CN103920297B - A kind of nanoparticle concentration method based on the evaporation of concussion auxiliary heating - Google Patents
A kind of nanoparticle concentration method based on the evaporation of concussion auxiliary heating Download PDFInfo
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Abstract
The present invention relates to a kind of nanoparticle concentration method based on the evaporation of concussion auxiliary heating, nano particle is also disperseed in a solvent, obtain the dispersion soln of nano particle, then the evaporation of concussion auxiliary heating is utilized to concentrate nanoparticles solution: the nanoparticles solution of dilution is carried out Synchronous Heating and concussion, by controlling the temperature of heating, the concentrated speed of speed and heat time adjustment nanoparticles solution, while heating and concussion, the device that fan etc. can be utilized to increase convection current blows operation, increase evaporation and the evaporation rate of solvent, the thickening efficiency of further raising nano particle.Compared with prior art, the advantages such as it is simple that the present invention has equipment, and thickening efficiency is high, and nano material loss is little, and the nanoparticulate dispersed after concentrated is good.
Description
Technical field
The invention belongs to nano material preparation and fabrication technical field, especially a kind of nanoparticle concentration method based on the evaporation of concussion auxiliary heating is related to, cross and utilize the method for concussion auxiliary heating under the size not changing nano particle in original solution and dispersity condition, reach nanoparticles solution efficient concentration, and reduce nano material and consume in process and lose.
Background technology
Nano material is because its size is little, and the large and quantum size effect of specific area, they have the property that conventional material does not possess, and have important value in development of new electronic material, structural material, optical material, chemical industry, pottery and medical material field.Such as, by adding the nano particle of good dispersion in conventional polymer material, the mechanical property that can increase substantially material makes to show that coating is more wear-resisting, the refractive index of optical material can be changed and do not affect the high light transmittance of macromolecular material itself, conduction and the heat conductivility of macromolecular material can be increased, realize its application in new field.
In recent years, the synthesis and preparation technology of nano material, particularly wet chemical methods develops rapidly, greatly facilitates the interest that people study nanometer material science.In order to obtain the nano particle of size uniform, in the process of synthesis of nano particle, the concentration of usual reactant controls lower.The nano particle General Decentralized synthesized thus is in water or other organic solvents, but the content of nano particle is very low usually.Carrying out sequent surface modification to the nano particle of synthesis or add man-hour to it further as additive, need one nanoparticle concentration method fast and effectively.For effectively utilizing the Small-scale fading of nano material, desirable concentration technique should be able to improve the concentration of particles in solution rapidly, and to the original characteristic of nano particle particularly dispersity can not destroy.
In existing nanoparticle concentration technology, the method for general nanoparticle concentration has ultracentrifugal method, naturally places the method for precipitation and the method for heating evaporation.High speed centrifugation generally has the particle of activating agent more effective for large-size, surface.For undersized nano particle, the centrifugal force that centrifuge produces is not enough to it is precipitated.High speed centrifugation method has the shortcoming of high energy consumption and low-yield.Further, high speed centrifugation can destroy the distribution of nanoparticle surface activating agent, causes the nano particle after concentrating again not disperse.Naturally place effectively concentrated usually also only to the particle of large-size, surperficial non-activity agent of the precipitation method, and this process efficiency is also very low.The method of heating evaporation solvent has concentrated speed faster.But nano material, because the very large and high surface energy of its specific area, is easily separated out at solution and Air Interface in solvent volatilization process, and the film of formation nano-particles self assemble, causes significant losses and the waste of nano material.
Summary of the invention
Object of the present invention be exactly in order to overcome above-mentioned prior art exist defect and provide a kind of based on concussion auxiliary heating evaporation nanoparticle concentration method.
Object of the present invention can be achieved through the following technical solutions:
Based on a nanoparticle concentration method for concussion auxiliary heating evaporation, adopt following steps:
(1) preparation of nanoparticles solution: also disperseed in a solvent by nano particle, obtains the dispersion soln of nano particle;
(2) method of concussion auxiliary heating evaporation is utilized to concentrate nanoparticles solution: nanoparticles solution is carried out Synchronous Heating and concussion, by control heating-up temperature be 30-150 DEG C, heating rate 0.5-60 DEG C/min, heat time is 0.1-10h, regulate the concentrated speed of nanoparticles solution, blow operation simultaneously, increase evaporation and the evaporation rate of solvent, improve the thickening efficiency of nano particle further.
Wherein, the solvent that the selection gist nano particle of temperature disperses, generally slightly lower than the boiling point 20-30 degree Celsius of solvent.But, the too low then concentrated speed of temperature is too slow, the too high stability that can have influence on again nano particle of temperature, under high temperature, nano particle may fuse the performance changing itself, heating rate is too low, has influence on concentrated efficiency, the too high solution that may cause is instantaneous overheated, affect the stability of nano particle, the too short heat time can make the amount that concentrates inadequate, oversize, can dry up, regulate the concentrated speed of nanoparticles solution, blow operation simultaneously, increase evaporation and the evaporation rate of solvent, improve the thickening efficiency of nano particle further.
Described nano particle is less than or equal to 100 nanometers for some on three dimension scale or multiple directions size, comprises metallic, metal oxide, metal chalcogenide, nonmetal oxide or other nano materials,
Described metallic comprises gold, silver, copper or platinum; Described metal oxide comprises titanium dioxide, zirconium dioxide or iron oxide; Described metal chalcogenide comprises zinc sulphide; Described nonmetal oxide comprises silica; Other described nano materials comprise CNT, graphite or Graphene.
Described nano particle is obtained by solid phase method, liquid phase method, sol-gal process, the precipitation method, evaporation heat of solution solution, oxidation-reduction method, solvent-thermal method or vapor phase method synthesis technique.
The dispersion soln of described nano particle can also be that the nano particle synthesized is re-dispersed into the solution formed in solvent.
The dispersion soln weight concentration of described nano particle is 0.01%-60%, and the solvent of employing comprises water, ethanol, methyl alcohol, isopropyl alcohol, acetone, chloroform, oxolane, toluene, hexane or cyclohexane.
Described concussion is ultrasonic vibration, machinery concussion or magnetic agitation.
Described heating adopts resistance heated, oil bath or heating water bath, electromagnetic irradiation heating or produces heat by ultrasonic vibration.
Described blowing operation accelerates convection current by fan or fume hood thus accelerates solvent evaporation and volatilization.
The weight concentration of concentrated nanoparticles solution is 0.01%-60%.
Compared with prior art, the present invention, can the rate of volatilization of regulable control solvent by regulating the temperature of heating, programming rate and heat time, and then the concentrating degree of nano particle that regulation and control obtain.Acoustic pressure drastic change when the high frequency sound wave produced by ultrasonator is propagated in the solution produces a large amount of bubbles in the solution rapidly, and constantly fierce explosion, the nano particle in solution is made to be in lasting vibrating state, thus effectively prevent nano particle from separating out at solution and Air Interface, decrease nano material and lose in process and consume.Thus obtained concentrated nano particle can keep original dispersity.To a certain extent, concussion can improve the dispersiveness of nano particle further.The dispersiveness of good nano particle is the follow-up further processing of nano material and the basis finally realizing commercial Application.In the process, the device that fan etc. can also be utilized to increase convection current blows operation, increases evaporation and the evaporation rate of solvent, improves the thickening efficiency of nano particle further, and can regulate and control the temperature of concentrated solution, reduce the impact of heating-up temperature on nanoparticle size and performance.
(1) adopt the method for heating evaporation solvent to concentrate nano particle, equipment is simple, and efficiency is high.
(2) adopt the method for ultrasonic vibration, ensure that nano particle is in concussion state in the solution, effectively prevent the precipitation of nano particle, decrease the loss of nano material in concentrated engineering and consumption.
(3) ultrasonic vibration effectively prevent the reunion of nano material, makes the nano particle after concentrating maintain original dispersiveness, is conducive to follow-up further processing and the application of nano material.
(4) evaporation and evaporation rate by utilizing the means such as fan to accelerate solvent further, put forward highly enriched efficiency, thickening temperature regulated and controled to ensure to size and the performance of concentrated nano particle.
Accompanying drawing explanation
Fig. 1 is 50 nanogold particle transmission electron microscope photos;
Fig. 2 is the contrast optical photograph before and after 50 nanogold particles concentrate;
Fig. 3 is the ultraviolet-visible spectrum before and after 5 nanogold particles concentrate;
Fig. 4 is 10 nanogold particle transmission electron microscope photos;
Fig. 5 is 5 titanium dioxide nanoparticle transmission electron microscope photos.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
(1) preparation of gold nano grain
By recipe requirements, HAuCl4 solution is added in the deionized water of boiling, stir and add sodium citrate solution again after 1 minute, then Keep agitation just obtain after 20 minutes mass concentration be 0.01% particle diameter be the gold grain (as shown in Figure 1) of 50 nanometers.
(2) gold nano grain is concentrated
Be that the beaker of the 50 nanogold particle aqueous solution is placed in the ultrasonator with heating function by being equipped with 100 milliliters of particle diameters, arranging heating-up temperature is 60 degrees Celsius, and programming rate is 5 centigrade per minutes, heating ultrasonic vibration 30 minutes.While heating, with fan, beaker mouth is blown, until concentration process terminates.As schematically shown in Figure 2, gold nano grain is concentrated to 50 milliliters, and solution surface does not have gold grain to separate out.As shown in Figure 3, UV-Vis spectra shows that the absworption peak of concentrated rear solution strengthens, but the position of absworption peak does not change.This shows that the gold nano grain concentration concentrated obtains increase, and its dispersity does not change.
Embodiment 2
(1) preparation of gold nano grain
By recipe requirements, HAuCl4 solution is added in the deionized water of boiling, stir and add sodium citrate solution again after 1 minute, then Keep agitation just obtains particle diameter after 10 minutes to be 10 nanometer mass concentrations be 0.04% gold grain solution (as shown in Figure 4).
(2) gold nano grain is concentrated
Be placed in the ultrasonator with heating function by the beaker that the 100 milliliter of 10 nanogold particle aqueous solution is housed, arranging heating-up temperature is 70 degrees Celsius, and programming rate is 2 centigrade per minutes, heating ultrasonic vibration 40 minutes.While heating, with fan, beaker mouth is blown, until concentration process terminates, obtain concentrated gold nano grain solution.
Embodiment 3
(1) preparation of titania nanoparticles
To in 45 milliliters of stainless steel hydrothermal reaction kettles, add 20 milliliters of cyclohexanes successively, 10 milliliters of oleic acid, 10 milliliters of oleyl amines and 1 milliliter of butyl titanate, after sealed reactor, reactor is transferred in 200 DEG C of baking ovens and is incubated 24 hours.Synthesis diameter be 5 nanometers (as shown in Figure 5) titania nanoparticles through washing after, be again dispersed in toluene solvant, obtain mass concentration be 2% titania nanoparticles solution.
(2) titania nanoparticles is concentrated
In fume hood, the beaker that 100 milliliters of above-mentioned titania solutions are housed is placed on warm table, arranging heating-up temperature is 40 degrees Celsius, carry out magnetic agitation (rotating speed is 600 rpms) 4 hours, obtain concentrated titania nanoparticles solution.
Embodiment 4
Based on a nanoparticle concentration method for concussion auxiliary heating evaporation, adopt following steps:
(1) preparation of nanoparticles solution: also disperseed in a solvent by nano particle, obtains the dispersion soln of nano particle;
(2) method of concussion auxiliary heating evaporation is utilized to concentrate nanoparticles solution: nanoparticles solution is carried out synchronous resistance heated and ultrasonic vibration, by control heating-up temperature be 30 DEG C, heating rate 0.5 DEG C/min, heat time is 10h, regulate the concentrated speed of nanoparticles solution, blow operation simultaneously, accelerate convection current by fan or fume hood thus accelerate solvent evaporation and volatilization, increase evaporation and the evaporation rate of solvent, the thickening efficiency of further raising nano particle, the weight concentration of the concentrated nanoparticles solution obtained is 0.01%.
Wherein, the solvent that the selection gist nano particle of temperature disperses, generally slightly lower than the boiling point 20-30 degree Celsius of solvent.But, the too low then concentrated speed of temperature is too slow, the too high stability that can have influence on again nano particle of temperature, under high temperature, nano particle may fuse the performance changing itself, heating rate is too low, has influence on concentrated efficiency, the too high solution that may cause is instantaneous overheated, affect the stability of nano particle, the too short heat time can make the amount that concentrates inadequate, oversize, can dry up, regulate the concentrated speed of nanoparticles solution, blow operation simultaneously, increase evaporation and the evaporation rate of solvent, improve the thickening efficiency of nano particle further.
Nano particle is some on three dimension scale or multiple directions size is less than or equal to 100 nanometers, comprise metallic, metal oxide, metal chalcogenide, nonmetal oxide or other nano materials, be titania nanoparticles in the present embodiment, obtained by solid phase method.The dispersion soln weight concentration of nano particle is 0.01%, adopts ethanol as solvent.
Embodiment 5
Based on a nanoparticle concentration method for concussion auxiliary heating evaporation, adopt following steps:
(1) preparation of nanoparticles solution: also disperseed in a solvent by nano particle, obtains the dispersion soln of nano particle;
(2) method of concussion auxiliary heating evaporation is utilized to concentrate nanoparticles solution: nanoparticles solution is carried out synchronous resistance heated and ultrasonic vibration, by control heating-up temperature be 60 DEG C, heating rate 5 DEG C/min, heat time is 8h, regulate the concentrated speed of nanoparticles solution, blow operation simultaneously, accelerate convection current by fan or fume hood thus accelerate solvent evaporation and volatilization, increase evaporation and the evaporation rate of solvent, the thickening efficiency of further raising nano particle, the weight concentration of the concentrated nanoparticles solution obtained is 10%.
Wherein, the solvent that the selection gist nano particle of temperature disperses, generally slightly lower than the boiling point 20-30 degree Celsius of solvent.But, the too low then concentrated speed of temperature is too slow, the too high stability that can have influence on again nano particle of temperature, under high temperature, nano particle may fuse the performance changing itself, heating rate is too low, has influence on concentrated efficiency, the too high solution that may cause is instantaneous overheated, affect the stability of nano particle, the too short heat time can make the amount that concentrates inadequate, oversize, can dry up, regulate the concentrated speed of nanoparticles solution, blow operation simultaneously, increase evaporation and the evaporation rate of solvent, improve the thickening efficiency of nano particle further.
Nano particle is some on three dimension scale or multiple directions size is less than or equal to 100 nanometers, comprise metallic, metal oxide, metal chalcogenide, nonmetal oxide or other nano materials, be zine sulfide nano particles in the present embodiment, obtained by liquid phase method.The dispersion soln weight concentration of nano particle is 10%, adopts chloroform as solvent.
Embodiment 6
Based on a nanoparticle concentration method for concussion auxiliary heating evaporation, adopt following steps:
(1) preparation of nanoparticles solution: also disperseed in a solvent by nano particle, obtains the dispersion soln of nano particle;
(2) method of concussion auxiliary heating evaporation is utilized to concentrate nanoparticles solution: nanoparticles solution is carried out synchronous resistance heated and ultrasonic vibration, by control heating-up temperature be 100 DEG C, heating rate 40 DEG C/min, heat time is 2h, regulate the concentrated speed of nanoparticles solution, blow operation simultaneously, accelerate convection current by fan or fume hood thus accelerate solvent evaporation and volatilization, increase evaporation and the evaporation rate of solvent, the thickening efficiency of further raising nano particle, the weight concentration of the concentrated nanoparticles solution obtained is 30%.
Wherein, the solvent that the selection gist nano particle of temperature disperses, generally slightly lower than the boiling point 20-30 degree Celsius of solvent.But, the too low then concentrated speed of temperature is too slow, the too high stability that can have influence on again nano particle of temperature, under high temperature, nano particle may fuse the performance changing itself, heating rate is too low, has influence on concentrated efficiency, the too high solution that may cause is instantaneous overheated, affect the stability of nano particle, the too short heat time can make the amount that concentrates inadequate, oversize, can dry up, regulate the concentrated speed of nanoparticles solution, blow operation simultaneously, increase evaporation and the evaporation rate of solvent, improve the thickening efficiency of nano particle further.
Nano particle is some on three dimension scale or multiple directions size is less than or equal to 100 nanometers, comprise metallic, metal oxide, metal chalcogenide, nonmetal oxide or other nano materials, be CNT in the present embodiment, obtained by evaporation heat of solution solution.The dispersion soln weight concentration of nano particle is 30%, adopts oxolane as solvent.
Embodiment 7
Based on a nanoparticle concentration method for concussion auxiliary heating evaporation, adopt following steps:
(1) preparation of nanoparticles solution: also disperseed in a solvent by nano particle, obtains the dispersion soln of nano particle;
(2) method of concussion auxiliary heating evaporation is utilized to concentrate nanoparticles solution: nanoparticles solution is carried out synchronous resistance heated and ultrasonic vibration, by control heating-up temperature be 150 DEG C, heating rate 60 DEG C/min, heat time is 0.1h, regulate the concentrated speed of nanoparticles solution, blow operation simultaneously, accelerate convection current by fan or fume hood thus accelerate solvent evaporation and volatilization, increase evaporation and the evaporation rate of solvent, the thickening efficiency of further raising nano particle, the weight concentration of the concentrated nanoparticles solution obtained is 50%.
Wherein, the solvent that the selection gist nano particle of temperature disperses, generally slightly lower than the boiling point 20-30 degree Celsius of solvent.But, the too low then concentrated speed of temperature is too slow, the too high stability that can have influence on again nano particle of temperature, under high temperature, nano particle may fuse the performance changing itself, heating rate is too low, has influence on concentrated efficiency, the too high solution that may cause is instantaneous overheated, affect the stability of nano particle, the too short heat time can make the amount that concentrates inadequate, oversize, can dry up, regulate the concentrated speed of nanoparticles solution, blow operation simultaneously, increase evaporation and the evaporation rate of solvent, improve the thickening efficiency of nano particle further.
Nano particle is some on three dimension scale or multiple directions size is less than or equal to 100 nanometers, comprise metallic, metal oxide, metal chalcogenide, nonmetal oxide or other nano materials, be Graphene in the present embodiment, obtained by evaporation heat of solution solution.The dispersion soln weight concentration of nano particle is 50%, adopts oxolane as solvent.
Claims (6)
1. based on a nanoparticle concentration method for concussion auxiliary heating evaporation, it is characterized in that, the method adopts following steps:
(1) preparation of nanoparticles solution: by nanoparticulate dispersed in a solvent, obtains the dispersion soln of nano particle;
(2) method that ultrasonic vibration auxiliary heating evaporates is utilized to concentrate nanoparticles solution: nanoparticles solution is carried out Synchronous Heating and concussion, by control heating-up temperature be 30-150 DEG C, heating rate 0.5-60 DEG C/min, heat time is 0.1-10h, regulate the concentrated speed of nanoparticles solution, blow operation simultaneously, increase evaporation and the evaporation rate of solvent, improve the thickening efficiency of nano particle further;
Described nano particle is some on three dimension scale or multiple directions size is less than or equal to the metallic of 100 nanometers, metal oxide, metal chalcogenide, nonmetal oxide or other nano materials,
Described metallic is gold, silver, copper or platinum; Described metal oxide is titanium dioxide, zirconium dioxide or iron oxide; Described metal chalcogenide is zinc sulphide; Described nonmetal oxide is silica; Other described nano materials are CNT, graphite or Graphene.
2. a kind of nanoparticle concentration method based on the evaporation of concussion auxiliary heating according to claim 1, it is characterized in that, described nano particle is obtained by solid phase method, sol-gal process, the precipitation method, evaporation heat of solution solution, oxidation-reduction method, solvent-thermal method or vapor phase method synthesis technique.
3. a kind of nanoparticle concentration method based on the evaporation of concussion auxiliary heating according to claim 1, it is characterized in that, the dispersion soln weight concentration of described nano particle is 0.01%-60%, and the solvent of employing comprises water, ethanol, methyl alcohol, isopropyl alcohol, acetone, chloroform, oxolane, toluene, hexane or cyclohexane.
4. a kind of nanoparticle concentration method based on the evaporation of concussion auxiliary heating according to claim 1, is characterized in that, described heating adopts resistance heated, oil bath or heating water bath, electromagnetic irradiation heating or produces heat by ultrasonic vibration.
5. a kind of nanoparticle concentration method based on the evaporation of concussion auxiliary heating according to claim 1, is characterized in that, described blowing operation accelerates convection current by fan or fume hood thus accelerates solvent evaporation and volatilization.
6. a kind of nanoparticle concentration method based on the evaporation of concussion auxiliary heating according to claim 1, it is characterized in that, the weight concentration of concentrated nanoparticles solution is 0.01%-60%.
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Citations (5)
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|---|---|---|---|---|
| US4985118A (en) * | 1987-03-24 | 1991-01-15 | Konica Corporation | Method for treating photographic process waste liquor through concentration by evaporation |
| CN101712822A (en) * | 2008-10-06 | 2010-05-26 | 施乐公司 | Fluorescent solid ink made with fluorescent nanoparticles |
| CN101780340A (en) * | 2009-01-20 | 2010-07-21 | 仝小林 | Decoction concentrating device for decocting clinical Chinese medicaments |
| CN102245168A (en) * | 2008-12-15 | 2011-11-16 | 诺瓦提斯公司 | Nanoparticle compositions |
| CN102740895A (en) * | 2009-12-23 | 2012-10-17 | 伊利诺伊大学董事会 | Nanoconjugates and nanoconjugate formulations |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11197401A (en) * | 1998-01-07 | 1999-07-27 | Hiroshi Morizaki | Method for accelerating evaporation of liquid |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4985118A (en) * | 1987-03-24 | 1991-01-15 | Konica Corporation | Method for treating photographic process waste liquor through concentration by evaporation |
| CN101712822A (en) * | 2008-10-06 | 2010-05-26 | 施乐公司 | Fluorescent solid ink made with fluorescent nanoparticles |
| CN102245168A (en) * | 2008-12-15 | 2011-11-16 | 诺瓦提斯公司 | Nanoparticle compositions |
| CN101780340A (en) * | 2009-01-20 | 2010-07-21 | 仝小林 | Decoction concentrating device for decocting clinical Chinese medicaments |
| CN102740895A (en) * | 2009-12-23 | 2012-10-17 | 伊利诺伊大学董事会 | Nanoconjugates and nanoconjugate formulations |
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