Reactor for producing ultra fine particles

The present invention relates to a reactor for producing ultra fine particles, particularly a reactor containing a plurality of porous rotors for producing ultra fine particles.

Ultra fine particles, e.g. metal oxides, organic compounds, inorganic compounds, and composite particles, can be used as new materials with high performance in microelectronics, information industry, aviation industry, chemical engineering, mechanical engineering, auto industry, bioengineering, etc. At present, the production of ultra fine particles can be classified into physical methods and chemical methods. Among the chemical methods, the precipitation method is the most common one, where a chemical precipitation reaction takes place in a stirring tank reactor or a mixing kettle reactor and in an ordinary gravitational field. The precipitation method has the following disadvantages: (1) non-uniform distribution of the particle sizes and difficult in controlling the particle size; (2) poor repeatability between batches of product; (3) slow mass transfer, long reaction time, large energy consumption, and low production efficiency. These disadvantages mainly are caused by non-uniform micro-mixing in the reactor, and poor micro-mass-transfer, etc.

U.S. Pat. No. 4,283,255 by Ramshaw, et at. (1981) disclose a technique for performing a mass transfer through a rotation pack bed. This technique is mainly used for the gas-liquid contact and the reaction thereof, wherein a pack bed rotating at a high speed is used to increase the liquid-gas mass-transfer efficiency. Similar rotation pack beds can also be found in U.S. Pat. Nos. 4,382,045; 4,382,900; and 4,400,275.

In 1996,Jiann-Feng Chen et al. disclosed (CN1116185A) an ultra-gravity method for preparing an ultra fine powder of calcium carbonate, wherein a carbonization reaction performing in a reaction vessel is improved by using an ultra-gravity reaction device. Said method reduces the carbonization time and enables the particles becoming ultra-fine, where the particle size can be controlled at 10˜100 nm with a uniform particle distribution.

In 2000, Jiann-Feng Chen et al. published (CN1258639A) a method for preparing an ultra fine powder of aluminum hydroxide by an ultra-gravity method, which comprises decomposing the carbon-containing compounds, and water-heating treatment. After the water-heating treatment, the particle size can be controlled at 1˜5 nm, and a needle-like crystal with an aspect ratio of 5˜100 can be obtained.

In 2001, Jiann-Feng Chen et al. published (CN1288856A) an ultra-gravity method for preparing an ultra fine powder of silicon dioxide, wherein an ultra-gravity reaction device is used to effectively reducing the carbonization time of water glass, thereby obtaining an ultra fine powder of silicon dioxide having a particle size of 15˜30 nm.

In 2001, Han et al. published a water-heating method for preparing an ultra fine powder of ferric oxide (U.S. Pat. No. 6,203,774), which comprises dissolving α-FeOOH in ethanol, and using a water-heating method together with a habit modifier to control the crystal pattern of the ferrous oxide obtained.

The use of an ultra-gravity device (rotation pack bed) has the following disadvantages: (1) non-uniform mass transfer efficiency, with the efficiency gradually decreasing towards the outer periphery of the rotation bed; (2) easy to form a situation where the density of the packing near the outer periphery is higher than that of the portion near the rotation axis due to the centrifugal force; (3) the rotation pack bed having a complicated structure such that the bed is liable in losing its dynamic balance and causing a frequent shut-down for maintenance.

A primary objective of the present invention is to provide a reactor for producing ultra fine particles, which is free of the abovementioned disadvantages.

Another objective of the present invention is to provide a reactor for producing ultra fine particles, which has an enhanced mixing efficiency.

A further objective of the present invention is to provide a method for preparing ultra fine particles.

FIG. 1 is a schematic cross-sectional view of a high-shear, high-vortex reactor according to a first preferred embodiment of the present invention;

FIG. 2 is a schematic top plan view of a part of the reactor in FIG. 1 .

FIG. 3 is a schematic top plan viewing a part of another high-shear, high-vortex reactor according to a second preferred embodiment of the present invention.

Legends:

10 . . . reaction chamber 1 . . . liquid inlet pipe 2 . . . perforation 3 . . . gas inlet 4 . . . external frame 5 . . . stainless steel screen 6 . . . rotation shaft 7 . . . reaction product outlet 8 . . . gas discharge pipe 20 , 20 ′, 20 ″, 20 a . . . porous rotors 30 . . . rotation table

In a conventional ultra-gravity device, the gas-liquid contact and mass transfer are mainly carried out at the liquid films on the surface of the packing of the rotation pack bed. The mass transfer rate in this device is mainly determined by the viscosity of the fluid, and the specific surface area of the packing, etc. The ultra-gravity device is an improvement over the ordinary pack bed reactor. The present invention now discloses a novel high-shear, high-vortex reaction device, which is mainly characterized in using a plurality of porous rotors. The novel high-shear, high-vortex reaction device according to the present invention uses the porous rotors rotating at a high speed to disperse the liquid flown out of the shaft into tiny liquid droplets, so that a liquid-gas mass transfer occurs on the surfaces of the tiny droplets. The liquid surface area per unit volume generated by the tiny droplets is far larger than that of the liquid films on the surface of the packing. Therefore, the mass transfer rate can be further increased. Further, the reactants required for the growth of crystal are confined in the tiny droplets, so that the crystallization reaction is terminated as soon as any one of the reactants contained therein is consumed, thereby controlling the crystal particles in the nanometer level.

In addition to being suitable for a gas-liquid contact reaction, the reaction device according to the present invention is also suitable for a liquid-liquid reaction.

During the precipitation crystallization reaction, the crystal nucleation reaction and the crystal growth reaction are competing with each other. That is, at the same time when the reaction takes place, a certain degree of super-saturation occurs. At this time, the nucleation reaction starts to take place. After the initiation of the nucleation reaction, the crystal growth reaction also starts to take place. The faster the nucleation reaction, the more reactants are being consumed, and the concentration of the starting material for crystal growth is lower. As a result of the competitive reactions, the crystal growth reaction is inhibited, as well as the size of the crystal product, thereby achieving the production of ultra fine particles.

One way of achieving the aforesaid result includes reinforcing the degree of micro-mixing in the reaction device such that a majority of reactants are consumed by the nucleation reaction in a first place without excessive amounts o reactants for the crystal growth reaction.

The novel high-shear, high-vortex reaction device according to the present invention can achieve the aforesaid result using a physical means. In addition to increasing the micro-mixing efficiency, the repetitively cutting of the fine droplets by the rotating porous rotors also has the spatial effects of increasing the degree of micro-mixing and inhibiting the crystal growth reaction. Therefore, in comparison with the conventional ultra-gravity reaction device, the present invention not only improves the degree of micro-mixing, but also diminishes the defect that the packing material of the conventional ultra-gravity reaction device is vulnerable to rotation. Further, the tiny droplets formed in the reactor have the function as a minute reactor same as that in the conventional micro-emulsion process, thereby achieving a better control on the particle size and particle distribution of the crystals.

FIGS. 1 and 2 show a high-shear, high-vortex reactor according to a first preferred embodiment of the present invention, wherein FIG. 2 shows the top plan view of a part of the reactor shown in FIG. 1 . Said high-shear, high-vortex reactor comprises: an enclosed reaction chamber 10 , two liquid inlet pipes 1 , a gas inlet 3 located on the outer peripheral wall of said reaction chamber 10 , eight porous rotors 20 , a rotation table 30 , a rotation shaft 6 , a reaction product outlet 7 located on the outer peripheral wall of said reaction chamber 10 and near the bottom thereof, and a gas discharge pipe 8 .

Said porous rotor 20 comprises a rectangular external frame 4 and a stainless steel screen 5 with a mesh number of 60–80 and supported on said external frame 4 , wherein said external frame 4 is perpendicularly fastened to the upper surface of said rotation table 30 . Said eight porous rotors 20 are radially relative to the rotation axis of said rotation shaft 6 , and fastened to the upper surface of said rotation table 30 at an equal angular interval. In another preferred embodiment according to the present invention, said porous rotor comprises two perpendicular posts fastened to the upper surface of said rotation table, and an endless belt of a stainless steel screen stretched on said two perpendicular posts.

Said rotation table 30 , through the rotation shaft 6 fastened to the lower surface thereof, is driven by an external motor (not shown in the figure) such that said eight porous rotors 20 rotate at a high speed around the rotation axis of said rotation shaft 6 .

Each of the two liquid inlet pipes 1 comprises an inlet part 1 a protruding from said reaction chamber 10 , and a perforation part 1 b surrounded by said eight rotors 20 . Said perforation part 1 b is provided with a plurality of perforations 2 facing said rotors 20 , and said perforation part 1 b is sealed at its bottom end.

Said gas discharge pipe 8 is connected to said reaction chamber 10 and is aligned with said rotation axis. Said gas discharge pipe 8 surrounds the inlet end part 1 a of the two inlet pipes 1 , thereby forming an annular passage for discharging the gas inside said reaction chamber 30 .

When performing a gas-liquid contact, a liquid is introduced into said reaction chamber 10 through the top inlet of the inlet part 1 a of said liquid inlet pipes 1 , and, through said perforations 2 , sprayed toward said porous rotors 20 into a reaction region of the reaction chamber 10 , where the liquid is splashed by said porous rotors 20 and divided into fine droplets. The fine droplets contact and react with a reactant gas injected through the gas inlet 3 . The non-gaseous reaction product flows out the reaction chamber 10 through the reaction product outlet 7 , and the gaseous portion is discharged through the gas discharge pipe 8 .

When performing a liquid-liquid contact, two different liquids are separately introduced into the reaction chamber 10 through the two liquid inlet pipes 1 , and, through said perforations 2 , separately sprayed toward said porous rotors 20 into the reaction region, where the liquids are splashed by said porous rotors 20 and divided into fine droplets, which contact and react with each other. The reaction product flows out through the reaction product outlet 7 , and, if there is a formation of a gas, the gas is discharged through the gas discharge pipe 8 .

The porous rotors 20 in the abovementioned example can have a wide variety of modifications including, but not limited to, the ones shown in FIG. 3 : a porous rotor 20 ′ being disposed on the rotation table 30 such that an imaginary plane (shown as a dot line) extending from the porous rotor 20 ′ substantially deviates from said rotation axis; a corrugated porous rotor 20 ″; and a curved porous rotor 20 a.