CN103639423B - Pure aluminium silicate coated with silver nano core-shell particle and preparation method and purposes - Google Patents
Pure aluminium silicate coated with silver nano core-shell particle and preparation method and purposes Download PDFInfo
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Abstract
<b>pure aluminium silicate coated with silver nano core-shell particle and preparation method and purposes. Nanometer</b><b>ag</b><b>owing to particle diameter is little, specific surface energy height, surfactivity point is many and have very excellent sterilization effect. But general nanometer</b><b>ag</b><b>when being applied to antifouling, sterilization coating, it is an insoluble problem with the consistency of coating. The inventive method comprises: the method comprises three steps: the first step adopts the preparation nanometer of reduction of ethylene glycol method</b><b>ag</b><b>powder body, the 2nd step nanometer</b><b>ag</b><b>the surface treatment of powder body, the 3rd step utilizes</b><b>al2(SO4)3</b><b>with</b><b>na2SiO3</b><b>precipitin reaction nanometer</b><b>ag</b><b>surface coating one layer</b><b>al2(SiO3)3</b><b>, obtain pure aluminium silicate coated with silver nano core-shell particle. The present invention relates to the making method of a kind of pure aluminium silicate coated with silver nano core-shell particle, can be used as the green insulating paint additive of pure aluminium silicate, play the functions such as antifouling, sterilization.</b>
Description
Technical field:
The corresponding product the present invention relates to the preparation method of a kind of pure aluminium silicate coated with silver nano core-shell particle, preparing in this way, and the purposes of this product in aluminum silicate composite heat-insulating coating additive. Belong to paint additive technical field.
Background technology:
Along with the high speed development of China's economy and steadily improving of living standards of the people, the coating industry driven by real estate and construction industry obtains unprecedented development. Due to the raising of people's environmental consciousness and the enhancement of environmental protection ideas, the green environmental friendly coatings of ecotope and human health close friend is become the development trend of coating products. Especially, under some particular surroundingss such as hospital operating room, Meat processing workshop, antifouling, the anti-microbial property of coating be it is also proposed higher requirement.
Aluminum silicate composite heat-insulating coating take natural fiber as main raw material, add the inorganic single-component packing dry powder thermal insulation coatings of a kind of novel green that a certain amount of inorganic auxiliary material is made through Compound Machining, the feature of such coating is green harmless, stable flame-retardant, there is the performances such as excellent sound-absorbing, high temperature resistant, cold-resistant, corrosion-resistant, not burning, be meet country fire-fighting and environmental requirement heat insulating coating material for wall in safety coefficient the highest, over-all properties and the optimal thermal insulation coatings of workability. Unique shortcoming of such coating does not have antifouling, biocidal efficacies.
As a kind of important precious metal, there is extremely strong sterilizing ability, and there is nontoxic, broad spectrum antibacterial, germ-killing efficiency height, not easily produce resistance, the feature such as difficult gathering in human body. Nanometer Ag owing to particle diameter is little, the plurality of advantages such as specific surface area and surface energy height, surfactivity point be many, show more excellent sterilization effect.
But, when nanometer Ag sterilant is applied to pure aluminium silicate coating, the consistency of nanometer Ag and pure aluminium silicate is an insoluble problem. Therefore, develop a kind of paint additive antifouling, biocidal efficacies that has outstanding with pure aluminium silicate paint compatibility and have very important meaning.
Summary of the invention:
It is an object of the invention to provide the preparation method of a kind of pure aluminium silicate coated with silver nano core-shell particle.
Above-mentioned purpose is achieved through the following technical solutions:
A preparation method for pure aluminium silicate coated with silver nano core-shell particle, the method comprises three steps: the first step adopts reduction of ethylene glycol method to prepare nanometer Ag powder body, and the surface treatment of the 2nd step nanometer Ag powder body, the 3rd step utilizes Al
2
(SO
4
)
3
And Na
2
SiO
3
Precipitin reaction at nanometer Ag Surface coating one layer of Al
2
(SiO
3
)
3
, obtain pure aluminium silicate coated with silver nano core-shell particle.
The preparation method of described pure aluminium silicate coated with silver nano core-shell particle, the preparation of the nanometer Ag powder body described in the first step adds 15mL ethylene glycol in there-necked flask, stir and it is heated to 150 DEG C ~ 170 DEG C, condensing reflux 1 hour at this temperature, the AgNO that will prepare in advance
3
Ethylene glycol solution and polyvinylpyrrolidone PVP ethylene glycol solution drip in described there-necked flask with the speed of 0.1 ~ 0.3mL/min simultaneously and add, at 150 ~ 170 DEG C, continue stirring 30 ~ 60 minutes after dropwising, it is cooled to room temperature afterwards and forms the solution containing nanometer Ag powder body.
The preparation method of described pure aluminium silicate coated with silver nano core-shell particle, in the preparation of the nanometer Ag powder body described in the first step, the molecular-weight average of described polyvinylpyrrolidone PVP is 10000 ~ 50000; In the preparation of the nanometer Ag powder body described in the first step, described polyvinylpyrrolidone PVP and AgNO
3
The ratio of amount of substance be 1.0:1.0 ~ 4.5:1.0.
The preparation method of described pure aluminium silicate coated with silver nano core-shell particle, the surface treatment of the nanometer Ag powder body described in the 2nd step is that the solution containing nanometer Ag powder body described in the first step is carried out high rotating speed centrifugation, and repeatedly wash with acetone and ethanol and obtain nanometer Ag powder body, described nanometer Ag powder body is dissolved in ethanol by ultrasonic disperse, makes 3.75 �� 10
-2
The nanometer Ag ethanolic soln of mol/L, stand-by; The PVP ethanolic soln prepared in advance is dripped in the nanometer Ag ethanolic soln carrying out ultrasonic disperse with the speed of 0.5mL/min, ultrasonic disperse process 20 ~ 40 minutes is continued after dropwising, afterwards described nanometer Ag ethanolic soln is carried out centrifugation, obtain the nanometer Ag powder body through PVP process.
The preparation method of described pure aluminium silicate coated with silver nano core-shell particle, in the surface treatment of the nanometer Ag powder body described in the 2nd step, described PVP monomer is 0.5:1.0 ~ 3.0:1.0 with the ratio of the amount of substance of nanometer Ag powder body.
The preparation method of described pure aluminium silicate coated with silver nano core-shell particle, the preparation of the pure aluminium silicate coated with silver nano core-shell particle described in the 3rd step the nanometer Ag powder body through PVP process described in the 2nd step is dissolved in deionized water form the nanometer Ag powder body aqueous solution, ultrasonic disperse is also heated to 75 DEG C, the Al that will prepare in advance
2
(SO
4
)
3
The aqueous solution and Na
2
SiO
3
The aqueous solution drips into the nanometer Ag powder body aqueous solution with the speed of 0.1 ~ 0.3mL/min, continues supersound process 30 ~ 90 minutes at 75 DEG C after dropwising, and after system is cooled to room temperature, centrifugation obtains pure aluminium silicate coated with silver nano core-shell particle;
The preparation method of described pure aluminium silicate coated with silver nano core-shell particle, in the preparation of the pure aluminium silicate coated with silver nano core-shell particle described in the 3rd step, described Al
2
(SO
4
)
3
The aqueous solution and Na
2
SiO
3
The concentration ratio of the aqueous solution is 1.0:3.0; Described Al
2
(SO
4
)
3
It is 0.02:1.00 ~ 0.06:1.00 with the ratio of the amount of substance of nanometer Ag powder body.
A pure aluminium silicate coated with silver nano core-shell particle prepared by described method, core material is the nanometer Ag powder body adopting reduction of ethylene glycol method to prepare, and mean diameter is 200-300nm, and described core material outside is coated with Al
2
(SiO
3
)
3
Outer shell, described Al
2
(SiO
3
)
3
Outer shell utilizes Al
2
(SO
4
)
3
And Na
2
SiO
3
Precipitin reaction become at nanometer Ag Surface coating;Described pure aluminium silicate clad nano galactic nucleus shell structure mean diameter is 400nm.
Pure aluminium silicate coated with silver nano core-shell particle prepared by a kind of described method is used as pure aluminium silicate green insulation, antifouling, sterilization paint additive.
Useful effect:
1. the pure aluminium silicate coated with silver nano core-shell particle that prepared by the present invention, mixed in aluminum silicate composite heat-insulating green coating, effectively improving the smelly performance antifouling, antibacterial, anti-of coating, exploitation especially antifouling for green environmental friendly coatings, antibiotic paint provides a kind of new technology.
Pure aluminium silicate coated with silver nano core-shell particle prepared by the present invention, at Ag nano particles Surface coating one layer of pure aluminium silicate, drastically increases the consistency of broad-spectrum sterilization nanometer Ag in pure aluminium silicate coating so that it is disperse more even in pure aluminium silicate coating.
Pure aluminium silicate coated with silver nano core-shell particle prepared by the present invention, wherein prepared Ag nano particles size is little, for 200-300nm, described pure aluminium silicate clad nano Ag nucleocapsid structure mean diameter is 400nm, its specific surface area and surface energy height, surfactivity site is many, has given full play to the sterilizing ability that nanometer Ag is extremely strong.
Pure aluminium silicate coated with silver nano core-shell particle prepared by the present invention; its preparation method is simple, does not need High Temperature High Pressure hydrothermal treatment consists and inert atmosphere protection roasting, in addition in preparation process; the preparation process of nanometer Ag does not need to add any template, is applicable to suitability for industrialized production.
Accompanying drawing illustrates:
Accompanying drawing 1 is the photo of part nanometer Ag powder scanning electronic microscope (SEM) the first state of the present invention.
Accompanying drawing 2 is the photo of part nanometer Ag powder scanning electronic microscope (SEM) the 2nd kind of state of the present invention.
Accompanying drawing 3 is the photo of part nanometer Ag powder scanning electronic microscope (SEM) the third state of the present invention.
Accompanying drawing 4 is the photo of part nanometer Ag powder scanning electronic microscope (SEM) the 4th kind of state of the present invention.
Accompanying drawing 5 is the photo of part pure aluminium silicate coated with silver nano core-shell particle the first state of SEM of the present invention.
Accompanying drawing 6 is the photo of part pure aluminium silicate coated with silver nano core-shell particle SEM the 2nd kind of state of the present invention.
Accompanying drawing 7 is nanometer Ag and the pure aluminium silicate coated with silver nano core-shell particle XRD curve of the present invention.
In figure, A is the XRD curve of nanometer Ag, and B is the XRD curve of pure aluminium silicate coated with silver nano core-shell particle, and C is Al (SiO
3
)
3
XRD curve.
Embodiment:
Embodiment 1:
A preparation method for pure aluminium silicate coated with silver nano core-shell particle, the method comprises three steps: the first step adopts reduction of ethylene glycol method to prepare nanometer Ag powder body, and the surface treatment of the 2nd step nanometer Ag powder body, the 3rd step utilizes Al
2
(SO
4
)
3
And Na
2
SiO
3
Precipitin reaction at nanometer Ag Surface coating one layer of Al
2
(SiO
3
)
3
, obtain pure aluminium silicate coated with silver nano core-shell particle.
Embodiment 2:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1, the preparation of the nanometer Ag powder body described in the first step is added in 100mL there-necked flask by 15mL ethylene glycol, stirs and heats, condensing reflux, condensing reflux 1 hour at 150 DEG C; By 0.3822gAgNO
3
Add the AgNO making 0.25mol/L in 9mL ethylene glycol
3
Ethylene glycol solution, adds the PVP ethylene glycol solution making 0.25mol/L in 9mL ethylene glycol (with AgNO by the PVP that 0.2501g molecular-weight average is 10000
3
The ratio of amount of substance is 1.0:1.0); Drip in above-mentioned there-necked flask with the speed of 0.1mL/min simultaneously and add AgNO
3
Ethylene glycol solution and PVP ethylene glycol solution;Continue after dropwising to stir 30min at 150 DEG C, solution is cooled to room temperature; By the mixing solutions height rotating speed centrifugation containing nanometer Ag, and repeatedly wash with acetone and ethanol, obtain nanometer Ag powder body; Nanometer Ag powder body is all dissolved in 60mL ethanol, makes 3.75 �� 10
-2
Mol/L nanometer Ag ethanolic soln is stand-by.
Embodiment 3:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2, the surface treatment of the nanometer Ag powder body described in the 2nd step is that the nanometer Ag ethanolic soln 30mL obtained is added ultrasonic disperse in there-necked flask, measures PVP(and the AgNO that 0.0625g molecular-weight average is 10000
3
The ratio of amount of substance be 0.5:1.0) add in 10mL ethanolic soln and make 5.625 �� 10
-2
The PVP ethanolic soln of mol/L; PVP ethanolic soln is dripped just in the nanometer Ag ethanolic soln of ultrasonic disperse with the speed of 0.5mL/min; Continue ultrasonic disperse 20min after dropwising, solution is carried out centrifugation, obtain the nanometer Ag through PVP process.
In the surface treatment of the 2nd step nanometer Ag powder body, adopting 0.125g molecular-weight average to be the PVP of 10000, the ultrasonic disperse time is 30min; In the preparation of the 3rd step pure aluminium silicate coated with silver nano core-shell particle, solution rate of addition is 0.2mL/min, and the supersound process time is 60min.
Embodiment 4:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2 or 3, the preparation of the pure aluminium silicate coated with silver nano core-shell particle described in the 3rd step is dissolved in 30mL deionized water by the nanometer Ag processed through PVP, and ultrasonic disperse is also heated to 75 DEG C; Measuring the concentration prepared in advance is 2.25 �� 10
-3
The Al of mol/L
2
(SO
4
)
3
Aqueous solution 10mL(Al
2
(SO
4
)
3
It is 0.02:1.00 with the ratio of nanometer Ag amount of substance) it is 6.75 �� 10 with concentration
-3
The Na of mol/L
2
SiO
3
Aqueous solution 10mL; By above-mentioned Al
2
(SO
4
)
3
The aqueous solution and Na
2
SiO
3
The aqueous solution is added drop-wise in the nanometer Ag aqueous solution of ultrasonic disperse with the speed of 0.1mL/min simultaneously, continues supersound process 30min at 75 DEG C after dropwising, and after system is cooled to room temperature, centrifugation obtains pure aluminium silicate coated with silver nano core-shell particle.
Embodiment 5:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2 or 3 or 4, in the preparation of the first step nanometer Ag powder body, temperature of reaction is 160 DEG C, PVP monomer and AgNO
3
The ratio of amount of substance is 1.5:1.0, and solution rate of addition is 0.2mL/min, and the reaction times is 60 minutes; In the surface treatment of the 2nd step nanometer Ag powder body, the ultrasonic disperse time is 40 minutes; In the preparation of the 3rd step pure aluminium silicate coated with silver nano core-shell particle, solution rate of addition is 0.3mL/min, and the supersound process time is 90 minutes.
Embodiment 6:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2 or 3 or 4 or 5, in the surface treatment of the 2nd step nanometer Ag powder body, adopts 0.25g molecular-weight average to be the PVP of 10000, and the ultrasonic disperse time is 20 minutes; In the preparation of the 3rd step pure aluminium silicate coated with silver nano core-shell particle, Al
2
(SO
4
)
3
Being 0.04:1.00 with the ratio of nanometer Ag amount of substance, solution rate of addition is 0.1mL/min, and the supersound process time is 60 minutes.
Embodiment 7:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2 or 3 or 4 or 5 or 6, in the preparation of the first step nanometer Ag powder body, temperature of reaction is 170 DEG C, PVP monomer and AgNO
3
The ratio of amount of substance is 2.0:1.0, and solution rate of addition is 0.3mL/min, and the reaction times is 30 minutes;In the surface treatment of the 2nd step nanometer Ag powder body, adopting 0.125g molecular-weight average to be the PVP of 10000, the ultrasonic disperse time is 30 minutes; In the preparation of the 3rd step pure aluminium silicate coated with silver nano core-shell particle, Al
2
(SO
4
)
3
Being 0.04:1.00 with the ratio of nanometer Ag amount of substance, solution rate of addition is 0.2mL/min, and the supersound process time is 90 minutes.
Embodiment 8:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2 or 3 or 4 or 5 or 6 or 7, in the surface treatment of the 2nd step nanometer Ag powder body, adopts 0.25g molecular-weight average to be the PVP of 10000, and the ultrasonic disperse time is 40 minutes; In the preparation of the 3rd step pure aluminium silicate coated with silver nano core-shell particle, solution rate of addition is 0.3mL/min, and the supersound process time is 30 minutes.
Embodiment 9:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2 or 3 or 4 or 5 or 6 or 7 or 8, in the preparation of the first step nanometer Ag powder body, adopts molecular weight to be the PVP of 40000, PVP monomer and AgNO
3
The ratio of amount of substance is 2.5:1.0, and the reaction times is 60 minutes; In the surface treatment of the 2nd step nanometer Ag powder body, 0.1876g molecular-weight average is adopted to be the PVP of 40000; In the preparation of the 3rd step pure aluminium silicate coated with silver nano core-shell particle, Al
2
(SO
4
)
3
Being 0.06:1.00 with the ratio of nanometer Ag amount of substance, the supersound process time is 90 minutes.
Embodiment 10:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2 or 3 or 4 or 5 or 6 or 7 or 8 or 9, in the surface treatment of the 2nd step nanometer Ag powder body, adopts 0.1876g molecular-weight average to be the PVP of 40000, and the ultrasonic disperse time is 30 minutes; In the preparation of the 3rd step pure aluminium silicate coated with silver nano core-shell particle, solution rate of addition is 0.2mL/min, and the supersound process time is 30 minutes.
Embodiment 11:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2 or 3 or 4 or 5 or 6 or 7 or 8 or 9 or 10, in the preparation of the first step nanometer Ag powder body, adopts molecular weight to be the PVP of 40000, PVP monomer and AgNO
3
The ratio of amount of substance is 3.0:1.0, and temperature of reaction is 160 DEG C, and solution rate of addition is 0.2mL/min; In the surface treatment of the 2nd step nanometer Ag powder body, adopting 0.1876g molecular-weight average to be the PVP of 40000, the ultrasonic disperse time is 40 minutes; In the preparation of the 3rd step pure aluminium silicate coated with silver nano core-shell particle, Al
2
(SO
4
)
3
Being 0.06:1.00 with the ratio of nanometer Ag amount of substance, solution rate of addition is 0.3mL/min, and the supersound process time is 60 minutes.
Embodiment 12:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2 or 3 or 4 or 5 or 6 or 7 or 8 or 9 or 10 or 11, in the surface treatment of the 2nd step nanometer Ag powder body, adopting 0.0625g molecular-weight average to be the PVP of 40000, the ultrasonic disperse time is 20 minutes; In the preparation of the 3rd step pure aluminium silicate coated with silver nano core-shell particle, Al
2
(SO
4
)
3
Being 0.02:1.00 with the ratio of nanometer Ag amount of substance, solution rate of addition is 0.1mL/min, and the supersound process time is 30 minutes.
Embodiment 13:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2 or 3 or 4 or 5 or 6 or 7 or 8 or 9 or 10 or 11 or 12, in the preparation of the first step nanometer Ag powder body, adopts molecular weight to be the PVP of 40000, PVP monomer and AgNO
3
The ratio of amount of substance is 3.5:1.0, and temperature of reaction is 170 DEG C, and solution rate of addition is 0.3mL/min, and the reaction times is 60 minutes;In the surface treatment of the 2nd step nanometer Ag powder body, adopting 0.125g molecular-weight average to be the PVP of 40000, the ultrasonic disperse time is 30 minutes; In the preparation of the 3rd step pure aluminium silicate coated with silver nano core-shell particle, solution rate of addition is 0.2mL/min, and the supersound process time is 60 minutes.
Embodiment 14:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2 or 3 or 4 or 5 or 6 or 7 or 8 or 9 or 10 or 11 or 12 or 13, in the surface treatment of the 2nd step nanometer Ag powder body, adopting 0.25g molecular-weight average to be the PVP of 40000, the ultrasonic disperse time is 20 minutes; In the preparation of the 3rd step pure aluminium silicate coated with silver nano core-shell particle, Al
2
(SO
4
)
3
Being 0.04:1.00 with the ratio of nanometer Ag amount of substance, solution rate of addition is 0.1mL/min.
Embodiment 15:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2 or 3 or 4 or 5 or 6 or 7 or 8 or 9 or 10 or 11 or 12 or 13 or 14, in the preparation of the first step nanometer Ag powder body, adopts molecular weight to be the PVP of 50000, PVP monomer and AgNO
3
The ratio of amount of substance is 4.0:1.0; In the surface treatment of the 2nd step nanometer Ag powder body, adopting 0.125g molecular-weight average to be the PVP of 50000, the ultrasonic disperse time is 30 minutes; In the preparation of the 3rd step pure aluminium silicate coated with silver nano core-shell particle, Al
2
(SO
4
)
3
Being 0.04:1.00 with the ratio of nanometer Ag amount of substance, solution rate of addition is 0.2mL/min, and the supersound process time is 90 minutes.
Embodiment 16:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2 or 3 or 4 or 5 or 6 or 7 or 8 or 9 or 10 or 11 or 12 or 13 or 14 or 15, in the surface treatment of the 2nd step nanometer Ag powder body, adopting 0.25g molecular-weight average to be the PVP of 50000, the ultrasonic disperse time is 40 minutes; In the preparation of the 3rd step pure aluminium silicate coated with silver nano core-shell particle, solution rate of addition is 0.3mL/min, and the supersound process time is 30 minutes.
Embodiment 17:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2 or 3 or 4 or 5 or 6 or 7 or 8 or 9 or 10 or 11 or 12 or 13 or 14 or 15 or 16, in the preparation of the first step nanometer Ag powder body, temperature of reaction is 160 DEG C, adopts molecular weight to be the PVP of 50000, PVP monomer and AgNO
3
The ratio of amount of substance is 4.5:1.0, and solution rate of addition is 0.2mL/min, and the reaction times is 60 minutes; In the surface treatment of the 2nd step nanometer Ag powder body, 0.1876g molecular-weight average is adopted to be the PVP of 50000; In the preparation of the 3rd step pure aluminium silicate coated with silver nano core-shell particle, Al
2
(SO
4
)
3
Being 0.06:1.00 with the ratio of nanometer Ag amount of substance, the supersound process time is 90 minutes.
Embodiment 18:
The preparation method of the pure aluminium silicate coated with silver nano core-shell particle described in embodiment 1 or 2 or 3 or 4 or 5 or 6 or 7 or 8 or 9 or 10 or 11 or 12 or 13 or 14 or 15 or 16 or 17, in the surface treatment of the 2nd step nanometer Ag powder body, the ultrasonic disperse time is 30 minutes; In the preparation of the 3rd step pure aluminium silicate coated with silver nano core-shell particle, solution rate of addition is 0.2mL/min, and the supersound process time is 30 minutes.
Embodiment 18:
Adopt the analysis means such as XRD, SEM, the pure aluminium silicate coated with silver nano core-shell particle gone out is prepared by the above embodiments and carries out analysis and characterization: can find out that 2 �� angles of wherein four peak values are respectively 38.1 �� by the XRD curve of nanometer Ag, 44.3 ��, 64.5 ��, 77.4 ��,<111>,<200>,<220>of corresponding pure Ag powder body,<311>four crystal faces, show that prepared nanometer Ag is the elemental silver of centroid cubic crystal system, with the data consistent on JCPDS card 04-0783;Can finding out that nanometer Ag shape looks prepared at different conditions are different by the SEM photograph analysis of nanometer Ag, wherein cube block nanometer Ag median size is between 200-300nm, and rod-like nano Ag mean diameter is 300nm, and length is between 10 ��m ~ 15 ��m; By pure aluminium silicate coated with silver nanoparticle SEM photograph it may be seen that nanoparticle is typical nucleocapsid structure.
Claims (6)
1.A preparation method for pure aluminium silicate coated with silver nano core-shell particle, is characterized in that: the method comprises three steps: the first step, adopts reduction of ethylene glycol method to prepare nanometer Ag powder body, the 2nd step, the surface treatment of nanometer Ag powder body, and the 3rd step, utilizes Al 2 (SO 4 ) 3 And Na 2 SiO 3 Precipitin reaction at nanometer Ag Surface coating one layer of Al 2 (SiO 3 ) 3 , obtain pure aluminium silicate coated with silver nano core-shell particle;
The preparation of the nanometer Ag powder body described in the first step adds 15mL ethylene glycol in there-necked flask, stirs and is heated to 150 DEG C ~ 170 DEG C, condensing reflux 1 hour at this temperature, the AgNO that will prepare in advance
3
Ethylene glycol solution and polyvinylpyrrolidone PVP ethylene glycol solution drip in described there-necked flask with the speed of 0.1 ~ 0.3mL/min simultaneously and add, at 150 ~ 170 DEG C, continue stirring 30 ~ 60 minutes after dropwising, it is cooled to room temperature afterwards and forms the solution containing nanometer Ag powder body;
In the preparation of the nanometer Ag powder body described in the first step, described polyvinylpyrrolidone PVP and AgNO
3
The ratio of amount of substance be 1.0:1.0 ~ 4.5:1.0;
The preparation of the pure aluminium silicate coated with silver nano core-shell particle described in the 3rd step is that through the nanometer Ag powder body of PVP surface treatment, the 2nd step is dissolved in the deionized water formation nanometer Ag powder body aqueous solution, and ultrasonic disperse is also heated to 75 DEG C, the Al that will prepare in advance
2
(SO
4
)
3
The aqueous solution and Na
2
SiO
3
The aqueous solution drips into the nanometer Ag powder body aqueous solution with the speed of 0.1 ~ 0.3mL/min, continues supersound process 30 ~ 90 minutes at 75 DEG C after dropwising, and after system is cooled to room temperature, centrifugation obtains pure aluminium silicate coated with silver nano core-shell particle;
In the preparation of the pure aluminium silicate coated with silver nano core-shell particle described in the 3rd step, described Al
2
(SO
4
)
3
The aqueous solution and Na
2
SiO
3
The concentration ratio of the aqueous solution is 1.0:3.0; Described Al
2
(SO
4
)
3
It is 0.02:1.00 ~ 0.06:1.00 with the ratio of the amount of substance of nanometer Ag powder body.
2.The preparation method of pure aluminium silicate coated with silver nano core-shell particle according to claim 1, is characterized in that: in the preparation of the nanometer Ag powder body described in the first step, the molecular-weight average of described polyvinylpyrrolidone PVP is 10000 ~ 50000.
3.The preparation method of pure aluminium silicate coated with silver nano core-shell particle according to claim 1 and 2, it is characterized in that: the surface treatment of the nanometer Ag powder body described in the 2nd step is that the solution containing nanometer Ag powder body described in the first step is carried out high rotating speed centrifugation, and repeatedly wash with acetone and ethanol and obtain nanometer Ag powder body, described nanometer Ag powder body is dissolved in ethanol by ultrasonic disperse, makes 3.75 �� 10 -2 The nanometer Ag ethanolic soln of mol/L, stand-by; The PVP ethanolic soln prepared in advance is dripped in the nanometer Ag ethanolic soln carrying out ultrasonic disperse with the speed of 0.5mL/min, ultrasonic disperse process 20 ~ 40 minutes is continued after dropwising, afterwards described nanometer Ag ethanolic soln is carried out centrifugation, obtain the nanometer Ag powder body through PVP process.
4.The preparation method of pure aluminium silicate coated with silver nano core-shell particle according to claim 3, is characterized in that: in the surface treatment of the nanometer Ag powder body described in the 2nd step, and described PVP monomer is 0.5:1.0 ~ 3.0:1.0 with the ratio of the amount of substance of nanometer Ag powder body.
5.A pure aluminium silicate coated with silver nano core-shell particle prepared by the method described in one of claim 1-4, is characterized in that:
Core material is the nanometer Ag powder body adopting reduction of ethylene glycol method to prepare, and mean diameter is 200-300nm, and described core material outside is coated with Al
2
(SiO
3
)
3
Outer shell, described Al
2
(SiO
3
)
3
Outer shell utilizes Al
2
(SO
4
)
3
And Na
2
SiO
3
Precipitin reaction become at nanometer Ag Surface coating; Described pure aluminium silicate clad nano galactic nucleus shell structure mean diameter is 400nm.
6.A kind of pure aluminium silicate coated with silver nano core-shell particle according to claim 5 is used as the green insulation of pure aluminium silicate series, antifouling, sterilization paint additive.
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| CN110814332B (en) * | 2019-11-08 | 2022-07-12 | 惠州达祺光电科技有限公司 | Silver nanowire post-treatment method |
| CN111187421B (en) * | 2020-01-15 | 2022-02-22 | 浙江理工大学 | Nanoparticle/metal-organic framework material and preparation method and application thereof |
| CN111618312B (en) * | 2020-04-28 | 2022-11-08 | 哈尔滨理工大学 | Preparation method of rod-shaped Ag powder, preparation method and application of rod-shaped Ag @ BST core-shell particles |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1470574A (en) * | 2003-06-16 | 2004-01-28 | 上海维来新材料科技有限公司 | Antibacterial negative ion coating |
| CN102391730A (en) * | 2011-10-17 | 2012-03-28 | 中国烟草中南农业试验站 | Nano functional coating |
| CN102548901A (en) * | 2009-09-22 | 2012-07-04 | 普瑞伯纳公司 | Biocidal colloidal dispersions of silica particles with silver ions adsorbed thereon |
| CN102985097A (en) * | 2010-04-16 | 2013-03-20 | 西班牙高等科研理事会 | Composition comprising aluminum silicates and silver nanoparticles as bactericides |
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| CN1470574A (en) * | 2003-06-16 | 2004-01-28 | 上海维来新材料科技有限公司 | Antibacterial negative ion coating |
| CN102548901A (en) * | 2009-09-22 | 2012-07-04 | 普瑞伯纳公司 | Biocidal colloidal dispersions of silica particles with silver ions adsorbed thereon |
| CN102985097A (en) * | 2010-04-16 | 2013-03-20 | 西班牙高等科研理事会 | Composition comprising aluminum silicates and silver nanoparticles as bactericides |
| CN102391730A (en) * | 2011-10-17 | 2012-03-28 | 中国烟草中南农业试验站 | Nano functional coating |
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