CN1332749C - Nano powder preparation method and reactor - Google Patents
Nano powder preparation method and reactor Download PDFInfo
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- CN1332749C CN1332749C CNB2004100869988A CN200410086998A CN1332749C CN 1332749 C CN1332749 C CN 1332749C CN B2004100869988 A CNB2004100869988 A CN B2004100869988A CN 200410086998 A CN200410086998 A CN 200410086998A CN 1332749 C CN1332749 C CN 1332749C
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Abstract
The present invention relates to a method for preparing nanometer powder and a nanometer powder reactor. The nanometer powder reactor of the present invention comprises a cabin body with a microemulsion region and a reaction region, an inner baffle plate dividing the microemulsion zone into a plurality of sub-regions, at least one porous component arranged on the inner baffle plate, a first feed inlet for conveying first solution to one of the sub-regions, a second feed inlet for conveying second solution to the other sub-region and a third feed inlet for conveying third solution to a plurality of sub-regions, wherein the inner baffle plate can rotate along a rotary shaft to generate supergravity in the radial direction of the reactor, and the injected solution can move to the outer diameter from the center of the reactor. The porous component is respectively mixed with the first solution, the second solution and the third solution to form a first microemulsion cell and a second microemulsion cell, and the first microemulsion cell can react with the second microemulsion cell in the reaction region to be prepared into the nanometer powder.
Description
Technical field
The invention relates to a kind of preparation method and nano-powder reactor of nano-powder, particularly about a kind of preparation method and nano-powder reactor that does not use the hypergravity micro emulsion born of the same parents nano-powder of emulsifying agent.
Background technology
Ultramicro powders such as organic compound, inorganic compound, metal oxide and composite particles have very superior performance, have been widely used in technical fields such as microelectronics, information, space flight, chemical industry, machinery, automobile and biology.At present the preparation method of ultramicro powder can be divided into two kinds of physics method and chemical methods, and being most widely used with the normal gravitational field precipitation method in the chemical method.The precipitation method are generally done precipitation reaction in tank diameter or stirred tank reactor, exist following shortcoming in actual applications: the size distribution of (1) particle is inhomogeneous, and is difficult to control; (2) repeated relatively poor between batch (batch) and batch products; (3) mass transfer efficiency is slow, thereby the required reaction time is long, energy consumption is big and production efficiency is low.The origin cause of formation that canvasses above-mentioned shortcoming mainly is that the interior microcosmic of reactor mixes inhomogeneous and micro-quality transmits undesirable.
In recent years, the rotating bed super gravity field technology is applied to prepare the problem that ultramicro powder has solved many normal gravitational field precipitation method effectively.The rotating bed super gravity field technology can be strengthened the quality transmission procedure significantly, thereby needs tens meters high reaction towers can use about about two meters rotation to replace originally.Application in separation programs such as absorption, parsing, distillation also has splendid effect.
People such as the Ramshaw of ICI company in 1981 and Mallinson are in U.S. Pat 4,283, disclose the RPB technology No. 255, and its gas access is the bottom that is arranged at reactor.People such as nineteen eighty-three Ramshaw and Mallinson are in U.S. Pat 4,400, disclose improvement technology No. 275, and it is that the outside that the gas access is modified to by the rotation drum is entered.The Wen of nineteen eighty-three ICI company is in U.S. Pat 4, disclose another improving technology 382, No. 900, it is that the mesh support screen that is positioned at the rotary container outside is originally partly changed into airtight baffle plate, make gas only can pass through the part area, liquid then flows out from the remainder area.Nineteen eighty-three Wen is in U.S. Pat 4,382, discloses another improving technology No. 045, and it is to install a baffle plate additional at fixed space.When liquid flows out the rotary container outside, meet baffle plate, flow out fixed space along passage, thereby can reduce the time of liquid holdup at fixed space along direction of rotation.
Beijing University of Chemical Technology in 1996 is old to be built people such as peak and discloses the hypergravity legal system in Chinese patent CN1116185A number and be equipped with the aluminium hydroxide micro powder technology, it is the carburizing reagent of originally carrying out in reactor to be changed in the hypergravity reaction unit force carburizing reagent, to shorten the carburizing reagent time, and make the particle superfineization, particle diameter can be controlled between 10 to 100 nanometers, and particle diameter is evenly distributed.2000 old builds people such as peak and discloses the hypergravity legal system in Chinese patent CN1258639A number and be equipped with the aluminium hydroxide micro powder technology, and its processing procedure comprises carbon and divides and decompose and hydrothermal treatment consists two parts.After the process hydrothermal treatment consists, the particle diameter of micro mist can be controlled between 1 to 5 nanometer, and the draw ratio of acicular crystal is between 5 to 100.People such as calendar year 2001 Chen Jianfeng are in Chinese patent CN1288856A number announcement hypergravity legal system prepared silicon dioxide micropowder technology, and it uses the hypergravity reaction unit to shorten the carbonization time of waterglass effectively, can obtain the fine silica powder of particle diameter between 15 to 30 nanometers.
This case inventor in 2002 executes people such as Tiggo in TaiWan, China patent TW205722 number and disclose high shear high-eddy nano-powder manufacturing installation for Chinese patent CNZL02254967.5 number, and microcosmic mixing efficiency of its preparation ferric oxide nano powder is higher than traditional rotating packed bed reactor significantly.
Hypergravity synthesis of nano powder still is a kind of improvement of the traditional reactor precipitation method, distributes though have preferable particle diameter, still has many difficulties when being applied to prepare the superfine nano powder below 20 nanometers.In addition, utilize emulsifying agent (surfactant) to produce micro emulsion born of the same parents (micell) technology of inclusive reaction thing at present, though can prepare the following nano-powder of 20 nanometers, yet, this technology is subject to can only use extremely low reactant concentration, thereby productive rate is quite low, is not suitable for a large amount of fast production.
Summary of the invention
Main purpose of the present invention provides a kind of preparation method and nano-powder reactor that does not use the hypergravity micro emulsion born of the same parents nano-powder of emulsifying agent.
For achieving the above object, the present invention has disclosed a kind of hypergravity micro emulsion born of the same parents nano-powder reactor that does not use emulsifying agent.This nano-powder reactor comprises: a cabin body comprises a microemulsified district and a reaction zone; At least one internal partition, separating described microemulsified district is several sub-regions, and this internal partition rotates along a rotating shaft; At least one first porous member and at least one second porous member are arranged at different sub-regions respectively; One first charging aperture is in order to carry one first solution to the sub-region with first porous member; One second charging aperture is in order to carry one second solution to the sub-region with second porous member; One the 3rd charging aperture is in order to carry one the 3rd solution respectively to the above-mentioned sub-region that has the sub-region of the first porous member and have the second porous member.
First solution and second solution are water-soluble, are insoluble to the 3rd solution that is oiliness in fact.
Described internal partition is the plectane with central openings, can rotate along a rotating shaft that is arranged at the center of this nano-powder reactor.Can move to external diameter by the center of nano-powder reactor to order about the solution that injects from first charging aperture, second charging aperture and the 3rd charging aperture at the radially generation hypergravity of nano-reactor by the rotation internal partition.In addition, the porous member can bounce and cut apart and mix first solution and the 3rd solution forming first micro emulsion born of the same parents that are uniformly distributed in the 3rd solution, and bounces and cut apart and mix second solution and the 3rd solution to form second micro emulsion born of the same parents that are uniformly distributed in the 3rd solution.The first micro emulsion born of the same parents and the second micro emulsion born of the same parents bounce by the porous member that is arranged at reaction zone and mix and prepare nano-powder to react.
On the other hand, the present invention also provides a kind of preparation method of nano-powder, and it comprises the following step: utilize one first porous member to mix first solution and the 3rd solution to form the first micro emulsion born of the same parents, this first solution contains first reactant; Utilize one second porous member to mix second solution and the 3rd solution to form the second micro emulsion born of the same parents, this second solution contains one second reactant; Mix the first micropore born of the same parents and the second micropore born of the same parents,, use the described nano-powder of preparation so that first reactant contacts second reactant.
Compared with prior art, hypergravity micro emulsion born of the same parents technology of the present invention need not use emulsifying agent can form the micro emulsion born of the same parents, and therefore the reactant that can use high concentration is suitable for a large amount of fast nano-powders of producing to improve productive rate significantly.Moreover, owing to do not use emulsifying agent, the reaction solution of finishing reaction via filter take out nano-powder after, recyclable water and the oil phase solvent of utilizing again.In addition, the average grain diameter of the nano-powder of the present invention's preparation is less, and the particle diameter distributed area is narrower.
Description of drawings
Fig. 1 is the schematic diagram of the nano-powder reactor of first embodiment of the invention;
Fig. 2 show Fig. 1 the nano-powder reactor the part assembly on look schematic diagram;
Fig. 3 is the response procedures schematic diagram of nano-powder reactor of the present invention;
Fig. 4 and Fig. 5 are the nano-powder reactor schematic diagram of second embodiment of the invention;
Fig. 6 (a) is the x-ray diffraction pattern of the zinc oxide nano-powder of hypergravity micro emulsion born of the same parents technology preparation of the present invention;
Fig. 6 (b) is the x-ray diffraction pattern of the zinc oxide nano-powder of traditional hypergravity precipitation method preparation;
Fig. 7 (a) is the dynamic light scattering nanometer particle size analysis chart of the zinc oxide nano-powder of hypergravity micro emulsion born of the same parents technology preparation of the present invention;
Fig. 7 (b) is the dynamic light scattering nanometer particle size analysis chart of the zinc oxide nano-powder of traditional hypergravity precipitation method preparation.
Primary clustering symbol description among the figure:
10 nano-powder reactors, 100 nano-powder reactors, 110 external partitions
16 rotating shafts of 112 the 3rd porous members, 12 cabin bodies, 14 internal partitions
23 lower plates, 24 sub-regions, 21 upper plates, 22 sub-regions, 20 microemulsified district
30 reaction zones, 31 upper plates, 32 discharging openings, 33 lower plates, 42 first charging apertures
44 second charging aperture 46A the 3rd charging aperture 46B the 3rd charging aperture
50 first porous members, 52 second porous members, 72 first solution
73 first reactants, 74 second solution, 75 second reactants 76 the 3rd solution
82 first micro emulsion born of the same parents, 84 second micro emulsion born of the same parents, 86 nano-powders
The specific embodiment
In the precipitated crystal course of reaction, the one-tenth nuclear reaction of crystal is the sequence competitive reaction with long brilliant reaction, i.e. the crystal of certain degree degree of supersaturation when reaction takes place.Become this moment nuclear reaction to begin to take place, and after becoming the nuclear reaction initiation, long brilliant reaction also begin simultaneously in succession.Become the speed of nuclear reaction faster, the reactant that is consumed also just the more and can be also just low for the reaction starting material concentration of long brilliant reaction.Under the principle of competitive reaction, suppress the size that long brilliant reaction also just can suppress the finished product crystal simultaneously, the preparation of reaching ultra-fine particles.
The means that suppress long brilliant reaction comprise strengthen microcosmic mixes in the reaction unit degree so that most reactant the very first time promptly by the nucleation reaction consumes, do not grow brilliant reaction and there is unnecessary reactant.Mode of another control crystal size on how much long brilliant environment of combinations body that exceeds, general microemulsion processing procedure commonly used just is to use this kind mode, and it is controlled in crystal in the formed microresponse device of micro emulsion drop, the size of the crystal of growing up with restriction.
The microemulsified reaction technology is one of numerous methods that prepare nano-powder, and the reaction environment limiting crystal that it provides is reflected in the micro emulsion born of the same parents less than micron and carries out.Specifically, in microemulsion, the micro emulsion particle that small " pond " is surrounded as for monolayer that surfactant and cosurfactant constituted, between tens nanometers, these small " ponds " separated from one another promptly are " microreactors " that reacts to its size several.Because " microreactor " has very big interface, help chemical reaction, so product has good uniform particles degree with dispersed.Yet,, therefore have the lower shortcoming of productive rate because the content of nano-powder is to be subject to the shared liquid fraction of micro emulsion born of the same parents in the liquid.Moreover for the sediment of avoiding aqueous phase take place to be reunited thereby can't effectively be improved concentration of reactants, and the emulsifying agent that uses also can produce the not tractable emulsifying agent waste water that contains except meeting influences the purity of product.
The hypergravity micro emulsion born of the same parents nano-powder reactor 10 of Fig. 1 and Fig. 2 example first embodiment of the invention, wherein Fig. 2 top view of the part assembly of this nano-powder reactor 10 of example only.As shown in Figure 1, this nano-powder reactor 10 comprises a cabin body 12 with a microemulsified district 20 and a reaction zone 30, one separation microemulsified district 20 is the internal partition 14 of several sub-regions 22 and 24, several are arranged at the first porous member 50 of sub-region 22 (being internal partition 14 upper surfaces), several are arranged at the second porous member 52 of sub-region 24 (being internal partition 14 lower surfaces), several are arranged at the 3rd porous member 54 of reaction zone 30, one be used to carry one first solution 72 to the sub-region 22 first charging aperture 42, one in order to carry one second solution 74 to the sub-region 24 second charging aperture 44 and can carry three charging aperture 46A and the 46B of one the 3rd solution 76 to several sub-regions 22 and 24.
Specifically, reaction zone 30 is to be made of a upper plate 31 and a lower plate 33, and microemulsified district 20 is made of a upper plate 21 and a lower plate 23, and the internal partition 14 that is arranged at 23 of upper plate 21 and lower plates then is separated into two sub-regions 22 and 24 with this microemulsified district 20.In addition, the first porous member 50, the second porous member 52 and the 3rd porous member 54 can be porous rotating vane or the screen cloth filler with several perforates, in order to increase the mixed effect of reaction solution.
Can move to external diameter by the center of nano-reactor 10 with the solution that orders about from first charging aperture 42, second charging aperture 44 and the 3rd charging aperture 46A and 46B ejection at the radially generation hypergravity of nano-reactor 10 by rotation internal partition 14.In addition, the first porous member 50 can bounce and cut apart and mix first solution 72 and the 3rd solution 76 and be uniformly distributed in the first micro emulsion born of the same parents, 82, the second porous members 52 in the 3rd solution 76 and then bounce and cut apart and mix second solution 74 and the 3rd solution 76 to form second micro emulsion born of the same parents 84 that are uniformly distributed in the 3rd solution 76 to form one.
Afterwards, the first micro emulsion born of the same parents 82 and the second micro emulsion born of the same parents 84 are driven by hypergravity and self-emulsifying microemulsion district 20 moves to reaction zone 30.Originally the first micro emulsion born of the same parents 82 and the second micro emulsion born of the same parents 84 that separated by internal partition 14 fully mix via the 3rd porous member 54 when entering reaction zone 30, thereby interior second reactant 75 of first reactant 73 in the first micro emulsion born of the same parents 82 and the second micro emulsion born of the same parents 84 can contact and carries out chemical reaction with formation nano-powder 86 at reaction zone 30.Hence one can see that, and the response procedures of nano-powder reactor 10 can be considered first micro emulsion born of the same parents 82 of parallel connection and the second micro emulsion born of the same parents' 84 one-tenth shaped reaction, the one-tenth shaped reaction of the nano-powder 86 of connecting again, as shown in Figure 3.
Because second reactant 75 that first reactant 73 that includes of the first micro emulsion born of the same parents 82 and the second micro emulsion born of the same parents 84 include is because of after the exhausting of chemical reaction, chemical reaction i.e. reactant and stopping for want of, therefore the size of nano-powder 86 can not continue to increase, but is subject to reactant content and time of contact that the first micro emulsion born of the same parents 82 and the second micro emulsion born of the same parents 84 include.
The hypergravity micro emulsion born of the same parents nano-powder reactor 100 of Fig. 4 and Fig. 5 example second embodiment of the invention.Compare with the nano-powder reactor 10 that only has an internal partition 14 among Fig. 1, middle nano-powder reactor 100 embodiment illustrated in fig. 4 has two internal partitions 14 and also comprises an external partition 110 in addition.This external partition 110 is to be arranged at reaction zone 30, and it highly is between two internal partitions 14, therefore the second micro emulsion born of the same parents 84 of described sub-region 24 are divided into two parts by external partition 110 when entering reaction zone 30, mix order with the first micro emulsion born of the same parents 82 from sub-region 22 equably by the 3rd porous member 54 respectively.Like this, first reactant 73 that includes of the first micro emulsion born of the same parents 82 and the second micro emulsion born of the same parents 84 and second reactant 75 can contact to carry out chemical reaction and generate nano-powder 86.
Fig. 6 (a) is the x-ray diffraction pattern of zinc oxide (ZnO) nano-powder of hypergravity micro emulsion born of the same parents technology preparation of the present invention, and Fig. 6 (b) is the x-ray diffraction pattern of the zinc oxide nano-powder of traditional hypergravity precipitation method preparation.The present invention utilizes Fig. 4 and nano-powder reactor 100 preparation Zinc oxide powders shown in Figure 5, wherein the radical length of internal partition 14 is 30 millimeters (rotating speed 3500rpm), the radical length of external partition 110 is about 60 millimeters (rotating speed 2500rpm), the first porous member 50 and the second porous member 52 are to be made of highly about 20 a millimeters porous screen cloth filler, and the 3rd porous member 112 then constitutes with 36 porous rotating vanes (mesh is 60).
First solution 72 is that concentration is the zinc sulfate (ZnSO of 0.2M
4) solution, second solution 74 is that concentration is NaOH (Na0H) solution of 0.5M, the 3rd solution 76 then adopts n-hexane.When reacting, first charging aperture 42 injects sub-region 22, the second charging apertures 44 with 0.18 liter/minute flow rate with solution of zinc sulfate and with 0.2 liter/minute flow rate sodium hydroxide solution is injected sub-region 24.The product that takes out from discharging opening 32 is zinc hydroxide Zn (0H)
2, it is dissolved in the ethylene glycol, and can obtains zinc oxide nano-powder in about 3 hours with 150 ℃ of heating.Can calculate that the size of the nano-powder of hypergravity micro-emulsion technology preparation of the present invention is about 19 nanometers by x-ray diffraction pattern according to the Scherrer equation, the size of the nano-powder of traditional hypergravity precipitation method preparation then is about 28 nanometers.Hence one can see that, and hypergravity micro-emulsion technology of the present invention can prepare the nano-powder of powder size less than 20 nanometers.
Fig. 7 (a) is dynamic light scattering (the dynamic light scattering of the zinc oxide nano-powder of hypergravity micro emulsion born of the same parents technology preparation of the present invention, DLS) nanometer particle size analysis chart, Fig. 7 (b) are the dynamic light scattering nanometer particle size analysis charts of the zinc oxide nano-powder of traditional hypergravity precipitation method preparation.As shown in the figure, the flat footpath particle diameter of the zinc oxide nano-powder of hypergravity micro emulsion born of the same parents technology preparation of the present invention is 36.4 nanometers, and particle diameter is distributed in the interval of 20 to 100 nanometers.Relatively, the flat footpath grain of the zinc oxide nano-powder of traditional hypergravity precipitation method preparation then is 105 nanometers, and particle diameter is distributed in the interval of 25 to 250 nanometers.Hence one can see that, and the average grain diameter of the nano-powder of hypergravity micro-emulsion technology preparation of the present invention is less, and the particle diameter distributed area is narrower.
Compared with prior art, hypergravity micro emulsion born of the same parents technology of the present invention has following characteristics:
1. the present invention need not use emulsifying agent can form the micro emulsion born of the same parents, and the reactant that can use high concentration is suitable for a large amount of fast nano-powders of producing to promote productive rate significantly.
2. owing to do not use emulsifying agent, the reaction solution of finishing reaction via filter take out nano-powder after, recyclable water and the oil phase solvent of utilizing again.
3. the average grain diameter of the nano-powder of the present invention's preparation is less, and the particle diameter distributed area is narrower.
Above embodiment only is explanation principle of the present invention and function, and unrestricted the present invention.Therefore those skilled in the art's modification and variation without prejudice to spirit of the present invention that the foregoing description is made still contained by the present invention.Protection scope of the present invention is as the criterion with claim.
Claims (15)
1. nano-powder reactor is characterized in that comprising:
One cabin body comprises a microemulsified district and a reaction zone;
At least one internal partition, separating described microemulsified district is several sub-regions, and this internal partition rotates along a rotating shaft;
At least one first porous member and at least one second porous member are arranged at different sub-regions respectively;
One first charging aperture is in order to carry one first solution to the sub-region with first porous member;
One second charging aperture is in order to carry one second solution to the sub-region with second porous member;
One the 3rd charging aperture, week is to carry one the 3rd solution respectively to the above-mentioned sub-region that has the sub-region of the first porous member and have the second porous member.
2. nano-powder reactor as claimed in claim 1 is characterized in that the described first porous member is the upper surface that is arranged at internal partition, and the described second porous member is the lower surface that is arranged at described internal partition.
3. nano-powder reactor as claimed in claim 1 is characterized in that it comprises two internal partitions that are arranged at the microemulsified district, and also comprises an external partition and at least one the 3rd a porous member that is arranged at reaction zone that is arranged at reaction zone.
4. nano-powder reactor as claimed in claim 3, the height that it is characterized in that the installation site of described external partition are between described two internal partitions.
5. nano-powder reactor as claimed in claim 3 it is characterized in that described internal partition and external partition are in the form of a ring, and this internal partition is to be arranged in the external partition.
6. nano-powder reactor as claimed in claim 5 is characterized in that described internal partition and external partition are to rotate in the same way along a rotating shaft.
7. nano-powder reactor as claimed in claim 5 is characterized in that described internal partition and external partition are along a rotating shaft reverse rotation.
8. nano-powder reactor as claimed in claim 1 is characterized in that described first charging aperture, second charging aperture and the 3rd charging aperture are the centers that is positioned at internal partition.
9. nano-powder reactor as claimed in claim 1 is characterized in that it also comprises a discharging opening that is connected in described reaction zone.
10. the preparation method of a nano-powder is characterized in that this method carries out, and comprises the following step in the described nano-powder reactor of claim 1:
Utilize one first porous member to mix first solution and the 3rd solution to form the first micro emulsion born of the same parents, this first solution contains first reactant;
Utilize one second porous member to mix second solution and the 3rd solution to form the second micro emulsion born of the same parents, this second solution contains one second reactant;
Mix the first micropore born of the same parents and the second micropore born of the same parents,, use the described nano-powder of preparation so that first reactant contacts second reactant.
11. the preparation method of nano-powder as claimed in claim 10 is characterized in that described first solution and second solution are insoluble to the 3rd solution.
12. the preparation method of nano-powder as claimed in claim 10, it is characterized in that the described first porous member is to mix first solution and the 3rd solution by rotation with cutting, and the second porous member is to mix second solution and the 3rd solution by rotation with cutting.
13. being the 3rd porous members by a rotation, the preparation method of nano-powder as claimed in claim 12, the step that it is characterized in that mixing the first micropore born of the same parents and the second micropore born of the same parents carry out.
14. the preparation method of nano-powder as claimed in claim 13 is characterized in that the direction of rotation of described the 3rd porous member is opposite with the direction of rotation of the first porous member.
15. the preparation method of nano-powder as claimed in claim 13 is characterized in that the direction of rotation of described the 3rd porous member is identical with the direction of rotation of the first porous member.
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| CN100434151C (en) * | 2006-06-19 | 2008-11-19 | 西安交通大学 | Preparation of emulsion for decreasing liquid-drop diameter continuouslly and gradually by porous film |
| CN101574632B (en) * | 2008-05-09 | 2011-07-13 | 北京化工大学 | Preparation method of cod-liver oil emulsion |
| GB0909154D0 (en) | 2008-09-25 | 2009-07-08 | Nanomaterials Tech Pte Ltd | A process for making particles for delivery of drug nanoparticles |
| CN103801242B (en) | 2012-11-03 | 2015-12-02 | 中国石油化工股份有限公司 | Reactor and the alkylation reaction method utilizing this reactor |
| CN103041722B (en) * | 2012-12-08 | 2015-07-01 | 中北大学 | Supergravity device for rapidly dissolving water-soluble polymers |
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