# US 2013/0156682 A1 · Method for producing isolatable oxide microparticles or hydroxide microparticles

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- Number: US 2013/0156682 A1
- Document ID: US20130156682A1
- Status: Published application
- Kind: A1
- Application number: 13/818,954
- Filed: 2011-08-26
- Published: 2013-06-20
- Earliest claimed: 2010-08-26
- Assignees: M. Technique Co., Ltd.
- Inventors: Jun Kuraki; Kaeko Araki; Masaki Maekawa; Daisuke Honda; Masakazu Enomura
- Web page: https://patentgrep.com/patent/US20130156682A1

## CPC

- C01G 23/0536: {by hydrolysing chloride-containing salts}
- B01D 9/0009: {by direct heat exchange with added cooling fluid}
- B01F 27/2712: {provided with ribs, ridges or grooves on one surface}
- B01F 27/2714: {the relative position of the stator and the rotor, gap in between or gap with the walls being adjustable}
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- C01B 13/36: by precipitation reactions in {aqueous} solutions {(C01B13/328 takes precedence)}
- C01F 5/02: Magnesia
- C01F 5/14: Magnesium hydroxide
- C01F 5/20: by precipitation from solutions of magnesium salts with ammonia
- C01F 17/218: Yttrium oxides or hydroxides
- C01G 1/02: Oxides
- C01G 23/0532: {by hydrolysing sulfate-containing salts}
- C01G 25/02: Oxides
- C01P 2002/54: one element only
- C01P 2004/04: obtained by TEM, STEM, STM or AFM
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- B01F: MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING (mixing paints B44D3/06)
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C01F: COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; sulfides or polysulfides of magnesium, calcium, strontium, or barium C01B17/42; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds other than ammonia or cyanogen containing nitrogen and non-metals and optionally metals C01B21/082; amides or imides of silicon C01B21/087}; metal {imides or} amides C01B21/092, {C01B21/0923}; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanic acid C01C3/14; salts of cyanamide C01C3/16; thiocyanates C01C3/20; {double sulfates of magnesium with sodium or potassium C01D5/12; with other alkali metals C01D15/00, C01D17/00})
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

A method for producing isolatable oxide microparticles or hydroxide microparticles using an apparatus that processes a fluid between processing surfaces of processing members that are arranged opposite each other so as to be able to approach to or separate from each other and such that at least one can rotate relative to the other. At least two fluids are mixed and oxide microparticles or hydroxide microparticles are separated, said two fluids including: a fluid containing a microparticle raw material solution comprising a microparticle raw material mixed into a solvent, and a fluid containing a microparticle-separation solution. Immediately thereafter, the following are mixed to obtain isolatable oxide microparticles or hydroxide microparticles: a fluid containing the separated oxide microparticles or hydroxide microparticles; and a fluid containing a microparticle-treatment-substance-containing solution that contains a microparticle-treatment substance that adjusts the dispersibility of the separated oxide microparticles or hydroxide microparticles.

## Claims

### Claim 1

A method for producing isolatable oxide microparticles or hydroxide microparticles, wherein
each of (I) a microparticle raw material solution which is obtained by mixing at least one microparticle raw material with a solvent, (II) a microparticle-separating solution, and (III) a microparticle-treating substance solution which is obtained by mixing at least one microparticle-treating substance with a solvent is prepared, wherein the method comprises:
(IV) a step of separating oxide microparticles or hydroxide microparticles, wherein
at least two fluids to be processed are used:
out of them, at least one fluid is the fluid which contains the microparticle raw material solution and at least one fluid other than the microparticle raw material solution is the fluid which contains the microparticle-separating solution, wherein
the fluid which contains the microparticle raw material solution is mixed with the fluid which contains the microparticle-separating solution in a thin film fluid formed between at least two processing surfaces which are disposed in a position they are faced with each other so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, and
(V) a step of mixing a fluid which contains the oxide microparticles or the hydroxide microparticles separated in the step (IV) with the fluid which contains the microparticle-treating substance solution, wherein
the microparticle-treating substance is a substance which controls dispersibility of the said separated oxide maicroparticles or hydroxide microparticles.

### Claim 2 (depends on 1)

The method for producing isolatable oxide microparticles or hydroxide microparticles according to claim 1, wherein
any one of the fluid which contains the microparticle raw material solution and the fluid which contains the microparticle-separating solution passes between the processing surfaces with forming the thin film fluid,
a separate introduction path independent of a flow path through which any one of the fluids passes is arranged,
at least any one of the at least two processing surfaces is provided with an opening to the introduction path,
any other one of the fluid which contains the microparticle raw material solution and the fluid which contains the microparticle-separating solution is introduced between the processing surfaces through the opening, whereby mixing the fluid which contains the microparticle raw material solution with the fluid which contains the microparticle-separating solution in the thin film fluid.

### Claim 3 (depends on 1)

The method for producing isolatable oxide microparticles or hydroxide microparticles according to claim 1, wherein the method comprises:
a step of separating oxide microparticles or hydroxylated oxide microparticles by mixing the fluid which contains the microparticle raw material solution with the fluid which contains the microparticle-separating solution in the thin film fluid formed between at least two processing surfaces which are disposed in a position they are faced with each other so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, and
a step of mixing the fluid which contains the oxide microparticles or the hydroxide microparticles separated in the above-mentioned step with the fluid which contains the microparticle-treating substance solution, wherein these steps are carried out continuously.

### Claim 4 (depends on 3)

The method for producing isolatable oxide microparticles or hydroxide microparticles according to claim 3, wherein
at least any one of the at least two processing surfaces is provided with an opening to introduce the fluid which contains the microparticle-treating substance solution between the processing surfaces,
the fluid which contains the microparticle raw material solution is mixed with the fluid which contains the microparticle-separating solution in the thin film fluid to separate oxide microparticles or hydroxide microparticles, and thereafter,
the microparticle-treating substance is contacted with and acted to the separated oxide microparticles or hydroxide microparticles in the thin film fluid.

### Claim 5 (depends on 3)

The method for producing isolatable oxide microparticles or hydroxide microparticles according to claim 3, wherein
an opening to supply the fluid which contains the microparticle-treating substance solution is arranged in a position to face a discharge part of the at least two processing surfaces,
the fluid which contains the microparticle raw material solution is mixed with the fluid which contains the microparticle-separating solution in the thin film fluid to separate the oxide microparticles or the hydroxide microparticles thereby discharging the fluid which contains the oxide microparticles or the hydroxide microparticles through the discharge part, and immediately thereafter,
the microparticle-treating substance is contacted with and acted to the separated oxide microparticles or hydroxide microparticles.

### Claim 6 (depends on 1)

The method for producing isolatable oxide microparticles or hydroxide microparticles according to claim 1, wherein a step of mixing the fluid which contains the separated oxide microparticles or hydroxide microparticles with the fluid which contains the microparticle-treating substance solution is carried out within one second after the step of separating the oxide microparticles or the hydroxide microparticles.

### Claim 7 (depends on 1)

The method for producing isolatable oxide microparticle or hydroxide microparticle according to claim 1, wherein dispersibility of the oxide microparticles or the hydroxide microparticles is controlled by controlling concentration of the microparticle-treating substance in the microparticle-treating substance solution that is contacted with and acted to the separated oxide microparticles or hydroxide microparticles.

### Claim 8 (depends on 1)

The method for producing isolatable oxide microparticles or hydroxide microparticles according to claim 1, wherein the microparticle-treating substance is an acidic substance or hydrogen peroxide.

### Claim 9 (depends on 2)

The method for producing isolatable oxide microparticles or hydroxide microparticles according to claim 2, wherein the method comprises:
a step of separating oxide microparticles or hydroxylated oxide microparticles by mixing the fluid which contains the microparticle raw material solution with the fluid which contains the microparticle-separating solution in the thin film fluid formed between at least two processing surfaces which are disposed in a position they are faced with each other so as to be able to approach to and separate from each other, at least one of which rotates relative to the other, and
a step of mixing the fluid which contains the oxide microparticles or the hydroxide microparticles separated in the above-mentioned step with the fluid which contains the microparticle-treating substance solution, wherein these steps are carried out continuously.

### Claim 10 (depends on 2)

The method for producing isolatable oxide microparticles or hydroxide microparticles according to claim 2, wherein a step of mixing the fluid which contains the separated oxide microparticles or hydroxide microparticles with the fluid which contains the microparticle-treating substance solution is carried out within one second after the step of separating the oxide microparticles or the hydroxide microparticles.

### Claim 11 (depends on 3)

The method for producing isolatable oxide microparticles or hydroxide microparticles according to claim 3, wherein a step of mixing the fluid which contains the separated oxide microparticles or hydroxide microparticles with the fluid which contains the microparticle-treating substance solution is carried out within one second after the step of separating the oxide microparticles or the hydroxide microparticles.

### Claim 12 (depends on 4)

The method for producing isolatable oxide microparticles or hydroxide microparticles according to claim 4, wherein a step of mixing the fluid which contains the separated oxide microparticles or hydroxide microparticles with the fluid which contains the microparticle-treating substance solution is carried out within one second after the step of separating the oxide microparticles or the hydroxide microparticles.

### Claim 13 (depends on 5)

The method for producing isolatable oxide microparticles or hydroxide microparticles according to claim 5, wherein a step of mixing the fluid which contains the separated oxide microparticles or hydroxide microparticles with the fluid which contains the microparticle-treating substance solution is carried out within one second after the step of separating the oxide microparticles or the hydroxide microparticles.

### Claim 14 (depends on 2)

The method for producing isolatable oxide microparticle or hydroxide microparticle according to claim 2, wherein dispersibility of the oxide microparticles or the hydroxide microparticles is controlled by controlling concentration of the microparticle-treating substance in the microparticle-treating substance solution that is contacted with and acted to the separated oxide microparticles or hydroxide microparticles.

### Claim 15 (depends on 3)

The method for producing isolatable oxide microparticle or hydroxide microparticle according to claim 3, wherein dispersibility of the oxide microparticles or the hydroxide microparticles is controlled by controlling concentration of the microparticle-treating substance in the microparticle-treating substance solution that is contacted with and acted to the separated oxide microparticles or hydroxide microparticles.

### Claim 16 (depends on 4)

The method for producing isolatable oxide microparticle or hydroxide microparticle according to claim 4, wherein dispersibility of the oxide microparticles or the hydroxide microparticles is controlled by controlling concentration of the microparticle-treating substance in the microparticle-treating substance solution that is contacted with and acted to the separated oxide microparticles or hydroxide microparticles.

### Claim 17 (depends on 5)

The method for producing isolatable oxide microparticle or hydroxide microparticle according to claim 5, wherein dispersibility of the oxide microparticles or the hydroxide microparticles is controlled by controlling concentration of the microparticle-treating substance in the microparticle-treating substance solution that is contacted with and acted to the separated oxide microparticles or hydroxide microparticles.

### Claim 18 (depends on 6)

The method for producing isolatable oxide microparticle or hydroxide microparticle according to claim 6, wherein dispersibility of the oxide microparticles or the hydroxide microparticles is controlled by controlling concentration of the microparticle-treating substance in the microparticle-treating substance solution that is contacted with and acted to the separated oxide microparticles or hydroxide microparticles.

### Claim 19 (depends on 2)

The method for producing isolatable oxide microparticles or hydroxide microparticles according to claim 2, wherein the microparticle-treating substance is an acidic substance or hydrogen peroxide.

### Claim 20 (depends on 3)

The method for producing isolatable oxide microparticles or hydroxide microparticles according to claim 3, wherein the microparticle-treating substance is an acidic substance or hydrogen peroxide.
