CN103318952A - Method for producing nano-sized tin dioxide - Google Patents
Method for producing nano-sized tin dioxide Download PDFInfo
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- CN103318952A CN103318952A CN2013103021471A CN201310302147A CN103318952A CN 103318952 A CN103318952 A CN 103318952A CN 2013103021471 A CN2013103021471 A CN 2013103021471A CN 201310302147 A CN201310302147 A CN 201310302147A CN 103318952 A CN103318952 A CN 103318952A
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Abstract
The invention relates to a vapor phase method for preparing tin dioxide, specifically to a method for producing nano-sized tin dioxide. The method provided by the invention comprises steps of: fusing, mixing, dispersing, primary oxidation, secondary oxidation, sizing, sedimentation, cooling and collection. After tin ingot fusion, air flow and a tin liquor are mixed to form a high-speed gas-liquid mixture; and then, the high-speed gas-liquid mixture is sprayed to an oxidizing chamber and hits the wall of the oxidizing chamber so as to make tin droplets to be fully dispersed and completely oxidized therein and raise product quality. Meanwhile, after tin ingot fusion, primary oxidation is firstly carried out, and first and secondary oxidations are then carried out. Thus, high energy consumption and high cost which are caused by direct high-temperature oxidation of the tin ingot are avoided, and incomplete oxidation of tin is solved.
Description
Technical field
The present invention relates to vapor phase process and prepare tindioxide, is the method for producing nano-stannic oxide specifically.
Background technology
Tindioxide is widely used in making electrode materials, electric conductive oxidation film, glass industry, electron trade, ceramic industry.Existing tindioxide preparation method comprises vapor phase process, liquid phase method and solid-phase synthesis three major types.Vapor phase process namely adopts 2260 ℃ of high temperature (〉) with the tin volatilization, under the severe condition such as electric arc, laser, make the tindioxide powder by controlling certain reaction pressure, temperature, gas mixing ratio and flow velocity etc. afterwards.Although vapor phase process prepares the tindioxide product purity and particle diameter is comparatively desirable, from existing technique device, the large-scale production difficulty is very large.Liquid phase method comprises sol-gel method (Sol-Gel), hydrothermal method, colloidal sol-hydrothermal crystallizing composite algorithm and liquid-phase precipitation method etc.Liquid phase method is to prepare tin dioxide powder method relatively more commonly used, and Liquid preparation methods tin dioxide powder industrialized implementation biggest obstacle is that liquid-solid separation difficulty, cost are higher, reagent consumption reaches greatly the discharge of wastewater problem.Also have in addition drying to topic, because can relate to the secondary agglomeration of particle, the pattern of gained powder is undesirable.Solid phase method prepares tindioxide and mainly comprises solid reaction process, metallic salt decomposition method, mechanochemical reaction etc.Wherein solid reaction process and mechanical crushing method are difficult to make uniform ultramicron, and easily mix impurity; The metallic salt decomposition method is that the organic tin salt pyrolytic decomposition is obtained tin dioxide powder, and the SnO2 pattern that makes is difficult to control, cost is very high.
Summary of the invention
But main purpose of the present invention is to provide energy efficient, improves the quality of products, reduces the method for preparing tindioxide of cost.
The technical solution used in the present invention is: a kind of method of producing nano-stannic oxide may further comprise the steps:
(1) melting: tin slab is added melter's heating, the preliminary oxidation of tin slab melting rear portion;
(2) mix: the tin liquor of melting is with after high pressure gas mix, from melter's inflow oxidizing chamber;
(3) scatter: the gas-liquid mixture that flows into oxidizing chamber scatters with spurting, and bump oxidation locular wall;
(4) once oxidation: the tin liquor that sprays into, clashes into is carried out once oxidation in oxidizing chamber;
(5) secondary oxidation: the oxide compound of the oxide compound of the preliminary oxidation of melter and oxidizing chamber once oxidation enters the secondary oxidation chamber and carries out secondary oxidation;
(6) sub-sieve: utilize screen cloth to the oxide compound sub-sieve of secondary oxidation, the oxide compound of release mesh is by screen cloth, and the oxide compound of defective granularity stays on and reacts in the secondary oxidation chamber;
(7) sedimentation cooling: utilize the sedimentation refrigerating unit that the oxide compound by screen cloth is carried out sedimentation, cooling;
(8) collect: utilize dust-precipitator to collect cooled oxide compound, finally obtain the nano level tindioxide.
As preferably, the Heating temperature of melter is 800--1200 ℃ in the step (1), and the air flow quantity of melter is 5L/h--15 L/h.
As preferably, the Heating temperature of oxidizing chamber is 1000--1400 ℃ in the step (4), and the air flow quantity of oxidizing chamber is 15L/h--30 L/h.
As preferably, the Heating temperature of secondary oxidation chamber is 1000--1400 ℃ in the step (5), and the air flow quantity of oxidizing chamber is 10L/h--20 L/h.
As preferably, the tin liquor of melting is mixed with high pressure gas in the cavity of the tubular shaft of high speed rotating, and mixed gas-liquid mixture sprays in oxidizing chamber from the axis hole of tubular shaft, and clashes into the oxidation locular wall.
From above scheme as can be known, after the tin slab melting of the present invention, utilize air-flow to mix with tin liquor and form gas-liquid mixture at a high speed, then spray to oxidizing chamber, and bump oxidation locular wall, tin being dripped fully scatter, its inner complete oxidation improves the quality of products; Simultaneously, invention at first by primary oxidation after the tin slab melting, is carried out once again, secondary oxidation, has not only avoided the direct high temperature oxidation of tin slab, causes that energy consumption is high, cost is high; And solved the incomplete problem of tin oxidation.
Description of drawings
Fig. 1 is FB(flow block) of the present invention;
Fig. 2 is the cross-sectional schematic of tubular shaft.
Embodiment
Below in conjunction with embodiment and Fig. 1 and Fig. 2 the present invention is described in further detail:
Method of the present invention may further comprise the steps:
(1) melting: tin slab is added melter's heating, and the preliminary oxidation of tin slab melting rear portion forms oxide compound; As preferably, Heating temperature is 800--1200 ℃, and the air flow quantity of melter is 5L/h--15 L/h;
(2) mix: the tin liquor of melting enters high speed rotating tubular shaft cavity 12 from the opening 11 of tubular shaft 1, mixes with the high pressure gas that enter from the tubular shaft port, then flows into oxidizing chamber from melter;
(3) scatter: the gas-liquid mixture of inflow oxidizing chamber scatters with spurting in oxidizing chamber from the axis hole 13 of tubular shaft, and clashes into the oxidation locular wall, thereby makes tin drip abundant oxidation;
(4) once oxidation: in oxidizing chamber, carry out once oxidation from the tin liquor that axis hole sprays into, clashes into; Preferred employing degree is 1000--1400 ℃, and the air flow quantity of oxidizing chamber is 15L/h--30 L/h;
(5) secondary oxidation: the oxide compound of the oxide compound of the preliminary oxidation of melter and oxidizing chamber once oxidation enters the secondary oxidation chamber and carries out secondary oxidation, and the Heating temperature of secondary oxidation chamber is 1000--1400 ℃, and the air flow quantity of oxidizing chamber is 10L/h--20 L/h;
(6) sub-sieve: utilize screen cloth to the oxide compound sub-sieve of secondary oxidation, the oxide compound of release mesh is by screen cloth, and the oxide compound of defective granularity stays on and reacts in the secondary oxidation chamber;
(7) sedimentation cooling: utilize the sedimentation refrigerating unit that the oxide compound by screen cloth is carried out sedimentation, cooling;
(8) collect: utilize dust-precipitator to collect cooled oxide compound, finally obtain the nano level tindioxide.
When using method of the present invention, can adopt to the temperature of each reaction zone different temperature control, and can adopt thermo detector etc. to realize temperature automatically controlled function, to reach the quantity-produced purpose.
Embodiment one
With 1000g tin slab heating and melting chamber, melter adopts 800 ℃ of heating, and air flow quantity is 5L/h, approximately after 10 minutes, passes into high pressure gas from the tubular shaft port; Oxidizing chamber adopts 1000 ℃ of heating, and air flow quantity is 15L/h; Simultaneously, 1000 ℃ of heating are adopted in the secondary oxidation chamber, and flow is 10L/h, and reactant is collected 1258.7 g tindioxide after cold sedimentation cooling, to the tindioxide analysis of collecting, and granularity＜86nm,
Whiteness is 89%, and oxidation ratio is 99.01%.
Embodiment two
With 1000g tin slab heating and melting chamber, melter adopts 950 ℃ of heating, and air flow quantity is 12L/h, approximately after 7 minutes, passes into high pressure gas from the tubular shaft port; Oxidizing chamber adopts 1300 ℃ of heating, and air flow quantity is 22L/h; Simultaneously, 1200 ℃ of heating are adopted in the secondary oxidation chamber, and flow is 15L/h, and reactant is collected the 1269.1g tindioxide after cold sedimentation cooling, to the tindioxide analysis of collecting, and granularity＜26nm,
Whiteness is 88%, and oxidation ratio is 99.85%.
Embodiment three
With 1000g tin slab heating and melting chamber, melter adopts 1000 ℃ of heating, and air flow quantity is 15L/h, approximately after 5 minutes, passes into high pressure gas from the tubular shaft port; Oxidizing chamber adopts 1400 ℃ of heating, and air flow quantity is 30L/h; Simultaneously, 1400 ℃ of heating are adopted in the secondary oxidation chamber, and flow is 20L/h, and reactant is collected the 1263.5g tindioxide after cold sedimentation cooling, to the tindioxide analysis of collecting, and granularity＜42nm,
Whiteness is 90%, and oxidation ratio is 99.39%.
Above demonstration and described ultimate principle of the present invention and principal character and advantage of the present invention; the technician of the industry should understand; the present invention is not subjected to the restriction of aforesaid way; without departing from the spirit and scope of the present invention; also have various changes and modifications, these changes and improvements all fall in the claimed scope of the present invention.
Claims (5)
1. method of producing nano-stannic oxide may further comprise the steps:
(1) melting: tin slab is added melter's heating, the preliminary oxidation of tin slab melting rear portion;
(2) mix: the tin liquor of melting is with after high pressure gas mix, from melter's inflow oxidizing chamber;
(3) scatter: the gas-liquid mixture that flows into oxidizing chamber scatters with spurting, and bump oxidation locular wall;
(4) once oxidation: the tin liquor that sprays into, clashes into is carried out once oxidation in oxidizing chamber;
(5) secondary oxidation: the oxide compound of the oxide compound of the preliminary oxidation of melter and oxidizing chamber once oxidation enters the secondary oxidation chamber and carries out secondary oxidation;
(6) sub-sieve: utilize screen cloth to the oxide compound sub-sieve of secondary oxidation, the oxide compound of release mesh is by screen cloth, and the oxide compound of defective granularity stays on and reacts in the secondary oxidation chamber;
(7) sedimentation cooling: utilize the sedimentation refrigerating unit that the oxide compound by screen cloth is carried out sedimentation, cooling;
(8) collect: utilize dust-precipitator to collect cooled oxide compound, finally obtain the nano level tindioxide.
2. method according to claim 1 is characterized in that: the Heating temperature of melter is 800--1200 ℃ in the step (1), and the air flow quantity of melter is 5L/h--15 L/h.
3. method according to claim 1 is characterized in that: the Heating temperature of oxidizing chamber is 1000--1400 ℃ in the step (4), and the air flow quantity of oxidizing chamber is 15L/h--30 L/h.
4. method according to claim 1 is characterized in that: the Heating temperature of secondary oxidation chamber is 1000--1400 ℃ in the step (5), and the air flow quantity of oxidizing chamber is 10L/h--20 L/h.
5. method according to claim 1, it is characterized in that: the tin liquor of melting is mixed with high pressure gas in the cavity of the tubular shaft of high speed rotating, and mixed gas-liquid mixture sprays in oxidizing chamber from the axis hole of tubular shaft, and clashes into the oxidation locular wall.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310302147.1A CN103318952B (en) | 2013-07-17 | 2013-07-17 | Method for producing nano-sized tin dioxide |
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| CN201310302147.1A CN103318952B (en) | 2013-07-17 | 2013-07-17 | Method for producing nano-sized tin dioxide |
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| CN103318952A true CN103318952A (en) | 2013-09-25 |
| CN103318952B CN103318952B (en) | 2015-03-25 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116041057A (en) * | 2022-12-26 | 2023-05-02 | 广东微容电子科技有限公司 | Barium titanate powder, preparation method and chip type multilayer ceramic capacitor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4623424A (en) * | 1983-09-07 | 1986-11-18 | National Institute For Researches In Inorganic Materials | Process for producing tin oxide fibers |
| CN1351961A (en) * | 2001-11-09 | 2002-06-05 | 财团法人工业技术研究院 | Process for producing transparent conductive oxide powder by air jet method |
| CN102616847A (en) * | 2012-04-05 | 2012-08-01 | 广西华锑科技有限公司 | Method for preparing catalyst grade antimony trioxide |
-
2013
- 2013-07-17 CN CN201310302147.1A patent/CN103318952B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4623424A (en) * | 1983-09-07 | 1986-11-18 | National Institute For Researches In Inorganic Materials | Process for producing tin oxide fibers |
| CN1351961A (en) * | 2001-11-09 | 2002-06-05 | 财团法人工业技术研究院 | Process for producing transparent conductive oxide powder by air jet method |
| CN102616847A (en) * | 2012-04-05 | 2012-08-01 | 广西华锑科技有限公司 | Method for preparing catalyst grade antimony trioxide |
Non-Patent Citations (1)
| Title |
|---|
| BRINZARI V, ET AL.: "Morphological rank of nano-scale tindioxide films deposited by spray pyrolysis from SnCl4·5H2O water solution", 《THE SOLID FILMS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116041057A (en) * | 2022-12-26 | 2023-05-02 | 广东微容电子科技有限公司 | Barium titanate powder, preparation method and chip type multilayer ceramic capacitor |
| CN116041057B (en) * | 2022-12-26 | 2023-11-24 | 广东微容电子科技有限公司 | Barium titanate powder, preparation method and chip type multilayer ceramic capacitor |
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| CN103318952B (en) | 2015-03-25 |
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Effective date of registration: 20200326 Address after: 547000 No.71, Chengxi Road, Hechi City, Guangxi Zhuang Autonomous Region Patentee after: GUANGXI HUAXI GROUP Co.,Ltd. Address before: 545000, the Guangxi Zhuang Autonomous Region, Liuzhou hi tech Road No. 15 standard workshop D seat, fifth floors East Patentee before: LIUZHOU BAIRENTE ADVANCED MATERIALS Co.,Ltd. |