CN100469427C - A continuous industrialized nano material dispersion device and method - Google Patents
A continuous industrialized nano material dispersion device and method Download PDFInfo
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- CN100469427C CN100469427C CNB2006101654107A CN200610165410A CN100469427C CN 100469427 C CN100469427 C CN 100469427C CN B2006101654107 A CNB2006101654107 A CN B2006101654107A CN 200610165410 A CN200610165410 A CN 200610165410A CN 100469427 C CN100469427 C CN 100469427C
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Abstract
The invention relates to a continuous industry nanometer separator and relative method, wherein said device comprises high-level premixing groove (1), high-level premixing groove, premixing liquid groove (4), throttle valve (3), tube pressurize pump (5), tube power ultrasonic processor (6), nanometer slurry output tube (7), sensor (8), output flux control valve (9), reflux control valve (10), reflux tube (11), nanometer slurry storage pot (12), and nanometer slurry packing device (13). The invention had the advantages that: it has high efficiency, it can reduce the additive consumption, it can avoid pollution, and it can continuously produce, with wide application.
Description
Technical field
The invention belongs to technical field of nano material, particularly relate to a kind of continuous industrialized nano powder dispersal device and method, disclose more precisely a kind of continuously, mass ground makes nano material the technology of the nanometer slurries of dispersion, and the equipment of realizing this process, belong to the nanometer technology application.
Background technology
Nano material is little owing to particle diameter, and specific area is big, the free energy height, and therefore generally speaking, nano material all exists with aggregating state.The nano material particle diameter of aggregating state is tens of a nano particle diameter, even hundreds of times, therefore can not embody the nanoscale effect well.In addition, nano material generally is used for the matrix material modification, therefore nano material need be added in the matrix material, thus the purpose of realization modification, still, if nano material directly adds in the matrix material without crossing dispersion, because nano material is in aggregating state, therefore is difficult in the matrix material and disperses so, improved the cost that disperses, increased the consumption of nano material, and the nano modification effect can not embody well.Therefore, need a kind of can effectively nano material the dispersion, make the method and apparatus that stabilized nano is disperseed slurries, for effective application of nano material provides condition.Can realize that the method that nano material is disperseed mainly contains mechanical agitation, high energy milling, chemical dispersion and ultrasonic wave dispersion etc.The dispersion process of existing employing said method is generally discontinuous, and can not realize continuous processing quantitatively.
Chinese patent application 200510112112.7 discloses a kind of nanometer bismuth titanate aqueous casting slurry and preparation method.This method is with the solid bismuth titanate powder of particle diameter less than 180 nanometers, adds in proportion in deionized water and the dispersant, grinds in the multi-directional ball grinding machine then, and milling time 15～24 hours obtains dispersed paste.Obviously, this method jitter time is long, is discontinuous dispersion, and also can follow abrasive media to enter in the slurries in grinding, and pollutes slurries.
Chinese patent application 200410077290.6 discloses a kind of particle dispersing method and equipment thereof.The equipment of this method comprises: a container, and it is with an agitating device; The conduit of a belt switch element is arranged at the container bottom, by conduit and switch element suspension is imported in the ultrasonator, after 3～10 minutes concussion, promptly obtains described particle dispersion.This is a method and apparatus discontinuous, that ultrasonic wave is in a small amount handled the dispersing nanometer material obviously.In addition, because the ultrasonator that this method adopts is a container type, because of the restriction of prior art, its power density is less, therefore need carry out the processing of long period.Obviously, this method and apparatus can not satisfy the needs that nano-dispersed is carried out in serialization, industrial mass.
Chinese patent application 01131537.7 discloses a kind of dispersing technology of Nano diamond, it is characterized in that Nano diamond is mixed by certain weight ratio with lubricating oil, add in the rearmounted excess of imports sonic disintegrator of dispersant, carry out the ultrasonic wave grinding dispersion treatment, 4～20 minutes processing times.Obviously, this technology is to carry out at small-sized, a discontinuous ultrasonic unit, can not satisfy the needs that nano-dispersed is carried out in serialization, industrial mass equally.
Chinese patent application 200610016672.7 discloses a kind of water repelling soliquoid of nano TiO 2 and preparation method thereof.The feature of this method is the surface that sodium metnylene bis-naphthalene sulfonate is adsorbed on nano titanium oxide as efficient wetting agent, an energy barrier is made on surface at TiO 2 particles, overcome the Van der Waals force between nano particle, again by high shear dispersion machine dispersed with stirring 30 minutes, obtain nano suspending liquid, the suspension nano-solid content that this method makes is lower, has only 2～3%.
Chinese patent application 01101802.X discloses a kind of nanometer optical catalyst mother solution and its production and use.The characteristics of this patent are to need to add a high proportion of additive, secondly are that preparation process need add stir process through grinding to add the ultrasonic wave processing or grind.By grinding what all directly bring is that milling time is long, the problem of grinding-material pollution nanometer mother liquor.In addition, add auxiliary dispersants and stabilizing agent in high proportion, additive might influence the use of product.
Nano-dispersed method and equipment that these are known, can't realize that serialization, industrially scalable prepare the nanometer slurries in a large number, can't effectively reduce the amount of the interpolation compound of aid dispersion and stabilized nanoscale slurries, and avoid the pollution of abrasive media the nanometer slurries.
Summary of the invention
The object of the present invention is to provide a kind of continuous industrialized nano powder dispersal device and method, solution equipment and process realize the high-dispersion nano slurries of continuous industry production all kinds and various concentration to the pollution problem of nanometer liquid.
In device of the present invention, comprise: the high-order premixed groove 1 of belt stirrer, the premix storage tank of belt stirrer 4 and with premixed groove joint slurries conveyance conduit 2 and choke valve 3, pipe pressurizing pump 5, tubular type power ultrasonic processor 6, nanometer slurries efferent duct 7 and be installed in detecting line sensor 8, output flow control valve 9 and return flow control valve 10 and reflux line 11 on the pipeline, nanometer serum storage tank 12, nanometer slurries pot-type equipment 13.High-order premix groove is vertical groove, and preferred vertical drum shape groove helps mixing, and the cell body material is stainless steel or enamel material, and paddle is installed in the groove, and the bottom of groove has and the joining pipeline of premixed liquid storage tank, and choke valve is arranged on the pipeline.The stirring arm axle is in the bottom of cell body.Select for use drum shape groove can realize sufficient stirring and evenly mixing, avoided the deposition dead angle.The premix storage tank is vertical groove, preferred vertical drum shape groove, the cell body material is stainless steel or enamel material, paddle is installed in the groove, the stirring arm axle is in the bottom of cell body, and the volume of premix storage tank is 1～4 times that aforesaid high-order premix cell body amasss, and assurance premix slurries are carried in processor for ultrasonic wave and do not interrupted, the bottom of groove has and the joining pipeline of tubular ultrasonic ripple processor, and booster pump is arranged on the pipeline.It is such carrying the mode of premixed liquid continuously to tubular ultrasonic ripple processor, the nanometer premixed liquid that need are handled is carried to tubular ultrasonic ripple processor continuously by the pipe pressurizing pump, regulate nanometer slurries processing speed by control booster pump and adjusting output flow control valve and return flow control valve, improve the pressure of nanometer slurries in the tubular ultrasonic ripple processor simultaneously, improve the cavitation threshold values of slurries, be implemented in and carry out the ultrasonic wave processing under the higher unit are ultrasonic radiation intensity.Several modes of PZT (piezoelectric transducer) head independently of different with the conventional fixed installation on wall of this tubular ultrasonic ripple processor, but the center radiation tubular type high power transducer of one, tube wall is the spoke side of transducer, radiant tube is round tube or rectangular tube, pipe wall material is stainless steel or titanium alloy, preferred titanium alloy material, transducer is for forcing the direct-cooling type transducer, 2～16 watts/square centimeter of the sound power density scopes of transducer, preferred 4～12 watts/square centimeter, frequency range 10～40KHz, optimized frequency 18～24KHz.
On tubular type high-power ultrasonic processor efferent duct, optical pickocff and return duct and return valve are installed in apparatus of the present invention, can online detection nanometer slurries dispersion effect, by the control return valve, regulate capacity of returns and ultrasonic power and control processing speed and control nanometer slurries quality.
Method of the present invention comprises the steps:
1) nano powder, solvent medium, dispersant and stabilizing agent etc. are added in the premix groove 1 in the technological requirement ratio, carry out abundant stirring and evenly mixing, obtain premixed liquid;
2) open choke valve 3, above-mentioned premixed liquid is sent in the premix slurry tank 4 by pipeline 2, choke valve 3;
3) by pipe pressurizing pump 5 premixed liquid in the premix slurry tank 4 is sent in the tubular ultrasonic ripple processor 6;
4) the nanometer slurries after online detection is handled by tubular ultrasonic ripple processor 6, and adjust power and the return flow control valve 10 and the output flow control valve 9 of tubular type power ultrasonic processor according to testing result;
5) qualified nanometer slurries are sent in the nanometer slurry tank 12 by pipeline, and canned by pot-type equipment 13.
Adopt continuous industrialized nano process for dispersing of the present invention can handle nano materials such as metal nano powder, oxide nonmetallic powder, salt nano powder, CNT, but be not limited only to above-mentioned nano powder, described nano powder particle diameter 5～100 nanometers.In addition, also be suitable for method of the present invention for the bigger powder body material of particle diameter.
Solvent medium of the present invention is meant the solution of dissolved solid nano powder, and they can be water-based value, organic media, oiliness is worth or the mixture of these media.The stabilizing agent that adds in the premixed liquid, dispersant are a kind or their mixtures wherein such as low-molecular polypropylene acid ammonium, low-molecular polypropylene acid sodium, carboxymethyl cellulose, lignosulfonates, methylene dinaphthalene sulfonate, and coupling agent is a kind or their mixtures wherein such as silane, titanate esters, borate, aluminic acid ester.And the interpolation total amount of described dispersant, stabilizing agent and coupling agent is less than 0.1～20%, and preferable range is 0.4～8%, and the auxiliary compounds amount of interpolation is few more, and is also just more little to the influence of follow-up nanometer slurry applications.The dispersant, stabilizing agent and the coupling agent kind that are fit to nano-dispersed method of the present invention are not limited only to above-mentioned listed dispersant, stabilizing agent and coupling agent kind.
A key character of the inventive method is to realize continous way processing and pressurized treatment, in the tubular type transducer, carry the premixed liquid slurry continuously by booster pump, improve the pressure of slurries simultaneously, 1.5～10 kilograms/cm2 of pressure of slurries in the transducer, 2.5～3.5 kilograms/cm2 of preferred pressure.Can improve the cavitation threshold values of treatment fluid by improving pressure, thereby can effectively improve the ultrasonic wave radiosity that applies to treatment fluid, realize dispersing nanometer powder fast and effeciently.Process for dispersing of the present invention has designed the step of section processes nanometer slurry reflux, can stablize treatment effect, realizes the control to the nano powder dispersion effect, regulates capacity of returns by return valve, and reflux ratio is 5%～60%, and preferred 15%.
Continuous industrial nano-dispersed method and apparatus of the present invention not only limits the use of in nano-dispersed, also can be used for the extraction, mixing, catalytic reaction in fields such as medicine, chemical industry, metallurgy etc.The professional and technical personnel can realize other purposes, but not deviate from principle of the present invention and application by improving or select for use wherein partial devices and method.
The invention has the advantages that, can and equip more effective than known before nano-dispersed or nano suspending liquid or nanometer slurry preparation method, and can realize reducing the auxiliary consumption that adds compound, no equipment is to the pollution of nanometer liquid, high effects such as nano-solid content, and can realize the high-dispersion nano slurries of continuous industry production all kinds and various concentration.
Description of drawings
Fig. 1, be device schematic diagram of the present invention, wherein: high-order premixed groove 1, pipeline 2, choke valve 3, premix storage tank 4, pipe pressurizing pump 5, tubular type power ultrasonic processor 6, nanometer slurries efferent duct 7, detecting line sensor 8, output flow control valve 9, return flow control valve 10, reflux line 11, nanometer serum storage tank 12, nanometer slurries pot-type equipment 13
The specific embodiment
Embodiment 1
An example of the device of the present invention shown in the figure, wherein pipeline carries booster pump to select the low discharge plunger displacement pump for use, and metered flow is 10 cubic metres/hour, 50 meters of lifts.Ultrasonic transducer is circular tubular type ultrasonic power transducer, and the ultrasonic wave radiosity is 4 watts/square centimeter, supersonic frequency 20KHz.Return flow control valve and output flow control valve adopt electronically controlled proportional valve.10 cubic metres of premixed liquid storage tank volumes, 5 cubic metres of premix groove volumes, cell body is stainless steel material.
Embodiment 2
Another example of device of the present invention shown in the figure, wherein pipeline carries booster pump to select low discharge vane type pipe pressurizing pump for use, and metered flow is 50 cubic metres/hour, 25 meters of lifts.Ultrasonic transducer is square tubular type ultrasonic power transducer, and the ultrasonic wave radiosity is 12 watts/square centimeter, supersonic frequency 24KHz.Return flow control valve and output flow control valve adopt electronically controlled proportional valve, 8 cubic metres of premixed liquid storage tank volumes, and 3 cubic metres of premix groove volumes, the cell body material is enamel material.
Embodiment 3
An embodiment of nano-dispersed method of the present invention, the preparation of nano silicon dispersion liquid: the nano-solid powder is a nano-silica powder, nano powder particle diameter 10～20 nanometers, solvent is a deionized water, solid concentration 10%, dispersant is selected low-molecular-weight polypropylene acid ammonium for use, total amount 0.6%, 2 cubic metres/hour of processing speeds, capacity of returns 14%, pressure 2.4 kg/cm, 12 watts/square centimeter of tubular ultrasonic wave power density, supersonic frequency 20KHz, nanometer slurries stable state, static do not have layering more than 3 months.
Embodiment 4
Another embodiment of nano-dispersed method of the present invention, the preparation of nano titanium oxide dispersion: the nano-solid powder is the nanometer titanium dioxide titanium valve, nano powder particle diameter 30～50 nanometers, solvent is a deionized water, solid concentration 18%, dispersant and stabilizing agent are that sodium lignin sulfonate and methylene two anti-sulfonic acid are received mixture, total amount 0.7%, 2.4 cubic metres/hour of processing speeds, capacity of returns 10%, pressure 2.8 kg/cm, 14 watts/square centimeter of tubular ultrasonic wave power density, supersonic frequency 24KHz, nanometer slurries stable state, static do not have layering more than 3 months.
Embodiment 5
Another embodiment of nano-dispersed method of the present invention, the preparation of nano-aluminium oxide dispersion liquid: the nano-solid powder is nanometer three oxygen two aluminium powders, nano powder particle diameter 20～30 nanometers, and solvent is a deionized water, solid concentration 14%, dispersant is selected the DARVANC dispersant of U.S. R.T.Vanderbilt company for use, total amount 0.6%, 2.2 cubic metres/hour of processing speeds, capacity of returns 12%, pressure 3 kg/cm, 6 watts/square centimeter of tubular ultrasonic wave power density, supersonic frequency 18KHz.Nanometer slurries stable state, static do not have layering more than 3 months.
Claims (8)
1, a kind of continuous industrialized nano powder dispersal device comprises: high-order premixed groove (1), premix storage tank (4), choke valve (3), pipe pressurizing pump (5), tubular ultrasonic ripple processor (6), nanometer slurries efferent duct (7), sensor (8), output flow control valve (9), return flow control valve (10), reflux line (11), nanometer serum storage tank (12), nanometer slurries pot-type equipment (13); It is characterized in that, paddle is installed in the high-order premixed groove (1), paddle is installed in the premix storage tank (4), premix slurries conveyance conduit (2) and high-order premixed groove joint, on tubular ultrasonic ripple processor nanometer slurries efferent duct, optical pickocff (8) is installed, can online detection nanometer slurries dispersion effect, reflux line and return flow control valve are installed simultaneously, regulate processing speed and control nanometer slurries quality; The nanometer premixed liquid that needs to handle is carried to tubular ultrasonic ripple processor by the pipe pressurizing pump, regulate nanometer slurries processing speed by control pipeline booster pump with adjusting output flow control valve and return flow control valve, improve the pressure of nanometer slurries in the tubular ultrasonic ripple processor simultaneously, improve the cavitation threshold values of slurries, be implemented in and carry out the ultrasonic wave processing under the higher unit are ultrasonic radiation intensity.
According to the described device of claim 1, it is characterized in that 2, high-order premixed groove is vertical groove, the cell body material is stainless steel or enamel material, and the bottom of groove has and the joining pipeline of premixed liquid storage tank, and choke valve is arranged on the pipeline.
3, according to the described device of claim 1, it is characterized in that, the premix storage tank is vertical groove, the cell body material is stainless steel or enamel material, the volume of premix storage tank is 1～4 times that high-order premix cell body amasss, the bottom of groove has and the joining pipeline of tubular ultrasonic ripple processor, and booster pump is arranged on the pipeline.
4, the described device of claim 1, it is characterized in that, processor for ultrasonic wave is a tubular type high-power ultrasonic processor, tube wall is the spoke side of transducer, radiant tube is round tube or rectangular tube, and pipe wall material is stainless steel or titanium alloy, and transducer is for forcing the direct-cooling type transducer, 2～16 watts/square centimeter of the sound power density scopes of transducer, frequency range 10～40KHz.
5, a kind of continuous industrialized nano powder process for dispersing is characterized in that processing step is:
A, nano powder, solvent medium, dispersant, stabilizing agent and coupling agent are added in the premix groove (1), carry out stirring and evenly mixing, obtain premixed liquid;
B, above-mentioned premixed liquid is sent in the premix slurry tank (4) by pipeline (2), choke valve (3);
C, the premixed liquid in the premix slurry tank (4) is sent in the tubular ultrasonic ripple processor (6) 1.5～10 kilograms/cm of pressure of slurries in the transducer by pipe pressurizing pump (5)
2
Nanometer slurries after d, online detection are handled by tubular ultrasonic ripple processor (6), and according to testing result adjustment return flow control valve (10) and output flow control valve (9);
E, nanometer slurries are sent into nanometer slurry tank (12), and canned by pot-type equipment (13).
6, in accordance with the method for claim 5, it is characterized in that described nano powder is metal nano powder, oxide nonmetallic powder, salt nano powder or CNT, described nano powder particle diameter 5～100 nanometers.
7, in accordance with the method for claim 5, it is characterized in that described solvent medium is the mixture of aqueous medium, organic media or these media.
8, in accordance with the method for claim 5, it is characterized in that, described stabilizing agent and dispersant are a kind or their mixtures in low-molecular-weight polypropylene acid ammonium, low molecular weight sodium polyacrylate, carboxymethyl cellulose, lignosulfonates or the methylene dinaphthalene sulfonate, coupling agent is silane, titanate esters, borate or aluminic acid ester a kind or their mixture wherein, and the chemical content total amount of the interpolation of described dispersant, stabilizing agent and coupling agent is 0.1～20%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101654107A CN100469427C (en) | 2006-12-19 | 2006-12-19 | A continuous industrialized nano material dispersion device and method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101654107A CN100469427C (en) | 2006-12-19 | 2006-12-19 | A continuous industrialized nano material dispersion device and method |
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| Publication Number | Publication Date |
|---|---|
| CN1994541A CN1994541A (en) | 2007-07-11 |
| CN100469427C true CN100469427C (en) | 2009-03-18 |
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| GB2483359A (en) * | 2010-08-31 | 2012-03-07 | Xerox Corp | Continuous process for preparing polymer nanodispersions |
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| CN102225320B (en) * | 2011-03-25 | 2014-11-26 | 泉州师范学院 | Dispersing device for micron/nano-particle suspension |
| CN102489341B (en) * | 2011-12-09 | 2013-10-02 | 华东理工大学 | Device and method for preparing carbon-supported platinum nanometer catalyst slurry |
| CN103082391B (en) * | 2013-01-30 | 2015-04-01 | 湖北中烟工业有限责任公司 | Ultrasonic emulsification feeding device and feeding method for cigarettes |
| CN103240049B (en) * | 2013-05-24 | 2014-08-06 | 张德福 | Reactor for industrially producing monodisperse nano materials |
| CN104549021B (en) * | 2015-01-13 | 2015-12-30 | 中国石油大学(华东) | A kind of hydrophobic nanoparticles and surfactant compound dispersion device and application |
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| CN107875961A (en) * | 2017-12-25 | 2018-04-06 | 苏州擎动动力科技有限公司 | Nano-powder decentralized system |
| CN108841426B (en) * | 2018-05-31 | 2021-07-20 | 烟台恒诺新材料有限公司 | Method for uniformly dispersing nano carbon material in lubricating oil |
| CN110003002B (en) * | 2019-04-26 | 2020-03-17 | 济南万兴达化工有限公司 | Production process of high-yield ethyl trifluoroacetate |
| CN111569816A (en) * | 2020-06-30 | 2020-08-25 | 江苏京控装备有限公司 | Solid-liquid homogeneous mixing pump matched multi-tube reactor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| GB2483359A (en) * | 2010-08-31 | 2012-03-07 | Xerox Corp | Continuous process for preparing polymer nanodispersions |
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| CN1994541A (en) | 2007-07-11 |
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