Process for producing nanometer grade powders

• US 7,211,230 B2
• Filed: 03/05/2002
• Issued: 05/01/2007
• Est. Priority Date: 03/07/2001
• Status: Expired due to Fees

• Current Assignee: Anshan University of Science and Technology
• Original Assignee: Anshan University of Science and Technology
• Inventors: Li, Hongxia, Li, Xiaoqi, Gao, Shoushan, Zhou, Yingyan, Wang, Kaiming, Wen, Chuangeng, Li, Lixiang
• Primary Examiner(s): Vanoy; Timothy C.
• Application Number:
  US10/471,142
• Publication Number:
  US 20040115123A1
• Time in Patent Office: 1,883 Days
• Field of Search: 423/1, 423/592.1, 423/579, 423/462, 423/299, 423/561.1, 423/69, 423/622, 423/101, 423/598, 423/594.16, 423/71, 423/84, 423/85, 423/608, 757/39, 757/40, 977/773, 977/775, 977/776, 977/777
• US Class Current: 423/1
• CPC Class Codes: C01G 1/00 Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general electrolytic production of inorganic compounds C25B1/00
• CPC Class Codes: Y10S 977/773 Nanoparticle, i.e. structure having three dimensions of 100 nm or less
• CPC Class Codes: Y10S 977/775 Nanosized powder or flake, e.g. nanosized catalyst
• CPC Class Codes: Y10S 977/776 Ceramic powder or flake
• CPC Class Codes: Y10S 977/777 Metallic powder or flake

Abstract

The present invention discloses a process for producing nanometer powders, comprising the following steps: (a) providing reactant solution A and reactant solution B that can rapidly react to form precipitate; (b) continuously adding said solution A and solution B into a mixing and reacting precipitator with a stator and a rotor in operation, respectively; and (c) post-treating the precipitate-containing slurry discharged continuously from the mixing and reacting precipitator. The present process could produce nanometer powders with adjustable particle size, good homogeneity in size and good dispersity. The method also has the characteristics of high production yield, simplicity in process and low consumption of energy. It could be applied to produce various nanometer powders of metals, oxides, hydroxides, salts, phosphides and sulfides as well as organic compounds.

Claims

1. A process for preparing a nanometer powder, comprising:

(a) providing a reactant solution A and a reactant solution B that can rapidly react to form a precipitate;

(b) continuously adding said solution A and solution B into a mixing and reacting precipitator with a stator and a rotor in operation, respectively, thereby obtaining a precipitate-containing slurry, wherein mixing, reacting and precipitation is completed in a short interval of 0.1 to 10 seconds; and

(c) post-treating the precipitate-containing slurry discharged continuously from the mixing and reacting precipitator.

2. The process as claimed in claim 1, wherein said solution A and solution B of step (a) comprise an auxiliary reacting agent and/or dispersant.

3. The process of claim 1, further comprising providing in said step (a) at least one auxiliary reacting solution selected from a group consisting of a dispersant, an auxiliary reacting agent and a pH regulator.

4. The process of claim 3, wherein, when there is only one auxiliary reacting solution, a distance h in an axis direction between an inlet of said auxiliary solution of a cylindrical mixing and reacting precipitator and inlets for solution A and solution B is in the range of zero to half of the axis-direction length of said mixing and reacting precipitator.

5. The process of claim 3, wherein, when there is a plurality of auxiliary reacting solutions, inlets of said plurality of auxiliary solutions on a cylindrical mixing and reacting precipitator and inlets for the solution A and the solution B are arranged around the cylindrical mixing and reacting precipitator on the same plane perpendicular to a rotating axis, or arranged successively on the cylindrical mixing and reacting precipitator along the rotating axis.

6. The process as claimed in claim 1, wherein said solution A and said solution B in step (a) are independently in the form of aqueous solution or organic solution.

7. The process of claim 6, wherein a temperature of said aqueous solution or organic solution is in a range from 15°

C. to a boiling point thereof.

8. The process of claim 1, further comprising:

in said step (b), rapidly dispersing said solution A and solution B by rapid stirring, shearing and strong turbulence, thereby breaking it into isolated micro liquid agglomerates and then completing a process of molecular diffusion, chemical reaction, nucleation and formation of nanometer particulate and of precipitate wherein mixing reacting zones are continuously orderly arranged along an advancing direction of the mixed solutions A and B, whereby step (b) is completed in a short interval of 0.1 to 10 seconds, wherein the precipitate-containing slurry continuously flows out of the mixing and reacting precipitator.

9. The process of claim 1, wherein, in step (b), said mixing and reacting precipitator is comprised of one stator and one rotor on the same axis, a speed of revolution of the rotor is in the range of 500 to 20000 rpm, a volume of flow of the reactant solution passing through the mixing and reacting precipitator is in the range of 0.02 to 3000m³/h.

10. The process of claim 9, wherein said stator or rotor comprises a stirring wing.

11. The process of claim 9, wherein said speed of revolution is between 800 and 12000 rpm.

12. The process of claim 1, wherein, in step (b), the mixing and reacting precipitator has a shape of a cylinder or a disc or any other symmetric form.

13. The process of claim 1, wherein in step (b) said mixing and reacting precipitator has a cylinder shape, and comprises two inlets for the reactant solutions and one or more inlets for auxiliary solutions installed on one side of the precipitator and an outlet for precipitate-containing mixed solution installed on the other side, wherein the difference between an inner diameter of the stator and an outer diameter of the rotor is in the range of 2 to 1000 mm.

14. The process of claim 13, wherein said difference between the inner diameter of the stator and the outer diameter of the rotor is in the range of 3 to 150 mm.

15. The process of claim 1, wherein, in step (b), when the mixing and reacting precipitator is of a cylinder-shape, a diameter of the stator is in the range of 150 to 10000 mm, inlets for the reactant solutions A and B are arranged on the stator, inlets for one or more auxiliary solutions are arranged within a half of the stator radius from the rotating axis and are arranged successively according to different values of a distance from the rotating axis, an outlet for the precipitate-containing slurry is arranged at an outer fringe of a disc of the stator, or the inlet of the reactant solutions A and B is arranged at the outer fringe of the disc of the stator, the inlet for the auxiliary solutions is provided near the outer fringe of the radius of the disc of the stator and the outlet of the precipitate-containing slurry is provided on a portion, near the center of rotating axis, of the disc of the stator.

16. The process of claim 15, wherein the diameter of the stator is between 200 and 1000 mm.

17. The process of claim 1, wherein said step (c) is started, after said precipitate-containing slurry flows out of the mixing and reacting precipitator continuously.

18. The process of claim 17, wherein said post-treating is started immediately after said precipitate-containing slimy flows out of the mixing and reacting precipitator.

19. The process of claim 1, wherein, said post-treating in step (c) comprise separation, drying and pulverization steps.

20. The process of claim 19, wherein said separation step comprises filtration and washing.

21. The process of claim 20, wherein said drying step further comprises azeotropic distillation.

22. The process of claim 20, wherein said filtration and washing is performed in a continuously operating facility.

23. The process of claim 1, wherein said nanometer powder is at least one selected from a group consisting of metals, oxides, hydroxides, salts, phosphides, sulfides and organic compounds.