CN1206072C - Process for continuously preparing superfine nano powder by precipitation method and special equipment thereof - Google Patents
Process for continuously preparing superfine nano powder by precipitation method and special equipment thereof Download PDFInfo
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- CN1206072C CN1206072C CN 03113326 CN03113326A CN1206072C CN 1206072 C CN1206072 C CN 1206072C CN 03113326 CN03113326 CN 03113326 CN 03113326 A CN03113326 A CN 03113326A CN 1206072 C CN1206072 C CN 1206072C
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- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000011858 nanopowder Substances 0.000 title claims abstract description 21
- 238000001556 precipitation Methods 0.000 title abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 49
- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- 238000010899 nucleation Methods 0.000 claims abstract description 23
- 230000006911 nucleation Effects 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 239000000725 suspension Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000005516 engineering process Methods 0.000 claims description 14
- 239000012716 precipitator Substances 0.000 claims description 10
- 230000003068 static effect Effects 0.000 claims description 8
- 239000000945 filler Substances 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 12
- 238000003756 stirring Methods 0.000 abstract description 10
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract 4
- 239000000047 product Substances 0.000 description 10
- 239000007789 gas Substances 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 241000080590 Niso Species 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- CJDPJFRMHVXWPT-UHFFFAOYSA-N barium sulfide Chemical compound [S-2].[Ba+2] CJDPJFRMHVXWPT-UHFFFAOYSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000010900 secondary nucleation Methods 0.000 description 1
- 238000012163 sequencing technique Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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Abstract
The invention relates to a process for continuously preparing superfine nano powder by a precipitation method, which comprises the steps of simultaneously feeding materials into a reaction kettle by a metering feeding device according to a certain proportion and speed, rapidly entering a crystal nucleus growing tube after uniform mixing and nucleation at a certain temperature and stirring speed, propelling the crystal nucleus growing tube forward under the action of a material mixing device, finally collecting suspension at an outlet at the tube end of the crystal nucleus growing tube, and drying the suspension properly to obtain the superfine nano powder. The control of the grain size is realized by respectively adjusting the temperature of the reaction kettle and the crystal nucleus growing tube, the proportion of reaction materials, the feeding speed, the stirring speed and other control factors. The invention can continuously carry out the precipitation reaction, and has high productivity; meanwhile, the nucleation process and the growth process in the precipitation reaction are separated, nucleation and growth are formed in a relatively stable environment, the particle size of the generated particles can be regulated, the monodispersity of the particles is good, the distribution is narrow, and the morphology difference is small. The invention also provides special equipment for the novel process.
Description
Technical field
The present invention relates to the preparation method of superfine powder, particularly relate to the specific equipment that a kind of precipitator method prepare ultra-fine nano-powder technology and this technology continuously.
Background technology
Ultra-fine nano-powder is meant the fines of particle diameter between 1～1000nm.Ultra-fine nano-powder causes characteristics such as unusual mechanics, electricity, magnetics, calorifics, optics and chemically reactive because of its surface effects, quantum size effect and macro quanta tunnel effect, it is had a wide range of applications at numerous areas such as catalysis, pigment, matrix materials.Therefore, the technology of preparing of nm-class more and more is subject to people's attention as an important step in the nanosecond science and technology research and development.In order to realize the nano material industrial scale, prepare the ultra-fine nano-powder that high-quality, particle size, distribution, pattern can be effectively controlled and just seem very important.
The method for preparing at present ultra-fine nano-powder is a lot, and precipitin reaction is the method for using always.Produce in the sedimentary process at chemical reaction, the formation of precipitate particles comprises nucleating process (being called nucleation process) and nuclear growth process (being called process of growth).Nucleation and process of growth all need be carried out under oversaturated condition.It is higher that the required degree of supersaturation ratio growth of nucleation requires.Because the nucleation process of precipitin reaction is often promptly finished in moment, thereby controlling factors such as the adding mode of material and admixture will influence the hypersaturated state and the final quality that influences product of solution to a great extent.
But actually, to prepare the superfine nano particle generally be to carry out in reactor discontinuous formula in precipitin reaction at present.One of reactant is at first joined in the reactor, and when another reactant adds fashionablely, chemical reaction begins, and along with the increase of degree of supersaturation, nucleus forms.When material constantly adds fashionablely, new nucleus constantly produces, and already present nucleus is constantly grown up simultaneously.Because the concentration of substrate material is bigger, and the reinforced time is longer, so for a long time, is reflected under the higher hypersaturated state and carries out, nucleation and growth two processes exist simultaneously, and the degree of supersaturation of material is in the state of variation along with the carrying out of reaction.Because nucleation is temporal difference successively, the time and the speed of each nucleus growth have nothing in common with each other, and cause reaction at the end, and the powder size that finally obtains is uneven, and monodispersity is relatively poor.
In order to change this situation, bibliographical information is arranged, and (Wang Jian Ai Ji is refined, sensitive materials, 1999 (3), 14-16), two kinds of materials that employing will participate in reaction add the method for reactor simultaneously, because the material moment reaction that adds, the hypersaturated state in the still and the feed rate of two kinds of materials are closely related, if two kinds of materials are at the uniform velocity added in proportion, make and maintain a metastable hypersaturated state in the reactor, the particulate growth is evenly carried out, to reach evengranular purpose.But these report that described reactor all belongs to the semi continuous operation of continuously feeding intermittent take-off, and operation easier is big, and the condition of control grain size is difficult to be grasped.
Summary of the invention
The invention provides the technology that a kind of precipitator method prepare ultra-fine nano-powder continuously, purpose is that the nucleation that makes precipitin reaction is separated with growth two processes and carried out continuously, can obtain the uniform high-quality ultra-fine nano-powder of size.
Another object of the present invention provides these precipitator method and prepares ultra-fine nano-powder technology institute specialized apparatus continuously, can adapt to the needs of this technological process.
The precipitator method of the present invention prepare ultra-fine nano-powder technology as follows continuously:
Reaction mass is reinforced to reactor with certain feed rate by a certain percentage through measurement charging device such as volume pump etc., keep required temperature of reaction in the still, after material under agitation mixes nucleation takes place, enter nucleus rapidly and become long tube, nucleus becomes the certain growth temperature of material maintenance in the long tube, become the interior material of long tube constantly pushing ahead in the process, by being arranged on mixing of materials mechanism (as spiral type static mixer or the filler) thorough mixing in the pipe, finally become the pipe end outlet of long tube to collect, get ultra-fine nano-powder through aftertreatment at nucleus.The present invention adopts two notes formula quantifying feeds, and two reactants are added to the bottom of still respectively simultaneously, can keep metastable degree of supersaturation in the still, and nucleation is carried out under certain speed.Controlling factors such as the proportioning of the temperature of the present invention by adjusting reactor respectively and become long tube with nucleus, reaction mass, feed rate, stir speed (S.S.) realize the control to the powder grain size.
The characteristics that the present invention finished according to one-tenth nuclear reaction moment of material in reactor will be gone into the reacted nucleation material of still and be shifted out rapidly, send into the tubular type nucleus district of growing up.Along with becoming nuclear reaction constantly to carry out in the still, and enter the grow up nucleus in district of tubular type nucleus and constantly grow up, finally from outlet output.The present invention is fed to nucleus from reactor and becomes the discharging of long-armed superfine nano particulate, forms the successive logistics.In the process that Way out moves continuously, nucleus is grown up into the powder of certain particle diameter gradually in the tubular type district.Because the time that each nucleus is stopped in nucleus becomes long tube is basic identical, so the granular size basically identical that finally grows up to.
In sum, the present invention has adopted the nucleation process of precipitin reaction and nucleus growth process technical scheme all disconnected from each other on time and space, become long tube by nucleus, the nucleus that different time is generated, enter nucleus successively according to the sequencing of nucleation and become long tube, and in pipe, grow up gradually in the moving process continuously and grow up to output successively, owing to material is identical at intraductal retention time, the time that is the nucleus growth is identical, therefore the particle size basically identical that grows up to.In addition, present method makes the parameter of whole process of preparation to be effectively controlled respectively, can regulate and control the degree of nuclei growth to the transfer rate of material by the length of tube or the change measurement charging device that change the tubular type district, thereby obtain the uniform high quality ultra-fine nano-powder of particle diameter.Advantage of the present invention is: precipitin reaction can be carried out continuously, the productivity height; Particulate nucleation and process of growth are separated, and nucleation, are grown under the metastable environment and carry out, and the deposit seeds particle diameter of generation can obtain regulation and control, and the particulate monodispersity is good, narrowly distributing, and pattern difference is little.
The specific equipment that the precipitator method of the present invention prepare ultra-fine nano-powder technology continuously comprises reactor, this reactor is furnished with jacketed type temperature control unit, whipping appts, feed-pipe, discharge nozzle and bleeder valve, the nucleus that comprises the arranged transversely that is connected with the bleeder valve of reactor in addition becomes long tube, the outer temperature control chuck that is provided with of pipe, be provided with mixing of materials mechanism in the pipe, nucleus becomes the outlet of long tube to communicate with the product receiving tank by material guiding pipe.The product receiving tank can be provided with the gas blow-down pipe.Said mixing of materials mechanism can be a static mixer, as spiral type mixer, also can be filler etc.
Feed-pipe and discharge nozzle lay respectively at the both sides of stir shaft.Feed-pipe can be two or many, is distributed on a side of stir shaft, and is passed into the bottom of reactor always.In the middle of nucleus becomes long tube, static mixer or filler can be housed, its objective is that the microcosmic in order to strengthen the vitellarium mixes.The liner of total system can constitute (as Stainless Acid Resistant Steel, titanium material, tetrafluoroethylene, plastics, glass, enamel or the like) by corrosion resistant material as required, so that be applicable to reaction and equipment washing under the various conditions.
Specific equipment of the present invention adopts two feed-pipes, and with two notes formula quantifying feeds, filling tube can be kept metastable degree of supersaturation in the still deeply to the bottom of still, and nucleation is carried out under certain speed.Material, mixes and takes place promptly to enter nucleus after the nucleation and become the long tube further growth by vigorous stirring in the bottom of reactor, and the fresh material of follow-up adding can not grown up on existing nucleus, has avoided secondary nucleation simultaneously.Can be controlled respectively each parameter (as stir speed (S.S.), temperature or the like) of nucleation district and vitellarium respectively like this,, can be obtained the particle of narrow distribution by selecting suitable operational condition.Such design can make reaction be carried out continuously, enhances productivity.Become long tube that mixing of materials device such as static mixer, filler etc. can be housed at nucleus, improve mass-transfer efficiency growth is evenly carried out, to improve the particulate monodispersity.
Specific equipment of the present invention is fit to prepare superfine nano particulate system by all kinds of precipitin reaction.The particle median size that generates can be regulated and control between the micron order at nano level.
Specific equipment of the present invention can be by the chuck heating to keep suitable temperature of reaction if be used to the precipitin reaction of absorbing heat; If be used for the heat release precipitin reaction, can remove reaction heat by the chuck cooling and keep temperature of reaction.
If precipitin reaction does not have gas to generate, then blow-down pipe only plays the purpose of the assurance system constant voltage that communicates with atmosphere in the reactor of the present invention; If generate the gas generation that also has except that precipitation in the reaction, then gas is emitted by blow-down pipe, if the gas that generates can cause environmental pollution or the value of recycling is arranged, then the gas with generation passes to finishing apparatus.
Description of drawings
Further specify the structure of specific equipment of the present invention below by accompanying drawing.
Accompanying drawing 1 is a structural representation of the present invention; Accompanying drawing 2 is the vertical view of reactor; Accompanying drawing 3 is static mixing screw structure unit block synoptic diagram.
Among the figure: the 1-reactor; The 2-chuck; The 3-filling tube; 4-powerful motor agitator; 5 bleeder valves; The 6-nucleus becomes long tube; 7-mixing of materials mechanism; The 8-material guiding pipe; 9-product receiving tank; The 10-blow-down pipe
The material that participates in precipitin reaction adds reactor 1 bottom respectively through filling tube 3-1,3-2 (referring to Fig. 2) in the proper ratio continuously by volume pump, and the temperature in the reactor 1 is controlled by chuck 2-1.Mixing of materials is even under the brute force of agitator 4 stirs, and nucleation process moment carries out.By the flow of by-pass valve control 5 adjusting dischargings, the material after nucleation is finished enters nucleus and becomes long tube 6 to carry out the growth of nucleus, and by growth temperature in the chuck 2-2 control tube, after reaction finished, material entered product receiving tank 9 through material guiding pipe 8 and treats aftertreatment.Blow-down pipe 10 is arranged, logical atmosphere or the gas discharge (or absorbing processing) that some precipitin reaction is generated above the product receiving tank 9.The temperature of total system is controlled by the logical thermostat(t)ed water of chuck, nucleus becomes mixing of materials mechanism 7 in the long tube, make the material uniform mixing, said mixing of materials device can be a spiral type static mixer shown in Figure 3, and material constantly advances in becoming long tube and is subjected to cloudy Buddhist nun's effect of spiral type static mixer in the process and reaches well-mixed purpose.By the structural parameter D that changes Fig. 3 unit block, the admixture that L changes material.
Embodiment
The preparation of embodiment 1 extra-fine nickel powder
20 kilograms of single nickel salt NiSO
46H
2O is dissolved in deionized water and forms 150 liters of solution, is heated to 80 ℃, is labeled as solution A.9 kilograms of diamines and 4.8 kilograms of sodium hydroxide are dissolved in deionized water and form 150 liters of solution, are labeled as solution B.Solution A and solution B are joined respectively in the reactor of the present invention with the flow of volume pump with 1.25 liters/minute.Temperature is controlled to be 80 ℃, 700 rev/mins of stirring velocitys by the logical thermostat(t)ed water of chuck in the reactor.Nucleus becomes the temperature of long tube to be controlled to be 60 ℃, and ammonia that reaction generates and nitrogen are introduced the ammonia absorption unit through blow-down pipe, and ammonia absorbs the back nitrogen purge.Enter the product receiving tank from the effusive nickel powder suspension of material guiding pipe, after filtration, washing, drying obtain product.Reaction was carried out 2 hours, median size is about 4.3 kilograms an of nickel powder about 30nm.
The preparation of embodiment 2 ultra-fine barium sulfate powders
Concentration is the sodium sulfate 315 premium on currency solution of 1.5 mol, is heated to 40 ℃, is labeled as solution A.Concentration is the barium sulphide 210 premium on currency solution of 0.75 mol, is heated to 40 ℃, is labeled as B.With the flow of solution A with 3 liters/minute, solution B joins respectively in the reactor of the present invention with 2 liters/minute flow with volume pump.Temperature is controlled to be 40 ℃, 500 rev/mins of stirring velocitys by the logical thermostat(t)ed water of chuck in the reactor.Nucleus becomes the temperature of long tube to be controlled to be 40 ℃.Enter the product receiving tank from the effusive barium sulfate suspension of material guiding pipe, after filtration, washing, drying obtain product.Reaction was carried out 1 hour 40 minutes, median size is about 35 kilograms an of ultra-fine barium sulfate about 1.0 μ m.
Claims (10)
1. the precipitator method prepare ultra-fine nano-powder technology continuously, it is characterized in that as follows: reaction mass is added to the reactor bottom respectively simultaneously, keep required temperature of reaction in the still, after material under agitation mixes nucleation takes place, enter nucleus and become long tube, under the effect of mixing of materials device, push ahead, finally become the pipe port of long tube to collect suspension, get ultra-fine nano-powder after drying at nucleus.
2. the precipitator method according to claim 1 prepare ultra-fine nano-powder technology continuously, it is characterized in that nucleus becomes material thorough mixing in the process of advancing in the long tube.
3. the precipitator method according to claim 1 and 2 prepare ultra-fine nano-powder technology continuously, it is characterized in that reactor adopts two notes formula quantifying feeds, and two reactants are dosed to the bottom of still respectively.
4. the precipitator method of a claim 1 prepare the specific equipment of ultra-fine nano-powder technology continuously, comprise fresh feed pump, reactor, this reactor is furnished with jacketed type temperature control unit, whipping appts, feed-pipe, discharge nozzle and bleeder valve, it is characterized in that the nucleus that also comprises the arranged transversely that is connected with the bleeder valve of reactor becomes long tube, pipe is outer to be provided with the temperature control chuck, and nucleus becomes the outlet of long tube to communicate with the product receiving tank by material guiding pipe.
5. according to the specific equipment of claim 4, it is characterized in that nucleus becomes to be provided with mixing of materials mechanism in the long tube.
6. according to the specific equipment of claim 5, it is characterized in that said mixing of materials mechanism is a static mixer.
7. according to the specific equipment of claim 5, it is characterized in that said mixing of materials mechanism is a filler.
8. according to the specific equipment of claim 4, it is characterized in that reactor adopts two feed-pipes, and go deep into bottom to still.
9. according to the specific equipment of claim 4 or 5 or 6 or 7 or 8, it is characterized in that the product receiving tank is provided with the gas blow-down pipe.
10. according to the specific equipment of claim 9, it is characterized in that said fresh feed pump is a volume pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03113326 CN1206072C (en) | 2003-04-29 | 2003-04-29 | Process for continuously preparing superfine nano powder by precipitation method and special equipment thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03113326 CN1206072C (en) | 2003-04-29 | 2003-04-29 | Process for continuously preparing superfine nano powder by precipitation method and special equipment thereof |
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| CN1446654A CN1446654A (en) | 2003-10-08 |
| CN1206072C true CN1206072C (en) | 2005-06-15 |
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| CN 03113326 Expired - Lifetime CN1206072C (en) | 2003-04-29 | 2003-04-29 | Process for continuously preparing superfine nano powder by precipitation method and special equipment thereof |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CZ296748B6 (en) * | 2004-03-10 | 2006-06-14 | Univerzita Palackého | Process for preparing amorphous ferric oxide |
| CN102153114B (en) * | 2011-05-31 | 2013-04-10 | 营口沃科瑞科技有限公司 | Reaction system and method for preparing nano magnesium hydroxide |
| CN107349892B (en) * | 2017-08-02 | 2019-11-19 | 四川金象赛瑞化工股份有限公司 | A kind of gas-solid-liquid phase reaction production method |
| CN113213520A (en) * | 2021-05-10 | 2021-08-06 | 清华大学 | Method and system for continuously preparing nano barium sulfate |
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