TWI374772B - Apparatus and method for synthesis of nano particles - Google Patents

Description

1374772 October 21, 100. Inventive Note: [Technical Field] [0001] The present invention relates to a nano-powder synthesis apparatus and method, and more particularly to a nano-powder for preparing nano-powder by chemical synthesis Synthetic device and method. [Prior Art] [0002] Nanomaterials can be roughly classified into nano powder, nano fiber, nano film and nano block by type, in which nano film and nano block are derived from nano powder. Therefore, the preparation of nano powder is quite important. The preparation method of the nano powder can be roughly divided into two physical and chemical preparation methods. Chemical preparation methods can be generally divided into: chemical vapor deposition, Sol-Gel, Microemulsion, polymer grafting, Chemical Precipitation, hydrothermal synthesis. (Hydro-Thermal), arc plasma method, sonochemical method, etc. [0003] The chemical immersion method is a major chemical method for preparing nanometer powder, which has the characteristics of simple operation, short process and low cost. The chemical precipitation method is generally carried out by adding a suitable precipitant to the solution to obtain a precipitate, which is subjected to filtration, washing, drying and calcination to obtain a nanopowder. According to the different precipitation methods, it can be divided into direct precipitation method, coprecipitation method and the like. The direct precipitation method is a method for preparing oxide nano particles directly from a solution by a precipitation operation; the coprecipitation method is to add a precipitant to a mixed salt solution of a plurality of metal ions, and the components are mixed and precipitated, which is commonly used for preparation. Multi-component or doped. The removal of the 〃丨 'chemical separation method to prepare the nano-powder-like system is completed in a tank or a mixer tank reactor. However, the chemical precipitation reaction is generally fast between ions 094133120 Form No. A0101 Page 4 / Total 15 Page 1374772 r · 1100. October 21 Modified replacement f-speed reaction, short reaction time, in a stirred tank or stirred dad reactor The reactants are not uniformly mixed in the micro liquid-liquid, which tends to cause the local concentration of the precipitate formed by the reaction to be too high to cause aggregation, thereby causing the nanometer powder to have a large particle size and a low utilization rate of the reactants. In view of the above, it is necessary to provide a nano-powder synthesizing apparatus and method which can obtain a nano-powder having an ultrafine particle size and which has a high utilization ratio of reactants. SUMMARY OF THE INVENTION [0006] Hereinafter, a nano-powder synthesizing apparatus and method for obtaining a nano-powder having an ultrafine particle size and having a high reactant utilization rate will be described by way of specific examples. [0007] A nano-powder synthesis device comprising: [0008] a reaction chamber comprising a top portion, a bottom portion and a side wall, the reaction chamber having a trapezoidal cross section and a top surface area larger than a bottom portion, the bottom portion being provided a liquid outlet; [0009] a first atomizer disposed on the sidewall; [0010] a second atomizer disposed at the top or bottom; and [0011] a centrifuge, and the outlet The liquid ports are connected. [0012] A method for synthesizing a nano powder, comprising the steps of: [0013] providing a nano-powder synthesis device; [0014] spraying the reaction chamber with a first atomizer and a second atomizer Entering at least two reactants for chemical reaction; 094133120 Form No. A0101 Page 5 of 15 Page 1003389922-0 [0015] [0015] 1374772

On October 21, 10.0, a solvent was injected into the reaction chamber according to the positive key, and the unreacted reactants and the products formed by the reactants were flushed into the centrifuge; [0016] The centrifuge was started. The reactants entering the centrifuge are chemically reacted, and the precipitate is separated by the centrifuge to obtain nano powder.

[0017] Compared with the prior art, the nanoparticle synthesis device and method, by means of the atomizer, enable the atomized reactants to collide with each other at high speed in the reaction chamber to fully mix and react; By means of the setting of the centrifuge, the reactants can be sufficiently reacted again and the precipitates can be separated; further, the nanometer powder having an ultrafine particle size can be obtained, and the reactant utilization rate is high. [Embodiment] [0018] The present invention will be described below. The examples are further described in detail. Referring to the first figure, a nano-powder synthesizing device 20 provided in an embodiment of the present invention includes a reaction chamber 22; and a centrifuge 24 connected to the reaction chamber 22. [0020] The reaction chamber 22 has a first sidewall 220 and a second sidewall 223 opposite to the first sidewall 220, a top portion 224, a bottom portion 227, a liquid inlet port 222, and a liquid at the bottom portion 227. Port 229. The cross section of the reaction chamber 22 is trapezoidal, and the area of the top portion 224 is larger than the area of the bottom portion 227. The first side wall 220 and the second side wall 223 are both inclined surfaces. The beveled surface of the first side wall 220 and the second side wall 223 facilitates a portion of the reactants and products in the reaction chamber 22 to flow to the liquid outlet 229, thereby facilitating product collection. The liquid inlet 222 is located at the top 224 of the reaction chamber 22 and is disposed adjacent to the top portion 224 of the reaction chamber 22 adjacent to the first side wall 220 and the second side wall 223; this arrangement facilitates the injection of liquid through the liquid inlet 222 Can fully flush the first side wall 220 and the 094133120 Form No. A0101 Page 6 / Total 15 Page 1003389922-0 1374772 r 100 years. On October 21, the shuttle is replacing the side wall 223 of the page. The inlet port 222 can be provided with a valve 221. The reaction chamber 22 may be an inverted cone or a truncated cone shape; preferably, the reaction chamber 22 is an inverted conical or truncated cone shape; in this embodiment, the reaction chamber is an inverted truncated cone shape. The liquid outlet 229 is used for the outflow of a portion of the reactants and products within the reaction chamber 22, which may be provided with a valve 229. [0021] The first side wall 220 and the second side wall 223 of the reaction chamber 22 are respectively provided with fog.

The chemist 25 and the atomizer 27. The atomizer 25 and the atomizer 27 have a plurality of nanometer (less than 1 micrometer) orifices, and the reactor chamber 22 can be sprayed with a high pressure atomized nanometer powder synthesis reactant; preferably, the orifice size Adjustable. The atomizer 25 and the atomizer 27 can be sprayed with the same reactants or can be sprayed with different reactants; the specific conditions can be determined according to the actual needs. The atomizers 25 and 27 can be externally coupled to a pump to replenish the atomizers 25 and 27 with pressurized reactants. [0022] An atomizer 26 and an atomizer 28 are disposed at the top and bottom of the reaction chamber 22, respectively. The atomizer 26 and the atomizer 28 have a plurality of nano-stage orifices, which can inject a high-pressure atomized nano-powder synthesis reaction with another reactant, and the reactants and the atomizer 25 and The reactant injected into the atomizer 27 is subjected to a high-speed impact reaction to synthesize a nanometer powder or a precursor of the nano powder. The atomizer 26 and the atomizer 28 can be sprayed with the same reactants, or can be sprayed with different reactants; the specific conditions can be determined according to the actual needs. The atomizers 26 and 28 can be externally coupled to a pump to supplement the atomizers 26 and 28 with pressurized reactants. Moreover, the atomizer 28 is arranged to spray the reactants from the bottom to the top, which is advantageous for increasing the reaction time of each reactant and allowing the respective reactants to fully react, thereby further enhancing the utilization rate of each reactant. 094133120 Form No. A0101 Page 7 of 15 1003389922-0 1374772 [0023] [0025] 100 years. October 21st, the shuttle is a private page. In addition, in order to facilitate precise control of the flow rate of each reactant, Each reactant is fully reacted; a flow controller can be added between the atomizers 25, 26, 27 and 28 and their respective pumps. The centrifuge 24 is coupled to the liquid outlet 229 of the reaction chamber 22, which can be used to re-react completely into the reactants entering the centrifuge 24 to increase the utilization of the reactants. Since the centrifuge 24 has a solid-liquid phase separation effect, it can also separate the precipitate located therein to obtain a precursor of the nano powder or the nano powder. The centrifuge 24 can be selected from a high speed centrifuge or an ultra high speed centrifuge. The bottom of the centrifuge 24 can be provided with a liquid outlet 242 for the outflow of liquid. The liquid outlet 242 can further be provided with a valve. The working process of the nano-powder synthesizing device 20 provided in this embodiment is as follows. [0026] (1) The atomizers 25, 26, 27 and 28 of the reaction chamber 22 are respectively connected. A pump (not shown) is pumped through the pump to the atomizers 25, 26, 27 and 28 and atomized into the reaction chamber 22 via atomizers 25, 26, 27 and 28. The size of the mist particles injected into the reaction chamber 22 is generally set to be less than 0.2 μm. Within the reaction chamber 22, the reactants are intensively mixed and reacted at high velocity, which will produce the first product. At least two of the reactants are introduced into the reaction chamber 22 via the atomizers 25, 26, 27 and 28.

(2) The solvent for washing is injected into the liquid inlet 222 of the reaction chamber 22, and the unreacted reactant and the product of the reactant in the reaction chamber are flushed into the centrifuge 24. The solvent for the soaking may be a water-soluble solvent (including water, and an organic solvent which is completely compatible with water, such as ethanol) or an oil-soluble solvent (e.g., acetone 'ether, trichlorodecane, ethyl acetate, etc.). The injection into the liquid inlet 222 094133120 Form No. A0101 Page 8 of 15 1003389922-0 1374772 [0028]

[0029]

[0031] The solvent for washing in the middle of 1100 can be sufficiently flushed through the first side wall 22〇 and the second side wall 22316 of the reaction chamber 22 to the unreacted reactant and the first product in the reaction chamber, and It is introduced into the centrifuge via the liquid outlet 229. The solvent for washing into the liquid inlet 222 may be the same as the water-soluble solvent, or the same as the oil-soluble solvent, or the water-soluble solvent and the oil-soluble solvent, respectively; the specific type of the product may depend on the type of the product. (3) starting the centrifuge 24' to cause the reactants entering the centrifuge 24 to react again under the south speed of the centrifuge 24 to generate a second product, which is advantageous for the full utilization of the reactants; and, in centrifugation The solid-liquid two-phase substance can be separated by the centrifugal force of the machine 24, and the nano-powder or nano-powder precursor in the first product and the second product is deposited on the side wall of the centrifuge 24, and other liquid substances can be discharged. The liquid port 242 flows out. For the nano-powder precursor, subsequent calcination is required to obtain the desired nano-powder. The following is a specific example to illustrate the operation process of the nano-powder synthesizing device 2, see the first embodiment 'second embodiment and the third embodiment: the first embodiment for the synthesis of the metal nano-powder, the atomizer 25 and 27, an aqueous solution containing a certain concentration of Μω+ (wherein Μ represents a metal such as Ag, Au, m = 1, 2, or 3) is sprayed into the reaction chamber 22, and is sprayed into the reaction chamber 22 by the atomizers 26, 28. A certain concentration of an aqueous solution of bh4_(borohydride) ions. The above two solutions react in the reaction chamber 22: Mm++ BH/+H 0 - M + B(OH)3 + H2; which obtains the first product, which includes the metal nanopowder. Water is injected into the reaction chamber 22 via the liquid inlet port 222, and the first product of the first side wall 220 and the second side wall 223 of the reaction chamber 22 is 094133120. Form No. A0101 Page 9 of 15 1003389922-0 1374772

On October 21, 1100, the correction was made for the ^ I ' ΝΓ + ion and bh "" ions into the centrifuge 24. In the centrifuge 24 ' 4

The MlD+ ion and the BH-ion are reacted again (the reaction formula is the same as in the first reaction 4) to form a second product. This second product also includes metal nanopowder. During the second chemical reaction, the metal nano-powder will be deposited on the side wall of the centrifuge 24 due to the separation of the solid-liquid two-phase material of the centrifuge 24, and the liquid substance may flow out through the liquid outlet 242 of the centrifuge 24. . Thereafter, the centrifuge 24 is turned on to collect the metal nanopowder, and the particle size thereof may range from 5O to 150 nm. [0032] Second Embodiment 0 [0033] For the synthesis of metal oxide nanopowder such as titanium dioxide, a certain concentration of TiCl4 (titanium carbide) solution may be sprayed into the reaction chamber 22 by atomizers 25 and 27, by mist. The chemistries 26, 28 spray an excess of a certain concentration of aqueous ammonia into the reaction chamber 22. The above two solutions will react in the reaction chamber 22 and the centrifuge 24 to form the first product and the second product, respectively. Water can be used as a solvent for washing in this embodiment. Thereafter, a titanium dioxide nanopowder dried 'calcined precursor TiCOH' can be collected in the centrifuge 24. The particle size of the finally obtained titanium dioxide nanopowder may range from 20 to 60 nm. Third Embodiment [0035] For the synthesis of a multi-component nano-powder such as BaTi〇3 (barium titanate), a certain concentration of BaC12 (gasification enthalpy) can be sprayed into the reaction chamber 22 by the atomizer 25. The solution 'is sprayed into the reaction chamber 22 by the atomizer 27 into the TiCl4 (titanium tetrachloride) solution having the same concentration as the BaC12 solution, and the atomizers 25 and 27 spray the excess into the reaction chamber 22 to contain a certain concentration of C2〇42. - (oxalate ion) solution The above three solutions will react in the reaction chamber 22 and the centrifuge 24 094133120 Form compilation A0101 Page 10 / 15 pages 1003389922-0 1374772 100 years. October 21st replacement The page generates the first product and the second product, respectively. Water can be used as the solvent for washing in this embodiment. Thereafter, in the centrifuge 24, BaTi(R) 3 nanometer powder, BaTiO(C2〇4)2·4H2〇, which is dried and generally burned, can be collected. The particle size of the finally obtained BaTi 〇 nanometer powder may range from ό 30 to 80 nm. In the embodiment of the present invention, by the arrangement of the atomizers 25, 26, 27 and 28, the atomized reactant can be sprayed into the reaction chamber 22 to enable the reactant to be in the reaction chamber 22. The high-speed impact of each other to fully mix and react 'finally obtain the ultrafine particle size of the nano-powder β centrifuge 24, the reaction can be fully reacted again, which is conducive to the utilization of the reactants; The solid-liquid two-phase substance can be separated, and the nano powder or the nano powder precursor can be separated. In addition, the position of the atomizer 28 is set to 'react the reactants from bottom to top, thereby increasing the reaction time between the reactants' to achieve a more efficient impact reaction. In addition, it can be understood that only the top 224 of the reaction chamber 22 and the first side wall 220 are provided with an atomizer, or only the top portion 224 of the reaction chamber 22 and the first side wall 220 and the second side wall 223 are atomized. , or only the bottom 227 and the second side wall 223 of the reaction chamber 22, or only the bottom 227 of the reaction chamber 22 and the first side wall 220 and the second side wall 223 are provided with an atomizer, etc., all of which belong to the protection scope of the present invention. . [0038] Other skilled in the art can also make other variations within the spirit of the present invention. The number of inlet ports, the number and position of the atomizers are appropriately changed for use in the design of the present invention, etc. [0039] In summary, the present invention has indeed met the requirements of the invention patent, and is proposed according to law. 1003389922-0 094133120 Form No. Α0101 Page 11/Total 15 Page 1374772 October 21, 2001 Shuttle Replacement Page Patent Application. However, the above description is only the preferred embodiment of the present invention, and equivalent modifications or variations made by those skilled in the art of the present invention should be included in the following claims. BRIEF DESCRIPTION OF THE DRAWINGS [0040] The first drawing is a schematic view of a nanometer powder synthesis apparatus according to an embodiment of the present invention. [Main component symbol description] [0041] Nano powder synthesis device: 20 [0042] Valve: 221 [0043] Inlet: 222 [0044] Top: 224 [0045] Discharge port: 229, 242 [0046] Fog Chemist: 25, 26, 27, 28 [0047] Reaction chamber: 22 [0048] First side wall: 220 [0049] Second side wall: 223 [0050] Bottom: 227 [0051] Centrifuge: 24

1003389922-0 094133120 Form No. A0101 Page 12 of 15

Claims (1)

100 years. October 21 revision replacement page 1374772. VII. Patent application scope: 1. A nano powder synthesis device, comprising: a reaction chamber comprising a top portion, a bottom portion and a side wall, wherein the reaction chamber has a cross section Trapezoidal, and the top area is larger than the bottom area, the bottom is provided with a liquid outlet, the top is provided with two liquid inlets, and the two liquid inlets are located adjacent to the top and the side wall, and the liquid inlet is used for a first atomizer is disposed in the reaction chamber and is disposed on the sidewall and has a plurality of nanometer first orifices, and the first atomizer is configured to atomize the first reactant and pass through the first orifice Spraying the atomized first reactant into the reaction chamber; a second atomizer disposed at the top or bottom and having a plurality of nanometer second orifices, the second atomizer is used for atomization The second reactant is injected into the reaction chamber through the second injection hole to inject the atomized second reactant; and a centrifuge is connected to the liquid outlet. 2. The nano-powder synthesizing device according to claim 1, wherein the reaction chamber has an inverted cone or a truncated cone shape. 3. The nano-powder synthesizing device according to claim 2, wherein the reaction chamber is an inverted cone or a truncated cone shape. 4. The nano-powder synthesizing device according to claim 1, wherein the liquid inlet is provided with a valve. 5. The nano-powder synthesizing device according to claim 1, wherein the first atomizer and the second atomizing device are respectively connected with a pump. 6. The nano-powder synthesizing device according to claim 5, wherein a flow controller is disposed between the first atomizer and the second atomizer and the corresponding pump. 094133120 Form No. A0101 Page 13 of 15 1003389922-0 1374772 100. The first half of the invention is the nano-powder synthesizing device of claim 1, wherein the A valve is provided at the liquid port. 8. The nano-powder synthesizing device according to claim 1, wherein the centrifuge comprises a high-speed centrifuge and an ultra-high-speed centrifuge. 9. A method for synthesizing a nano powder comprising the steps of: providing a nano-powder synthesizing device according to claim 1; spraying the reaction chamber with a first atomizer and a second atomizer At least two reactants are subjected to a chemical reaction; a solvent is introduced into the reaction chamber through two inlet ports, and the unreacted reactant and the product formed by the reactant are injected into the reaction chamber through the liquid outlet The centrifuge; and starting the centrifuge to chemically react the reactants entering the centrifuge, and separating the precipitate by the centrifuge to obtain a nanometer powder. The method for synthesizing nano-powder according to claim 9, wherein the solvent is introduced through a liquid inlet provided at the top of the reaction chamber and located at a position adjacent to the side wall of the reaction chamber. The method for synthesizing nano powder according to claim 9, wherein the solvent comprises a water-soluble solvent and an oil-soluble solvent. The method for synthesizing nano-powder according to claim 11, wherein the water-soluble solvent is selected from the group consisting of water and ethanol. The method for synthesizing nano-powder according to claim 11, wherein the oil-soluble solvent is selected from the group consisting of acetone, diethyl ether, tri-methane, and ethyl acetate. The nano-powder synthesis method according to claim 9, wherein the nano-powder has a particle size ranging from 20 to 150 nm. 094133120 Form No. A0101 Page 14 of 15 1003389922-0