqueous solution of said reductive agent is 0.01-60%, specifically can be 5-10%, preferred 1-20%; In the said soaking step, temperature is 25-90 ℃, and preferred 30-60 ℃, the time is 1-48 hour, specifically can be 10 hours, preferred 12-24 hour; In the said reactions step, temperature is 10-90 ℃, and preferred 25-50 ℃, the time is 2-10 hour, specifically can be 2-8 hour, preferred 6-8 hour.
Method for preparing and the Janus particle of metal composite, also belong to protection scope of the present invention.This Janus particulate diameter is 10nm-100 μ m, preferred 400nm-1 μ m.
The Janus particulate method of preparation inorganic compounding provided by the invention; The Janus particles dispersed that comprises the steps: modification is adsorbed in the solution of inorganics precursor; After absorption finishes with the reaction that in alcohol and water, is hydrolyzed of gained Janus particles dispersed, the Janus particle that reacting finishes obtains said inorganic compounding (also promptly utilizing the Janus particle of the inorganic compounding that sol-gel method prepares).
In this method, in the solution of said inorganics precursor, the inorganics precursor is selected from Si (OCH
3)
4, Si (OCH
2CH
3)
4, Si{OCH (CH
3)
2}
4, Si (OCH
2CH
2CH
2CH
3)
4, Na
2SiO
3, TiCl
4, Ti (OCH
3)
4, Ti (OCH
2CH
3)
4, Ti{OCH (CH
3)
2}
4, Ti (OCH
2CH
2CH
2CH
3)
4, TiOSO
4, SnCl
4, Sn (OCH
3)
4, Sn (OCH
2CH
3)
4, Sn{OCH (CH
3)
2}
4, Sn (OCH
2CH
2CH
2CH
3)
4, ZrCl
4, Zr (OCH
3)
4, Zr (OCH
2CH
3)
4, Zr{OCH (CH
3)
2}
4, Zr (OCH
2CH
2CH
2CH
3)
4, AlCl
3, Al (OCH
3)
4, Al (OCH
2CH
3)
4, Al{OCH (CH
3)
2}
4, Al (OCH
2CH
2CH
2CH
3)
4And Al
2(SO
4)
3In any one, preferred Si (OCH
3)
4And Ti (OCH
3)
4In any one, solvent is that the total number of carbon atoms is the monohydroxy-alcohol of 1-10, said the total number of carbon atoms is the monohydroxy-alcohol of 1-10, preferred alcohol; The mass percentage concentration of the solution of said inorganics precursor is 0.01%-60%, preferred 20-50%; The mass percentage concentration of said Janus particle in the solution of said inorganics precursor is 0.1%-40%, preferred 10-20%; In the said adsorption step, temperature is 25-90 ℃, and preferred 30-60 ℃, the time is 1-48 hour, preferred 12-24 hour; In the said hydrolysis reaction step, the pH value of solution is 1-13, preferred 8-10; In the said hydrolysis reaction step, the pH value of solution is that to use mass percentage concentration be that 35% hydrochloric acid or 25% ammoniacal liquor are regulated; In the said hydrolysis reaction step, temperature is 25-90 ℃, and preferred 30-60 ℃, the time is 1-48 hour, preferred 12-24 hour.
Method for preparing and the Janus particle of inorganic compounding, also belong to protection scope of the present invention.This Janus particulate diameter is 10nm-100 μ m, preferred 400nm-1 μ m.
Preparation SiO provided by the invention
2The SiO of partial functionization
2Compound Janus particulate method comprises the steps: the Janus particles dispersed for preparing the gained inorganic compounding in non-polar solvent, to react behind adding silane coupling agent and the water, and reaction finishes and obtains said SiO
2The SiO of partial functionization
2Compound Janus particle.
In this method, said silane coupling agent is the compound with following structure: C
nH
2n+1-Si (R
2)
3, C
nH
2n+1-SiCH
3(R
2)
2, R
3-C
mH
2mSi (R
2)
3,
R
3-C
m?H
2mSi?CH
3(R
2)
2、(C
2H
5O)
3-Si-(CH
2)
3-S-S-S-S-(CH
2)
3-Si-(OC
2H
5)
3、(C
2H
5O)
3-Si-(CH
2)
3-S-S-(CH
2)
3-Si-(OC
2H
5)
3。
Wherein, n is the integer of 1-121, the integer of preferred 5-50, and m is the integer of 0-126, the integer of preferred 5-50;
R
2Be Cl, OCH
3, OCH
2CH
3Or OC
2H
4OCH
3
R
3Be NH
2, CH
2=CH, HS, SCN, NHCONH
2, phenyl, epoxy group(ing), Cl, NH
2(CH
2)
2NH,
Or
The preferred octadecyl Trimethoxy silane of said silane coupling agent; Said non-polar solvent is selected from least a in monohydroxy-alcohol that the total number of carbon atoms is 1-10 and the vinyl acetic monomer, and said the total number of carbon atoms is the monohydroxy-alcohol of 1-10, preferred alcohol; Said silane coupling agent accounts for the 1-10% of the Janus particle weight of preparation gained inorganic compounding, specifically can be 5%; The mass percent concentration of Janus particle in said non-polar solvent of said preparation gained inorganic compounding is 0.1-40%, is specially 10%; The mass percentage concentration of said water is 0.1-40%, is specially 8.7%, preferred 1-20%; In the said reactions step, temperature is 25-40 ℃, and preferred 25-30 ℃, the time is 5-24 hour, is specially preferred 12-24 hour 10 hours.
Method for preparing and SiO
2The SiO of partial functionization
2Compound Janus particle also belongs to protection scope of the present invention.This Janus particulate diameter is 10nm-100 μ m, preferred 400nm-1 μ m.
The SiO of preparation polymer moieties functionalization provided by the invention
2Compound Janus particulate method comprises the steps: in the following Janus particle any one be dispersed in the acid solution and reacts, and reaction finishes and obtains the SiO of said polymer moieties functionalization
2Compound Janus particle: Janus particle or preceding method that preceding method prepares the gained inorganic compounding prepare gained SiO
2The SiO of partial functionization
2Compound Janus particle.
In this method, said acid solution is selected from least a in sulfuric acid, hydrochloric acid and the nitric acid; The mass percentage concentration of said Janus particle in acid solution is 0.1-40%, preferred 10-30%; The mass percentage concentration of said acid solution is 1-100%, preferred 35-100%; In the said reactions step, temperature is 25-90 ℃, and preferred 25-40 ℃, the time is 1-48 hour, preferred 12-24 hour.
Method for preparing and the SiO of polymer moieties functionalization
2Compound Janus particle also belongs to protection scope of the present invention.This Janus particulate diameter is 10nm-100 μ m, preferred 400nm-1 μ m.
The present invention is a seed with crosslinked polymeric colloid particle, through the seeded emulsion polymerization method, based on the mechanism that is separated, obtains having the Janus particle of double properties.Inorganic through the compound preparation of functional group modification and functional mass again, metal, MOX compound have the Janus particle of electricity, magnetic, light characteristic, can be used for field of materials; This type Janus particle has emulsifying property in organic and inorganic disperse phase or different organic disperse phase, this type Janus particle all exists great application prospect at aspects such as self-assembly, super-hydrophobic and nanometer motors simultaneously.Method provided by the invention, simple and easy to do, not only have the feasibility of scale operation, and can be through modification and functional mass compound to adapt to different demands.
Description of drawings
Fig. 1 is the embodiment of the invention 1 preparation gained Janus particulate scanning and a transmission electron microscope photo.
Fig. 2 is the embodiment of the invention 3 preparation gained Janus particulate scanning and transmission electron microscope photos.
Fig. 3 is a Janus particulate infrared spectrum before and after the embodiment of the invention 4 preparation gained modifications.
Fig. 4 is the optical microscope photograph and the camera photo of the embodiment of the invention 4 preparation gained emulsions.
Fig. 5 is the embodiment of the invention 5 preparation gained absorption Fe
3O
4Scanning of particulate Janus particulate and transmission electron microscope photo.
Fig. 6 is the embodiment of the invention 10 preparation gained composite S iO
2Janus particulate scanning and transmission electron microscope photo.
Embodiment
Below in conjunction with specific embodiment the present invention is done further elaboration, but the present invention is not limited to following examples.Said method is ordinary method if no special instructions.Said material all can get from open commercial sources if no special instructions.
Embodiment 1, prepare the Janus particle in enormous quantities
Is that 50% crosslinked polypropylene nitrile hollow ball-shape particle (shell thickness is 100nm) is dispersed in the 15g water with the 0.5g diameter for the 400nm degree of crosslinking, and ultra-sonic dispersion is even, obtains mass percentage concentration and be 3.2% seed solution; In addition, with 0.25g monomer styrene (St), 0.75g linking agent Vinylstyrene (DVB); 0.5g emulsifying agent sodium laurylsulfonate (SDS), 0.5g mass percentage concentration are the aqueous solution and the 15g water of 1% the Potassium Persulphate as initiator (KPS), mix ultrasonic emulsification; Obtain emulsion system; In this emulsion system, the mass percentage concentration of monomer styrene is 1.5%, and the mass percentage concentration of linking agent Vinylstyrene is 4.4%; The mass percentage concentration of emulsifying agent sodium laurylsulfonate is 2.9%, and the mass percentage concentration of initiator potassium persulfate is 0.03%; Above-mentioned seed solution is heated to 80 ℃, begins to drip the above-mentioned emulsion system then, rate of addition is 0.1ml/ minute, and dropping is incubated 6 hours after finishing.Reaction finishes, and with ethanol/water centrifuge washing product, obtains Janus particle provided by the invention.
Characterize gained Janus particulate structure with sem (SEM) and transmission electron microscope (TEM), as shown in Figure 1.Can know that by Fig. 1 this embodiment prepares gained Janus particle and has snowman's shape structure, and two portions have various structure and size.
Embodiment 2, prepare the Janus particle in enormous quantities
With the 0.5g diameter for the 1um degree of crosslinking be 50% the solid spherical particles dispersed of crosslinked polypropylene nitrile in 15g water, ultra-sonic dispersion is even, obtains mass percentage concentration and be 3.2% seed solution; In addition, with 0.25g monomer styrene (St), 0.75g linking agent Vinylstyrene (DVB); 0.5g emulsifying agent sodium laurylsulfonate (SDS), 0.5g mass percentage concentration are the aqueous solution and the 15g water of 1% the Potassium Persulphate as initiator (KPS), mix ultrasonic emulsification; Obtain emulsion system; In this emulsion system, the mass percentage concentration of monomer styrene is 1.5%, and the mass percentage concentration of linking agent Vinylstyrene is 4.4%; The mass percentage concentration of emulsifying agent sodium laurylsulfonate is 2.9%, and the mass percentage concentration of initiator potassium persulfate is 0.03%; Above-mentioned seed solution is heated to 80 ℃, begins to drip the above-mentioned emulsion system then, rate of addition is 0.5ml/ minute, and dropping is incubated 6 hours after finishing.Reaction finishes, and with ethanol/water centrifuge washing product, obtains Janus particle provided by the invention.
Embodiment 3, prepare the Janus particle in enormous quantities
Is that 50% crosslinked polymethylmethacrylaparticles hollow ball-shape particle (shell thickness is 100nm) is dispersed in the 15g water with the 0.5g diameter for the 400nm degree of crosslinking, and ultra-sonic dispersion is even, obtains mass percentage concentration and be 3.2% seed solution; In addition, with 0.25g monomer styrene (St), 0.75g linking agent Vinylstyrene (DVB); 0.5g emulsifying agent sodium laurylsulfonate (SDS), 0.5g mass percentage concentration are the aqueous solution and the 15g water of 1% the Potassium Persulphate as initiator (KPS), mix ultrasonic emulsification; Obtain emulsion system; In this emulsion system, the mass percentage concentration of monomer styrene is 1.5%, and the mass percentage concentration of linking agent Vinylstyrene is 4.4%; The mass percentage concentration of emulsifying agent sodium laurylsulfonate is 2.9%, and the mass percentage concentration of initiator potassium persulfate is 0.03%; Above-mentioned seed solution is heated to 80 ℃, begins to drip the above-mentioned emulsion system then, rate of addition is 0.1ml/ minute, and dropping is incubated 6 hours after finishing.Reaction finishes, and with ethanol/water centrifuge washing product, obtains Janus particle provided by the invention.
Characterize this embodiment with sem (SEM) and transmission electron microscope (TEM) and prepare gained Janus particulate structure, as shown in Figure 2.Can know that by Fig. 2 this embodiment prepares gained Janus particle and has snowman's shape structure, and two portions have various structure and size.
The Janus particle of embodiment 4, preparation modification
With 1g embodiment 1 preparation gained Janus particles dispersed in the 100g mass percentage concentration is 5% sodium hydroxide (NaOH) aqueous solution; Heat up then; Back flow reaction 24h; Using mass percentage concentration then is that 10% hydrochloric acid (HCl) transfers to neutrality with reaction system, with ethanol/water centrifuge washing product, obtains the Janus particle after the modification provided by the invention.
Characterize product structure with sem (SEM) and transmission electron microscope (TEM), characterize product with Fourier infrared spectrum (FTIR) and form, as shown in Figure 3,2240cm
-1The peak at place refers to itrile group; 1240cm
-1And 1157cm
-1The peak refer to carboxyl.
The Janus particles dispersed that this embodiment is prepared gained 0.002g modification adds 5g toluene then in 5g water, ultrasonic emulsification obtains emulsion.With opticmicroscope this emulsion is characterized, can be known by Fig. 4, this emulsion is a homogenous emulsion.
Embodiment 5, preparation Fe
3O
4Particle compound Janus particle
With the Janus particles dispersed after the 1g embodiment 4 preparation gained modifications is the Fe of the chitosan protection of 0.1wt% in 10g concentration
3O
4In the particle dispersion (diameter is 4nm), room temperature was adsorbed 5 hours down for 25 ℃, and centrifugal cleaning obtains Fe provided by the invention
3O
4Particle compound Janus particle.
This Janus particle is characterized product with SEM and TEM, can know that this product structure is correct.Can know Fe like Fig. 5
3O
4Particle is adsorbed on Janus particulate seed ball portion basically.
This embodiment of 0.002g is prepared gained Fe
3O
4Particle compound Janus particles dispersed adds 5g toluene then in 5g water, ultrasonic emulsification obtains emulsion.With opticmicroscope this emulsion is characterized, the gained result is as shown in Figure 5.Can know that by Fig. 5 this emulsion is a homogenous emulsion.
Embodiment 6, preparation Pt particle compound Janus particle
Is in the Pt particle dispersion of chitosan protection of 0.1wt% (diameter is 2nm) with the Janus particles dispersed after the modifications of 1g embodiment 4 preparation gained in 10g concentration; Room temperature was adsorbed 5 hours down for 25 ℃; Centrifugal cleaning obtains Pt particle compound Janus particle provided by the invention.
With SEM and TEM product is characterized, gained result and Fig. 5 do not have substantive difference, no longer endure here and state.Can know that by The above results this product structure is correct, be Pt particle compound Janus particle.
Embodiment 7, preparation Au particle compound Janus particle
Is in the Au particle dispersion of chitosan protection of 0.1wt% (diameter is 8nm) with the Janus particles dispersed after the modifications of 1g embodiment 4 preparation gained in 10g concentration; Room temperature was adsorbed 5 hours down for 25 ℃; Centrifugal cleaning obtains Au particle compound Janus particle provided by the invention.
With SEM and TEM product is characterized, gained result and Fig. 5 do not have substantive difference, no longer endure here and state.Can know that by The above results this product structure is correct, be Au particle compound Janus particle.
The Janus particle of embodiment 8, preparation Pd metal composite
To 10g Palladous chloride (concentration 1wt%), room temperature was soaked 10 hours for 25 ℃ with the Janus particles dispersed after the modifications of 1g embodiment 4 preparation gained, the palladium salt that do not adsorb of the centrifugal flush away of water then, and cleaning the back redispersion is the Hydrazine Hydrate 80 N of 5wt% in 8g concentration
2H
4In the aqueous solution, room temperature was reacted 8 hours down for 25 ℃, and after reaction finished, centrifugal cleaning obtained the Janus particle of Pd metal composite provided by the invention.
With SEM and TEM product is characterized, gained result and Fig. 5 do not have substantive difference, no longer endure here and state.Can know that by The above results this product structure is correct, be the Janus particle of Pd metal composite.
The Janus particle of embodiment 9, preparation Ag metal composite
To 10g Silver monochloride (concentration 10wt%), room temperature was soaked 10 hours for 25 ℃ with the Janus particles dispersed after the modifications of 1g embodiment 4 preparation gained, and 10% Hydrazine Hydrate 80 N cleaned the back redispersion and in the 20g mass percentage concentration be by the silver salt that do not adsorb of the centrifugal flush away of water then
2H
4In the aqueous solution, room temperature was reacted 2 hours down for 25 ℃, and after reaction finished, centrifugal cleaning obtained the Janus particle of Ag metal composite provided by the invention.
With SEM and TEM product is characterized, gained result and Fig. 5 do not have substantive difference, no longer endure here and state.Can know that by The above results this product structure is correct, be the Janus particle of Ag metal composite.
Embodiment 10, preparation SiO
2Compound Janus particle
With the Janus particles dispersed after the modifications of 1g embodiment 4 preparation gained by 1g tetraethoxy Si (OCH
2CH
3)
4In the inorganics precursor solution of forming with the 5g absolute ethyl alcohol, and to use mass percentage concentration be that 25% ammoniacal liquor is regulated its pH value to 9,25 ℃ of following whip attachment of room temperature 10 hours; The tetraethoxy that does not adsorb with the centrifugal flush away of absolute ethyl alcohol then, after cleaning with particles dispersed in 10g ethanol, add 1g water again; Room temperature hydrolysis 5 hours, after hydrolysis reaction finished, water is centrifugal to be cleaned; Lyophilize gets pressed powder, is SiO provided by the invention
2Compound Janus particle.
With SEM and TEM above-mentioned product is characterized, the gained result is as shown in Figure 6.Can know that by Fig. 6 this product structure is correct, SiO
2Basically be compounded in Janus particulate seed ball portion.
Embodiment 11, preparation TiO
2Compound Janus particle
In by 1g tetrabutyl titanate and 5g absolute ethyl alcohol, and to use mass percentage concentration be its pH value to 9 of ammoniacal liquor adjusting of 25%, 25 ℃ of following whip attachment of room temperature 10 hours with the Janus particles dispersed after the modifications of 1g embodiment 3 preparation gained; The tetrabutyl titanate that does not adsorb with the centrifugal flush away of absolute ethyl alcohol then, after cleaning with particles dispersed in 10g ethanol, add 1g water again; Room temperature hydrolysis 5 hours, after hydrolysis reaction finished, water is centrifugal to be cleaned; Lyophilize gets pressed powder, obtains TiO provided by the invention
2Compound Janus particle.
With SEM and TEM above-mentioned product is characterized, gained result and Fig. 6 do not have substantive difference, no longer endure here and state.Can know that by The above results this product structure is correct, TiO
2Basically be compounded in Janus particulate seed ball portion.
Embodiment 12, preparation SiO
2The SiO of partial function processing (hydrophobicity processing)
2Compound Janus particle
With 1g embodiment 10 preparation gained SiO
2Compound Janus particle places by 10g ethanol, 1g water and 0.05g silane coupling agent octadecyl Trimethoxy silane CH
3(CH
2)
17Si (OCH
3)
3In the mixing solutions of forming, the unreacted silane coupling agent of the centrifugal flush away of ethanol is used in the following 25 ℃ of reactions of air tight condition 10 hours then, obtains the SiO that hydrophobicity provided by the invention is handled
2Compound Janus particle.
With SEM and TEM above-mentioned product is characterized, gained result and Fig. 6 do not have substantive difference, no longer endure here and state.Can know that by The above results this product structure is correct, be the SiO of hydrophobicity processing
2Compound Janus particle.
The SiO of embodiment 13, preparation polymer moieties functionalization (wetting ability processing)
2Compound Janus particle
With gained SiO among the 1g embodiment 10
2Compound Janus particles dispersed in the 10g mass percentage concentration is 98% the vitriol oil, the following 40 ℃ of reactions of air tight condition 4 hours, the water centrifuge washing obtains the SiO that wetting ability provided by the invention is handled then
2Compound Janus particle.
With SEM and TEM above-mentioned product is characterized, gained result and Fig. 6 do not have substantive difference, no longer endure here and state.Can know that by The above results this product structure is correct, be the SiO of wetting ability processing
2Compound Janus particle.
Claims (21)
1. one kind prepares Janus particulate method, after comprising the steps: crosslinked polymeric colloid particles dispersed obtained seed solution in water, emulsion system is added drop-wise in the said seed solution reacts, and reaction finishes and obtains said Janus particle; Wherein, said emulsion system is obtained by monomer, linking agent, emulsifying agent, initiator and water mixing and emulsifying.
2. method according to claim 1; It is characterized in that: said crosslinked polymeric colloid particle is selected from least a in polyacrylonitrile and the polyacrylic ester, and degree of crosslinking is 10-80%, and preferred 50%; Said crosslinked polymeric colloid particulate diameter is 10nm-100 μ m; Preferred 400nm-1 μ m, said crosslinked polymeric colloid particle is hollow or solid polymeric colloid particle, in the said hollow crosslinked polymeric colloid particle; Shell thickness is 1nm-10um, preferred 100nm-1um;
Said monomer is selected from least a in the alkene that the total number of carbon atoms is 4-24, optimization styrene; Said linking agent is selected from least a in Vinylstyrene and the ethylene glycol dimethacrylate; Said initiator is selected from least a in Potassium Persulphate, ammonium persulphate, Sodium Persulfate and the hydrogen peroxide; Said emulsifying agent is selected from least a in sodium laurylsulfonate and the sodium lauryl sulphate.
3. method according to claim 1 and 2 is characterized in that: the mass percentage concentration of said seed solution is 0.1-30%, preferred 1-10%; The mass percentage concentration of said monomer in said emulsion system is 0.1-20%, preferred 1-10%; The mass percentage concentration of said linking agent in said emulsion system is 0.1-20%, preferred 1-10%; The mass percentage concentration of said emulsifying agent in said emulsion system is 0.01-5%, preferred 0.1-3%; The mass percentage concentration of said initiator in said emulsion system is 0.01-1%, preferred 0.01-0.1%; The weight of said emulsion system is 0.1-20 times of said seed solution weight, and preferred 10-20 doubly; In the said dropping step, rate of addition is 0.01-5ml/ minute, preferred 0.1-0.5ml/ minute; In the said reactions step, temperature is 60-90 ℃, and preferred 75-85 ℃, the time is 2-10 hour, preferred 6-8 hour.
The arbitrary said method preparation of claim 1-3 and the Janus particle.
5. one kind prepares modification Janus particulate method; Comprise the steps: the arbitrary said method preparation of claim 1-3 and the Janus particles dispersed in basic soln, carry out back flow reaction; Reaction finishes and with acidic solution reaction system is transferred to neutrality again, obtains the Janus particle of said modification.
6. method according to claim 5 is characterized in that: said basic soln is selected from least a in the aqueous solution of the aqueous solution and Pottasium Hydroxide of sodium hydroxide, and the mass percentage concentration of said basic soln is 0.05-20%, preferred 1-10%; Said acidic solution is selected from least a in hydrochloric acid and the acetic acid, and the mass percentage concentration of said acidic solution is 0.05-30%, preferred 1-10%; The arbitrary said method preparation of said claim 1-3 and the mass percentage concentration of Janus particle in reaction system be 0.1-60%, preferred 10-40%; In the said reactions step, the time is 1-24 hour, preferred 12-24 hour.
Claim 5 or the preparation of 6 said methods and the Janus particle of modification.
8. one kind prepares nano particle compound Janus particulate method, and the Janus particles dispersed of the said modification of claim 7 in water, is added the nanoparticles solution that has opposite charges and adsorbs, and obtains said nano particle compound Janus particle;
Wherein, the said nano particle that has opposite charges is selected from SiO
2, TiO
2, Au, Ag, Fe, Pd, Pt, FeO, Fe
3O
4, Fe
2O
3, Al
2O
3, SnO
2, Eu
2O
3, MnO
2, CaCO
3, in CoO, NiO, ZnO and the CdTe nano particle any one, preferred Au, Ag, Pd and Fe
3O
4In any one; The said particle diameter that has the nano particle of opposite charges is 1-50nm, preferred 2nm-10nm; The mass percentage concentration of the Janus particle of said modification in the system of being made up of the Janus particle and the water of said modification is 0.1-40%, preferred 10-20%; In the said adsorption step, temperature is 20-40 ℃, and preferred 20-30 ℃, the time is 1-24 hour, preferred 12-24 hour.
The preparation of the said method of claim 8 and nano particle compound Janus particle.
10. Janus particulate method for preparing metal composite; Comprise the steps: the Janus particle of the said modification of claim 7 is immersed in the aqueous solution of metal cation salt; The aqueous solution that adds reductive agent again after immersion finishes reacts, the Janus particle that reaction finishes and obtains said metal composite.
11. method according to claim 10 is characterized in that: in the aqueous solution of said metal cation salt, said metal cation salt is any one in the soluble salt of following metals ion: Au
3+, Ag
+, Pt
2+, Pd
2+, Fe
2+, Fe
3+, Zn
2+, Mn
2+, Co
2+, Ni
2+, Cu
2+And Mg
2+, any one in the preferred perchlorate of said metal cation salt, muriate, nitrate salt and the vitriol; Said reductive agent is selected from NaBH
4, LiB (C
2H
5)
3H and N
2H
4In any one; The mass percentage concentration of the aqueous solution of said metal cation salt is 0.01-60%, preferred 10-30%; The mass percentage concentration of said Janus particle in the aqueous solution of metal cation salt is 0.1-40%, preferred 10-30%; The mass percentage concentration of the aqueous solution of said reductive agent is 0.01-60%, preferred 20-40%; In the said soaking step, temperature is 25-90 ℃, and preferred 30-60 ℃, the time is 1-48 hour, preferred 12-24 hour; In the said reactions step, temperature is 10-90 ℃, and preferred 25-50 ℃, the time is 2-10 hour, preferred 6-8 hour.
12. the Janus particle of claim 10 or 11 preparation gained metal composite.
13. Janus particulate method for preparing inorganic compounding; Comprise the steps: the Janus particles dispersed of the said modification of claim 7 is adsorbed in the solution of inorganics precursor; After finishing, absorption, reacts the Janus particle that finishes and obtain said inorganic compounding with the reaction that in alcohol and water, is hydrolyzed of gained Janus particles dispersed.
14. method according to claim 13 is characterized in that: in the solution of said inorganics precursor, the inorganics precursor is selected from Si (OCH
3)
4, Si (OCH
2CH
3)
4, Si{OCH (CH
3)
2}
4, Si (OCH
2CH
2CH
2CH
3)
4, Na
2SiO
3, TiCl
4, Ti (OCH
3)
4, Ti (OCH
2CH
3)
4, Ti{OCH (CH
3)
2}
4, Ti (OCH
2CH
2CH
2CH
3)
4, TiOSO
4, SnCl
4, Sn (OCH
3)
4, Sn (OCH
2CH
3)
4, Sn{OCH (CH
3)
2}
4, Sn (OCH
2CH
2CH
2CH
3)
4, ZrCl
4, Zr (OCH
3)
4, Zr (OCH
2CH
3)
4, Zr{OCH (CH
3)
2}
4, Zr (OCH
2CH
2CH
2CH
3)
4, AlCl
3, Al (OCH
3)
4, Al (OCH
2CH
3)
4, Al{OCH (CH
3)
2}
4, Al (OCH
2CH
2CH
2CH
3)
4And Al
2(SO
4)
3In any one, preferred Si (OCH
3)
4And Ti (OCH
3)
4In any one, solvent is that the total number of carbon atoms is the monohydroxy-alcohol of 1-10, preferred alcohol; The mass percentage concentration of the solution of said inorganics precursor is 0.01-60%, preferred 20-50%; The mass percentage concentration of said Janus particle in the solution of said inorganics precursor is 0.1-40%, preferred 10-20%; In the said adsorption step, temperature is 25-90 ℃, and preferred 30-60 ℃, the time is 1-48 hour, preferred 12-24 hour; In the said hydrolysis reaction step, the pH value of solution is 1-13, preferred 8-10; In the said hydrolysis reaction step, the pH value of solution is that to use mass percentage concentration be that 35% hydrochloric acid or 25% ammoniacal liquor are regulated; In the said hydrolysis reaction step, temperature is 25-90 ℃, and preferred 30-60 ℃, the time is 1-48 hour, preferred 12-24 hour.
15. the Janus particle of claim 13 or 14 preparation gained inorganic compounding.
16. one kind prepares SiO
2The SiO of partial functionization
2Compound Janus particulate method, the Janus particles dispersed that comprises the steps: claim 13 or 14 is prepared the gained inorganic compounding is reacted behind adding silane coupling agent and the water in non-polar solvent, and reaction finishes and obtains said SiO
2The SiO of partial functionization
2Compound Janus particle.
17. method according to claim 16 is characterized in that: said silane coupling agent is the compound with following structure: C
nH
2n+1-Si (R
2)
3, C
nH
2n+1-SiCH
3(R
2)
2, R
3-C
mH
2mSi (R
2)
3,
R
3-C
mH
2mSiCH
3(R
2)
2、(C
2H
5O)
3-Si-(CH
2)
3-S-S-S-S-(CH
2)
3-Si-(OC
2H
5)
3、(C
2H
5O)
3-Si-(CH
2)
3-S-S-(CH
2)
3-Si-(OC
2H
5)
3；
Wherein, n is the integer of 1-121, the integer of preferred 5-50, and m is the integer of 0-126, the integer of preferred 5-50;
R
2Be Cl, OCH
3, OCH
2CH
3Or OC
2H
4OCH
3
R
3Be NH
2, CH
2=CH, HS, SCN, NHCONH
2, phenyl, epoxy group(ing), Cl, NH
2(CH
2)
2NH,
The preferred octadecyl Trimethoxy silane of said silane coupling agent; Said non-polar solvent is selected from least a in monohydroxy-alcohol that the total number of carbon atoms is 1-10 and the vinyl acetic monomer, preferred alcohol; Said silane coupling agent accounts for the 1-10% of the Janus particle weight of claim 13 or 14 preparation gained inorganic compounding; The mass percent concentration of Janus particle in said non-polar solvent of said claim 13 or 14 preparation gained inorganic compounding is 0.1-40%; The mass percentage concentration of said water is 0.1-40%, preferred 1-20%; In the said reactions step, temperature is 25-40 ℃, and preferred 25-30 ℃, the time is 5-24 hour, preferred 12-24 hour.
18. claim 16 or 17 preparation gained SiO
2The SiO of partial functionization
2Compound Janus particle.
19. SiO who prepares the polymer moieties functionalization
2Compound Janus particulate method comprises the steps: in the following Janus particle any one be dispersed in the acid solution and reacts, and reaction finishes and obtains the SiO of said polymer moieties functionalization
2Compound Janus particle: the Janus particle of claim 13 or 14 preparation gained inorganic compounding or claim 16 or 17 preparation gained SiO
2The SiO of partial functionization
2Compound Janus particle.
20. method according to claim 19 is characterized in that: said acid solution is selected from least a in sulfuric acid, hydrochloric acid and the nitric acid; The mass percentage concentration of said Janus particle in said acid solution is 0.1-40%, preferred 10-30%; The mass percentage concentration of said acid solution is 1-100%, preferred 35-100%; In the said reactions step, temperature is 25-90 ℃, and preferred 25-40 ℃, the time is 1-48 hour, preferred 12-24 hour.
21. the SiO of claim 19 or 20 preparation resulting polymers partial functionizations
2Compound Janus particle.
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| CN2011100564778A CN102675547A (en) | 2011-03-09 | 2011-03-09 | Janus particle with double properties and preparation method thereof |
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