CN100355495C - Nanometer fluid preparation method using rotating packed bed reactor - Google Patents
Nanometer fluid preparation method using rotating packed bed reactor Download PDFInfo
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- CN100355495C CN100355495C CNB2004100987931A CN200410098793A CN100355495C CN 100355495 C CN100355495 C CN 100355495C CN B2004100987931 A CNB2004100987931 A CN B2004100987931A CN 200410098793 A CN200410098793 A CN 200410098793A CN 100355495 C CN100355495 C CN 100355495C
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Abstract
The present invention discloses a method for preparing organic phase fluid dispersed with metal oxide nanometer particles, such as heat conducting fluid or lubricating oil, which comprises the steps: an alkali water solution (water phase) and an organic solution (organic phase) containing metal organic acid salts are put into a reactor of a rotary filling bed; the two solutions radically flow through the rotary filling bed under the action of large centrifugal force; the organic phase contacts the water phase in the two solutions; reactants in the two phases rapidly make an alkali neutralization and oxidation reaction to prepare metal oxide nanometer particles on the contact surface of the two phases, the formed metal oxide nanometer particles can be stably dispersed in the organic phase, and then the nanometer fluid is prepared.
Description
Technical field
The invention relates to for example preparation method of heat-conducting fluid or lubricating oil of a kind of oil phase fluid that is dispersed with metal oxide nanoparticles.
Background technology
Nano-fluid is a kind of new functional fluid, its preparation method mainly is that (as: liquid such as heat-conducting fluid, lubricating oil or water that radiator, engine or refrigerating and air conditioning system are commonly used) adds the solid particles that a small amount of (＜5%) is of a size of nano-scale in traditional working fluid, with the service behaviour (as increasing the coefficient of heat conduction or friction resistant coefficient, product is then as nano heat-conductive fluid or nano lubricating oil, nanometer machine oil etc.) that improves fluid.The general method for preparing nano-fluid can be divided into two kinds: the one, and single stage preparation method (one-stepmethod), another is the rapid preparation method of multistep (multi-step method).Present single stage preparation method mainly is to utilize the physical vapor method, directly imports in the working fluid behind the generation nano particle under high vacuum high temperature and in the airtight reactor, or for to utilize the method for arc discharge directly in the water fluid, to generate nano particle; Its advantage is all few, the easy dispersion of nanometer particle congery in the nano-fluid that is generated, and major defect comprises that then the composition and the preparation speed that are difficult to accurately to control nano particle are too slow, is not suitable for a large amount of productions.Another kind of multistep prepares rule suddenly to be synthetic earlier or to buy nano particle, and then utilizes specific process for dispersing to make it to be scattered in the middle of the fluid; Its advantage is that fluid forms can variation and possess the volume production potentiality, shortcoming then be nano particle easily assemble and in fluid the meeting rapid subsidence, cause the relatively poor problem of fluid stable character.
In recent years, the research of RPB and application solved many under normal gravitational field insoluble problem.Especially RPB can greatly be strengthened matter and passes process, makes tens meters high towers can be with the RPB about 2 meters.Use in separation processes such as absorption, stripping, distillation and all obtained beyond thought effect, for example United States Patent (USP) the 4283255th; 4382045; 4382900; And No. 4400275.Chinese patent publication number CN1116146A (1996) proposes to use this matter to pass the preparation method of the ultra-fine grain of equipment, wherein two kinds of out of phase liquid is fed to the shaft core position of a RPB through distributor by the inner and outer pipe of concentric tubes, by the rotational gravity field action, in packed bed the contact and react.Yet the method for this CN1116146A is that its resulting metal inorganic hydrochlorate particle is to be present in the liquid with precipitated form at the metal inorganic hydrochlorate particle of preparation free settling.To so far, do not see open report as yet in the application of nano-fluid preparation.The content of aforementioned patent is merged in this case in the reference mode.
Summary of the invention
Main purpose of the present invention is to provide a kind of single stage preparation method of nano-fluid.
Another object of the present invention is providing the single stage preparation method who is scattered in nano-fluid wherein that a kind of metal oxide nanoparticles can be stable.
A kind of preparation method who is dispersed with the organic facies fluid of metal oxide nanoparticles who finishes according to content of the present invention comprises for achieving the above object: an organic solution that is dissolved with metal organic acid salt of alkaline aqueous solution of water and organic facies is fed to RPB in the rotation of an axle center, this RPB is to be positioned at a cabin, wherein this two solution radial flow under big centrifugal action is crossed RPB, organic facies and water are in contact with one another therein, reactant in the two-phase reacts on two phase-contact surfaces and forms metal oxide nanoparticles, and what formed metal oxide nanoparticles was stable is scattered in the organic facies.
Preferable, a liquid that contains the two phase stratification of water and organic facies is collected in the bottom that the inventive method further is included in this cabin; And the water and the organic facies of separating the liquid of this two phase stratification, with obtain metal oxide nanoparticles stable be scattered in wherein an organic facies fluid.Better, the inventive method further comprises volatilization or distills a part of organic solvent that removes in this organic facies fluid, and obtains the organic facies fluid that a metal oxide nanoparticles content increases.Better, the inventive method further comprises the organic facies fluid that will be dispersed with metal oxide nanoparticles and mixes with an oil phase fluid; And volatilization or distillation remove organic solvent in the fluid-mixing that is obtained, and obtain an oil phase fluid that is dispersed with metal oxide nanoparticles.Better, the inventive method further comprises the organic facies fluid that metal oxide nanoparticles content is increased and mixes with an oil phase fluid; And volatilization or distillation remove organic solvent in the fluid-mixing that is obtained, and obtain an oil phase fluid that is dispersed with metal oxide nanoparticles.This oil phase fluid that is dispersed with metal oxide nanoparticles can be used as a heat-conducting fluid or lubricating oil.
Preferable, this organic solution is that this metal organic acid salt is dissolved in a carbon number between the organic solvent of 7 to 32 hydrocarbon or the hydrocarbon fluoridized and form.Better, this hydrocarbon is alkane, alkene or alkynes.Best, this hydrocarbon is an alkane.
Preferable, this metal organic acid salt is that carboxylate has following chemical formula: [RCOO]
zM
Z+, wherein R is a carbon number between 7 to 32 saturated or unsaturated hydrocarbon hydrophobic group, or carbon number between 7 to 32, have the saturated of one or two hydroxyl or a unsaturated hydrocarbon hydrophobic group; M is a metal, and z is the valence mumber of metal.Better, R is a carbon number between 11 to 23 saturated or unsaturated hydrocarbon hydrophobic group; And M is Cu, Zn, Fe, Al, Zr or Ag.
Preferable, this metal organic acid salt is copper oleate (copper oleate), copper abietinate (copperabietate), ethyl acetoacetate copper (copper ethylacetoacetate), copper naphthenate (coppernaphthenate), cupric octoate (copper octoate), copper resinate (copper resinate), ricinoleic acid copper (copper ricinoleate), copper stearate (copper stearate), zinc oleate (zinc oleate), ethyl acetoacetate zinc (zinc ethylacetoacetate), zinc octoate (zinc octoate), zinc ethyl hexanoate (zinc2-ethylhexoate), zinc laurate (zinc laurate), zinc linoleate (zinc linoleate), zinc palmitate (zincpalmitate), zinc ricinate (zinc ricinoleate), zinc stearate (zinc stearate), zinc undecylenate (zinc undecylenate), iron octoate (ferric octoate), iron oleate (ferric oleate), ferric resinate (ferric resinate), ferric stearate (ferric stearate), thylhexoic acid iron (ferric 2-ethylhexoate), aphthenic acids ferrous (ferrous naphthenate), stearic acid ferrous (ferrous stearate), or sad ferrous (ferrous octoate).
Preferable, this alkaline aqueous solution is soluble in water and prepare with being dissolvable in water inorganic base in the water or organic base.
Preferable, this alkaline aqueous solution is the aqueous solution of alkali metal hydroxide.
Preferable, this alkaline aqueous solution has a temperature between room temperature to 100 ℃, and organic solution has one between the temperature of room temperature to the boiling point of the organic solvent of this organic solution.
Preferable, this alkaline aqueous solution and organic solution are that the axle center district by this RPB is imported into.
Preferable, this RPB comprises around a centre gangway district in axle center and centers on the annular fill area in this centre gangway district, filler has been fixed in this annular fill area, and should the annular fill area and this centre gangway district only be fluid communication by both interfaces, and should be fluid communication with this cabin excircle by the annular fill area by this annular fill area.
Preferable, this metal oxide nanoparticles has the size of several nanometers to one hundred nanometers.
The present invention is directed to the scattering problem of nano particle in the organic facies fluid and solve,, could in one step, finish synthetic and its dispersion steps in fluid of nano particle simultaneously again in conjunction with the architectural characteristic of RPB and the principle of two phase reaction.The inventive method has the advantage of high-quality biography speed and two-phase interface reaction, and can prepare the good nano-fluid of disperse properties under high efficiency, two-forty condition in one step.The inventive method has the potentiality of volume production.
Embodiment
Below, will with a preferred embodiment the present invention be described with reference to graphic.One is suitable for particle diameter increase of the present invention is shown in Fig. 1 with the RPB system.
Alkaline aqueous solution is delivered to a liquid-inlet 9 from raw material tank 1 with liquid pump 14, by a liquid distribution trough 10 of being located at the axle center district of a ring rotation packed bed 3 aqueous solution is sprayed to this annular packing 12 equably.Simultaneously, the organic solution that is dissolved with metal organic acid salt is delivered to a liquid-inlet 6 from raw material tank 2 with liquid pump 15, by a liquid distribution trough 4 of being located at the axle center district of a ring rotation packed bed 3 organic solution is sprayed to this annular packing 12 equably.This ring rotation packed bed 3 is the rotatable inside that is arranged at a cabin 11.This ring rotation packed bed 3 is driven under the effect of variable speed driver 13, produce great centrifugal force, make this two solution fast moving and cut into more fine drop outward for this annular packing 12, and in this annular packing 12, contact with each other, reactant in two solution like this will carry out acid-base neutralization and oxidation reaction apace and obtain metal oxide nanoparticles on two phase-contact surfaces, product will flow out this annular packing 12, and come together in the bottom in the cabin 11 of RPB, drain into product feeder 8 by liquid outlet 7 at last.Can form the liquid of the two phase stratification that contains water and organic facies in feeder 8 product, and stable being scattered in this organic facies of formed metal oxide nanoparticles.Through further decant (Decantation) or other suitable separation method, the liquid of this two phase stratification can be divided into water and organic facies, so obtain being dispersed with the organic facies fluid (abbreviating nano-fluid as) of metal oxide nanoparticles.
The present invention will further be understood by the following example, and these embodiment but not are used to limit the scope of the invention as illustrative purposes only.
Description of drawings
Fig. 1 is the schematic flow sheet of preferred embodiment of the present invention.
Fig. 2 is transmission electron microscope (transmission electron microsscopy, the TEM) photo of the copper oxide nano particle in the middle of the prepared nano-fluid of embodiments of the invention 1.
Fig. 3 is the grading curve that utilizes the copper oxide nano particle in the middle of the prepared nano-fluid of the embodiment of the invention that light scattering method records 1.
Figure 4 shows that the TEM photo of the zinc oxide nano-particle in the middle of the prepared nano-fluid of embodiments of the invention 2.
Reference numeral
1. aqueous feed solution groove 2. organic solution raw material tanks 3. RPBs
4,10. liquid distributor 6,9. liquid-inlet 7. liquid outlets
8. cabin 12. annular packings of feeder 11. RPBs
13. variable speed driver 14,15. liquid pumps
The specific embodiment
The preparation of embodiment 1, organic phase nano cupric oxide fluid
The specification of the employed RPB of present embodiment is as follows:
Filler stainless steel braiding silk screen, line footpath 0.22mm
Filler specific area 603m
2/ m
3
Packed bed voidage 96.7%
Annular packed bed inside radius 6.1cm
Annular packed bed outer radius 14.7cm
Packed bed axial height 9.5cm
With (C
17H
33COO)
2Cu and NaOH are dissolved in respectively in normal octane and the water, concentration respectively is 0.1mol/L and 0.2mol/L, and place and respectively be heated to more than 90 ℃ in the different feeds groove, relend and help pump to transmit this two raw material, flow with 0.1L/min reacts the above-mentioned RPB that injects rotating speed 1800rpm simultaneously, the temperature of this RPB is controlled in 90 ℃, and reaction pressure is 1atm.Collect the product after reaction is finished, but be the two phase stratification liquid of organic facies and water natural layering.The organic facies of taking out the upper strata is the organic facies fluid that contains nano cupric oxide.Figure 2 shows that transmission electron microscope (transmission electron microscopy, the TEM) photo of the copper oxide nano particle that prepared fluid is central.Fig. 3 is the grading curve that utilizes light scattering method to record.Fig. 2 and 3 shows that the particle size of the copper oxide nano particle in the middle of the prepared fluid of present embodiment is mainly below 10nm.
If when the organic facies solvent changed n-dodecane into, the fluid preparation process was the same; But the organic facies raw material all is controlled in more than 120 ℃ in the temperature of temperature in the raw material tank and supergravity reactor, also can obtain a finely disseminated organic facies nano-fluid after the reaction.
Present embodiment prepared organic phase nano-fluid can further utilize vacuum distillation method to remove a part of solvent, solids content is increased to more than the 10 weight %, and does not influence dispersiveness.
(UK), the coefficient of heat conduction that can record the prepared 2 weight % nano-fluids of present embodiment has promoted more than 10% than former fluid (normal octane or n-dodecane) coefficient of heat conduction measurement equipment that designs by the hot plate method principle for H471, P.A.Hilton Ltd..
The preparation of embodiment 2, organic facies nano zine oxide fluid
Get (C
17H
33COO)
2Zn and (C
17H
31COO)
2Zn is dissolved in normal octane respectively, and concentration respectively is 0.25mol/L and 0.5mol/L.Use these the two kinds of organic solutions and the NaOH aqueous solution (concentration is 0.15mol/L) to carry out two phase reaction respectively.The temperature of the aqueous solution of organic solution and NaOH is respectively 100 ℃ and 90 ℃.The aqueous solution of organic solution and NaOH all injects the RPB of embodiment 1 with the flow of 0.1L/min, in rotating speed 1800rpm, and 100 ℃ of the temperature of RPB, and pressure is to react under the 1atm.Collect the product after reaction is finished, be the two phase stratification liquid of organic facies and water natural layering, the organic facies in the middle of taking out is the organic facies fluid that contains nano zine oxide.Figure 4 shows that the central zinc oxide nano-particle TEM photo of fluid of preparation, particle size is below the 40nm, contains non-single shape stuff and other stuff such as ball-shaped and triangle simultaneously.
The preparation of embodiment 3, organic facies nano-sized iron oxide fluid
(C
17H
33COO)
3The preparation of Fe
Get C
17H
33The COONa aqueous solution (concentration is 0.05mol/L) and inorganic molysite FeCl
3(also can use Fe
2(SO
4)
3) aqueous solution (concentration is 0.08mol/L) is with C
17H
33COO: Fe
3+The ratio of=3: 1 (mol ratio) is mixed mutually, and mixed sediment is filtered, cleans and drying, can get (the C of rufous
17H
33COO)
3The Fe solid.
Nanometer Fe
2O
3The preparation of fluid
With (C
17H
33COO)
3Fe and NaOH are dissolved in compound concentration in normal octane and the water respectively and respectively are the organic solution and the aqueous solution of 0.15mol/L and 0.5mol/L, and place and respectively be heated to more than 70 ℃ in the different material groove, relend the RPB that helps pump this two raw material to be injected embodiment 1 with the flow of 0.1L/min, in rotating speed 1800rpm, 70 ℃ of the temperature of RPB, and pressure is to react under the 1atm.Collect the product after reaction is finished, be the two phase stratification liquid of organic facies and water natural layering, the organic facies in the middle of taking out is the organic facies fluid that contains nano-sized iron oxide.Prepared organic phase nano-fluid can further utilize vacuum distillation method to remove a part of solvent to improve nanometer Fe
2O
3The content of particle, and can not influence its disperse properties.
The preparation of embodiment 4, organic facies nano magnetic iron oxide fluid
With (C
17H
35COO)
2Fe and NaOH are dissolved in compound concentration in normal octane and the water respectively and respectively are the organic solution and the aqueous solution of 0.02mol/L and 0.4mol/L, and place in the different material groove, relend the RPB that helps pump this two raw material to be injected embodiment 1 with the flow of 0.1L/min, in rotating speed 1800rpm, 40 ℃ of the temperature of RPB, and pressure is to react under the 1atm.Collect the product that reactor flowed out, be the two phase stratification liquid of organic facies and water natural layering, the organic facies in the middle of taking out is the organic facies fluid that contains magnetic ferric oxide nano particles.Prepared magnetic organic facies nano-fluid can further utilize vacuum distillation method to remove a part of solvent with raising magnetic ferric oxide nano particles content, and can not influence its disperse properties.
The preparation of embodiment 5, nano lubricating oil
By the resulting organic facies nano-fluid of the present invention, can be used for preparing nano lubricating oil indirectly.Utilize decompression distillation to remove organic solvent in the nano-fluid, the oxide nano-particles in the organic facies fluid then is transferred in the middle of the lubricating oil and keeps dispersion stabilization originally originally.
After getting 100 milliliters of cupric oxide nano fluid that embodiment 1 method makes 400 milliliters (about 0.5～1 weight % of solid content) and commercially available Mobil SuperSyn 5W-50 lubricating oil and mixing mutually with stirrer, the disperse properties of observing copper oxide nano particle is not influenced by mixed process.Further this oil mixture is utilized (60 ℃ of decompression distillation, 35Torr) remove wherein normal octane after, can obtain the nano lubricating oil of the about 5 weight % of solid content, and copper oxide nano particle wherein can keep fine dispersion stability, reach not sedimentation more than 6 months.
The test of nano lubricating oil high temperature disperse properties
Get and held temperature after the nano lubricating oil for preparing is warming up to 200 ℃ with 20 ℃/min heating rate one hour.Cool off its color of observation and sedimentation character after one hour, found that the situation before nano lubricating oil is kept heating.Repeat above-mentioned heating-cooling experiment (more than at least three times) for several times, found that the outward appearance and the dispersiveness of the nano lubricating oil through repeating heat treated is not subjected to temperatures involved, be illustrated in the dispersion stabilization under the high-temperature operation.
The present invention is described in, and person skilled in the art scholar still can make multiple variation and the modification that does not break away from following claim.
Claims (13)
1. preparation method who is dispersed with the organic facies fluid of metal oxide nanoparticles, comprise a organic solution that is dissolved with metal organic acid salt with alkaline aqueous solution of water and organic facies and be fed to RPB in the rotation of an axle center, this RPB is to be positioned at a cabin, wherein this two solution radial flow under centrifugal action is crossed RPB, organic facies and water are in contact with one another therein, reactant in the two-phase reacts on two phase-contact surfaces and forms metal oxide nanoparticles, and what formed metal oxide nanoparticles was stable is scattered in the organic facies;
Described RPB comprises around a centre gangway district in axle center and centers on the annular fill area in this centre gangway district, filler has been fixed in this annular fill area, and should the annular fill area and this centre gangway district only be fluid communication by both interfaces, and should be fluid communication with this cabin excircle by the annular fill area by this annular fill area;
The bottom collection one in described cabin contains the liquid of the two phase stratification of water and organic facies; And the water and the organic facies of separating the liquid of this two phase stratification, with obtain metal oxide nanoparticles stable be scattered in wherein an organic facies fluid;
Described alkaline aqueous solution and organic solution are that the axle center district by this RPB is imported into;
Described organic solution is that this metal organic acid salt is dissolved in a carbon number between the organic solvent of 7 to 32 hydrocarbon or the hydrocarbon fluoridized and form;
Described alkaline aqueous solution is the aqueous solution of alkali metal hydroxide.
2. the method for claim 1, it further comprises volatilization or distillation and removes a part of organic solvent in this organic facies fluid, and obtains the organic facies fluid that a metal oxide nanoparticles content increases.
3. the method for claim 1, it further comprises the organic facies fluid that will be dispersed with metal oxide nanoparticles and mixes with an oil phase fluid; And volatilization or distillation remove organic solvent in the fluid-mixing that is obtained, and obtain an oil phase fluid that is dispersed with metal oxide nanoparticles.
4. method as claimed in claim 2, it further comprises the organic facies fluid that metal oxide nanoparticles content is increased and mixes with an oil phase fluid; And volatilization or distillation remove organic solvent in the fluid-mixing that is obtained, and obtain an oil phase fluid that is dispersed with metal oxide nanoparticles.
5. as claim 3 or 4 described methods, wherein this oil phase fluid that is dispersed with metal oxide nanoparticles is a heat-conducting fluid or lubricating oil.
6. the method for claim 1, wherein this hydrocarbon is alkane, alkene or alkynes.
7. method as claimed in claim 6, wherein this hydrocarbon is an alkane.
8. method as claimed in claim 1, wherein this metal organic acid salt is that carboxylate has following chemical formula: [RC00]
zM
Z+, wherein R is a carbon number between 7 to 32 saturated or unsaturated hydrocarbon hydrophobic group, or carbon number between 7 to 32, have the saturated of one or two hydroxyl or a unsaturated hydrocarbon hydrophobic group; M is a metal, and z is the valence mumber of metal.
9. method as claimed in claim 8, wherein R is a carbon number between 11 to 23 saturated or unsaturated hydrocarbon hydrophobic group; And M is Cu, Zn, Fe, Al, Zr or Ag.
10. method as claimed in claim 1, wherein this metal organic acid salt is copper oleate, copper abietinate, ethyl acetoacetate copper, copper naphthenate, cupric octoate, copper resinate, ricinoleic acid copper, copper stearate, zinc oleate, ethyl acetoacetate zinc, zinc octoate, zinc ethyl hexanoate, zinc laurate, zinc linoleate, zinc palmitate, zinc ricinate, zinc stearate, zinc undecylenate, iron octoate, iron oleate, ferric resinate, ferric stearate, thylhexoic acid iron, aphthenic acids is ferrous, stearic acid is ferrous or sad ferrous.
11. the method for claim 1, alkaline aqueous solution wherein are soluble in water and prepare with being dissolvable in water inorganic base in the water or organic base.
12. the method for claim 1, alkaline aqueous solution wherein have a temperature between room temperature to 100 ℃, and organic solution has one between the temperature of room temperature to the boiling point of the organic solvent of this organic solution.
13. the method for claim 1, wherein this metal oxide nanoparticles has the size of several nanometers to one hundred nanometers.
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| KR101698762B1 (en) * | 2010-04-30 | 2017-01-23 | 삼성에스디아이 주식회사 | Method of preparing lithium transition metal phosphate |
| CN103041722B (en) * | 2012-12-08 | 2015-07-01 | 中北大学 | Supergravity device for rapidly dissolving water-soluble polymers |
| CN104368301B (en) * | 2013-08-14 | 2016-08-17 | 中国石油化工股份有限公司 | A kind of supergravity reactor and reaction method |
| CN108568306B (en) * | 2017-03-08 | 2020-10-20 | 中国石油化工股份有限公司 | Preparation method and application of basic copper-zinc carbonate double salt |
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|---|---|---|---|---|
| US4283255A (en) * | 1977-12-01 | 1981-08-11 | Imperial Chemical Industries Limited | Mass transfer process |
| US4400275A (en) * | 1980-12-08 | 1983-08-23 | Imperial Chemical Industries Plc | Mass transfer apparatus and process |
| CN1116146A (en) * | 1995-05-26 | 1996-02-07 | 北京化工大学 | Preparing method for ultromicro granule |
| CN1454917A (en) * | 2002-04-30 | 2003-11-12 | 财团法人工业技术研究院 | Method of removing volatile component from high-viscosity liquid using rotary packed bed |
| CN1461731A (en) * | 2002-05-31 | 2003-12-17 | 湘潭大学 | Preparation method of nanometer grade super fine calcium carbonate |
| CN2597059Y (en) * | 2003-01-29 | 2004-01-07 | 杭州盛大高科技机电有限公司 | Internal balance type compression filling device |
-
2004
- 2004-12-16 CN CNB2004100987931A patent/CN100355495C/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4283255A (en) * | 1977-12-01 | 1981-08-11 | Imperial Chemical Industries Limited | Mass transfer process |
| US4400275A (en) * | 1980-12-08 | 1983-08-23 | Imperial Chemical Industries Plc | Mass transfer apparatus and process |
| CN1116146A (en) * | 1995-05-26 | 1996-02-07 | 北京化工大学 | Preparing method for ultromicro granule |
| CN1454917A (en) * | 2002-04-30 | 2003-11-12 | 财团法人工业技术研究院 | Method of removing volatile component from high-viscosity liquid using rotary packed bed |
| CN1461731A (en) * | 2002-05-31 | 2003-12-17 | 湘潭大学 | Preparation method of nanometer grade super fine calcium carbonate |
| CN2597059Y (en) * | 2003-01-29 | 2004-01-07 | 杭州盛大高科技机电有限公司 | Internal balance type compression filling device |
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