CN1172769A - Method for producing particle diantimony trioxide and its device - Google Patents
Method for producing particle diantimony trioxide and its device Download PDFInfo
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- CN1172769A CN1172769A CN 97107945 CN97107945A CN1172769A CN 1172769 A CN1172769 A CN 1172769A CN 97107945 CN97107945 CN 97107945 CN 97107945 A CN97107945 A CN 97107945A CN 1172769 A CN1172769 A CN 1172769A
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Abstract
A process for producing micro particles of Sb2O3 features that an antimony oxide furnace with reverberatoryh furnace's structure, which has a high-temp gasifying reaction chamber over its cylindrical reaction chamber and a built-in burnner is used, and full-cubic crystal of Sb2O3 in 0.05-0.2 microns of granularity is obtained by regulating the supply of fuel, keeping temp in gasifying reaction chamber to 900-1800 deg. C and controlling the ratio of high-temp furnace gas containing Sb2O3 to suddenly cooling air. Ultra-high-purity Sb2O3 with 99.85% of main component and over 98% of whiteness can also be obtained. Its advantages are high output and less energy consumption.
Description
The invention relates to a method and a device for producing fine antimony trioxide.
One of the main uses of antimony trioxide is as flame retardant synergist for plastics, chemical fiber fabrics and the like, but when a certain amount of flame retardant is added into a plastic or chemical fiber substrate, the physical properties of the product, such as impact strength, tensile strength and the like, are reduced. Particularly, when antimony trioxide is added into a chemical fiber matrix for spinning, the maximum particle size of the antimony trioxide is required to be not more than 1 micron, otherwise, the spinning production is influenced. In fact, under the condition that the amount of antimony trioxide doped in the product is the same, the finer the granularity is, the better the flame retardant effect is, and the influence on the physical properties of the product is smaller. In some fields such as catalysts and chemical vectors, antimony trioxide is required to have a high purity, with a main component of 99.85% or more, and the content of impurity elements such as lead, arsenic, and higher oxides of antimony such as antimony tetroxide must be low.
Currently, particulate antimony trioxide is generally produced by the pyrogenic process, for example, US4347060 and CN103844.4A by the plasma process. The common antimony trioxide is used as raw material, the raw material is gasified at the high temperature of more than 2000 ℃ of plasma tail flame, and then the raw material is quenched to generate the antimony trioxide fine product. The method can obtain the product with the granularity less than 0.3 micron, but needs to use the antimony trioxide as the raw material, and has high energy consumption, thereby having high production cost. JP5918116 discloses a method and apparatus for producing fine antimony trioxide, wherein metallic antimony is melted in an electric furnace, blown to oxidize the surface of antimony liquid, high temperature air is blown to dilute the antimony trioxide vapor to reduce the concentration, and then the vapor is quenched to obtain fine antimony trioxide product. However, this method is limited to laboratory production and yields are very low. The antimony white furnace with the reverberatory furnace structure, which is disclosed in CN85102489.0, produces antimony trioxide by taking metallic antimony as a raw material, wherein the average particle size is 1.0-1.6 microns, the particle size distribution range is large, and the particle sizes are slightly uneven.
The main purpose of the invention is to utilize the antimony white furnace with the reverberatory furnace structure to overcome the defects of the prior art and directly produce the particle antimony trioxide, wherein the particle size of the product is less than 0.2 micron, the particle size distribution range is narrow, and the particle size of the product is uniform.
It is another object of the present invention to produce ultra-high purity antimony trioxide simultaneously with the production of particulate antimony trioxide.
The purpose of the invention is realized as follows: as the metallic antimony liquidin the antimony white furnace hearth of the reverberatory furnace structure can emit a large amount of heat to make the central temperature of an oxidation reaction zone reach more than 1000 ℃ during the oxidation reaction, but when high-temperature furnace gas containing antimony trioxide rises through the cylindrical reaction chamber to meet cooling air, the temperature is gradually reduced to 500-600 ℃, the condensation point of the antimony trioxide is 656 ℃, so that the antimony trioxide is partially condensed into solid particles before quenching, the particle size of a final product is coarsened, and the particle size is not largeAnd (4) uniformity. Meanwhile, in the gradual cooling process, the proper temperature range for the generation of the antimony tetroxide is 500-900 ℃, so that a small amount of antimony tetroxide is produced to cause the main component of the product to be lower. Therefore, in order to overcome the defect, the invention discloses a high-temperature gasification reaction chamber which is arranged at the upper end of a cylindrical reaction chamber of an antimony white furnace, and the antimony trioxide steam is heated to 900-1800 ℃ when passing through the high-temperature gasification reaction chamber by supplying fuel to the reaction chamber for combustion so as to form a uniformly distributed gas state, and the granular antimony trioxide can be gasified even if the granular antimony trioxide exists in the furnace gas before entering the high-temperature gasification chamber. At the same time, the antimony tetroxide produced is also dissociated: avoiding the formation of antimony tetroxide which is a high-valence oxide of antimony in the productThe purity of the final product is greatly improved. Introducing high-temperature furnace gas of a gasification reaction chamber into an quenching mixer at the top end of the gasification reaction chamber, quenching by using a large amount of cooling air, controlling the ratio of the total amount of the high-temperature furnace gas containing antimony trioxide to the amount of the cooling air to be 1: 2-10, instantly cooling the high-temperature furnace gas to about 200 ℃, condensing the high-temperature furnace gas into cubic crystal particle antimony trioxide powder, and collecting the cubic crystal particle antimony trioxide powder in a cloth bag dust collection system.
The fuel used for combustion in the high-temperature gasification reaction chamber can be any one of liquefied petroleum gas, natural gas, coal gas, oil gas, methane, alcohol and gasoline or a mixture of more than two of the liquefied petroleum gas, the natural gas, the coal gas, the oil gas, the methane, the alcohol and the gasoline.
The production apparatus of the present invention will be further described with reference to the accompanying drawings:
the attached figure is a front view of the apparatus used in the method of the invention.
The device for producing the particle antimony trioxide comprises an antimony white furnace 1 with a reverberatory furnace structure and a high-temperature gasification reaction chamber 9 arranged at the upper end of a cylindrical reaction chamber 2 of the antimony white furnace 1, wherein 1-4 burners 8 are uniformly distributed on the periphery of an inner wall 10 of the reaction chamber formed by ramming refractory mortar, and fuel and air required by the burners 8 are supplied by a set of independent supply system 4 capable of adjusting the supply amount of the fuel and the air. A quenching mixer 12 is arranged at the high-temperature furnace gas discharge end of the high-temperature gasification reaction chamber 9. On one side of the quenching mixer 12 is a cooling air inlet pipe 11, and the lower part of the quenching mixer 12 is closely connected with the high-temperature gasification chamber 9 and is a high-temperature furnace gas inlet 7. The other side of the quenching mixer 12 is a quenching mixing area 6, the quenching mixing area 6 is developed in a streamline shape, a cooling air lower air inlet 5 is arranged at the bottom of the position with the minimum cross section area, and the position with the maximum cross section area of the quenching mixing area 6 is connected with the cooled furnace gas outlet pipe 3.
The particle antimony trioxide prepared by the invention has the advantages of high yield and low energy consumption, and the specific surface area of the obtained product is more than 11m2Per g, average particle size less than 0.2 micron, and can produce ultra-pure trioxide with main component over 99.85% and whiteness over 98 degAnd (3) antimony disulfide.
The following are examples of the present invention:
example 1 uses metallic antimony II as raw material, and its chemical composition is: 99.84% of Sb, 0.02% of AS, 0.11% of Pb, 0.011% of Fe, 5.4m per hour2Adding 300kg of metallic antimony into the antimony white furnace, using liquefied petroleum gas as fuel, maintaining the temperature in the gasification reaction chamber 9 at 1300-1600 ℃, and controlling the total amount of high-temperature antimony trioxide furnace gas and the quenching mixer 12 when the storage furnace gas leaves the gasification reaction chamber 9 and enters the quenching mixer 12The ratio of the total amount of the cold air is 1: 6-8, the obtained product is collected by a cloth bag dust collecting system, 345kg of product is obtained every hour, and the physical and chemical detection result of one batch number of 10 tons of product is as follows:
total specific surface area: 12.02m2/g
Specific surface area average particle size: 0.090 micron
Particle size distribution (weight percent):
0-0.12 micron: 56.2 percent
0.12-0.22 micron: 29.9 percent
0.22-0.60 micron: 13.9 percent
The crystal form is as follows: 99.7% cubic crystal form
Whiteness (zeiss whiteness meter): 98.5 degree
Chemical components:
Sb2O399.92％
AS2O30.028％，
PbO 0.031％
Fe2O30.0016％
TAI (tartaric insoluble): 0.020 percent
EG (ethylene glycol) dissolution residue: 133ppm of
The chemical components of the raw material metallic antimony used in example 2 are: 99.79% of Sb, 0.029% of As, 0.16% of Pb and 0.015% of Fe, coal gas is used As fuel, the temperature of a gasification reaction chamber is maintained to be 1000-1200 ℃, the ratio of the gas quantity of a high-temperature furnace to the air quantity of quenching is controlled to be 1: 3-4 during quenching, the other conditions are the same As example 1, 5 tons of Sb are obtained, and the physicochemical detection results of the product are As follows:
total specific surface area: 11.67m2/g
Specific surface area average particle size: 0.093 micron
Particle size distribution:
0-0.12 micron: 53.6 percent
0.12-0.22 micron: 31.7 percent
0.22-0.60 micron: 14.7 percent
The crystal form is as follows: 99.8% cubic crystal form
Whiteness (zeiss whiteness meter); 98.3 degree
Chemical components: sb2O399.89％ AS2O30.032％
PbO 0.045％ Fe2O30.0016％
TAI (tartaric insoluble): 0.023% EG residue: 169ppm of
Claims (5)
1. A process for preparing granular antimony trioxide by reverberatory furnace features that the furnace gas containing antimony trioxide and discharged from cylindrical reaction chamber of antimony trioxide is introduced to a high-temp gasifying reaction chamber, the fuel is supplied to said gasifying reaction chamber for combustion to raise temp until the antimony trioxide in said furnace gas is completely in gas state, the high-temp furnace gas discharged from gasifying reaction chamber is introduced to quenching mixer for quenching it with a lot of cooling air to quickly crystallize the gaseous antimony trioxide, and the granular antimony trioxide is finally obtained by cloth bag dust-collecting system.
2. The method for producing fine particulate antimony trioxide as claimed in claim 1, wherein the temperature in the high-temperature gasification reaction chamber is 900 to 1800 ℃.
3. The method for producing fine particulate antimony trioxide as claimed in claim 1, wherein the ratio of the amount of the high-temperature furnace gas to the amount of the quenching air is 1: 2 to 10.
4. The method of producing fine antimony trioxide according to claim 1, wherein the fuel used is any one of liquefied petroleum gas, natural gas, coal gas, oil gas, methane gas, alcohol, and gasoline, or a mixture of two or more thereof.
5. The apparatus for producing fine antimony trioxide as claimed in claim 1, comprising an antimony white furnace [1]of reverberatory furnace structure, characterized in that it further comprises a high temperature gasification reaction chamber [9]installed at the upper end of the cylindrical reaction chamber [2]of the antimony white furnace, 1 to 4 burners [8]uniformly distributed around the inner wall [10]of the reaction chamber pounded with fire clay, a set of independent supply system [4]for supplying fuel and air required for combustion by the burners [8]and capable of adjusting the supply of fuel and air, a quench mixer [12]installed at the top end of the high temperature gasification reaction chamber [9], the quench mixer [12]comprising a cooling air inlet pipe [11]at one side thereof, a high temperature furnace gas inlet [7]connected at the lower portion thereof to the top of the high temperature gasification reaction chamber [9], and a quench mixing zone [6]at the other side thereof, the quench mixing zone [6]being developed in a streamline shape, the bottom of the minimum cross section of the mixing zone is provided with a cooling air lower air inlet (5), and the maximum cross section of the quenching mixing zone (6) is connected with a mixed furnace gas outlet pipe (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97107945A CN1051058C (en) | 1997-01-29 | 1997-01-29 | Method for producing particle diantimony trioxide and its device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97107945A CN1051058C (en) | 1997-01-29 | 1997-01-29 | Method for producing particle diantimony trioxide and its device |
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| Publication Number | Publication Date |
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| CN1172769A true CN1172769A (en) | 1998-02-11 |
| CN1051058C CN1051058C (en) | 2000-04-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN97107945A Expired - Lifetime CN1051058C (en) | 1997-01-29 | 1997-01-29 | Method for producing particle diantimony trioxide and its device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100334002C (en) * | 2005-03-11 | 2007-08-29 | 锡矿山闪星锑业有限责任公司 | Method and its device for producing catalyst grade super high purity Sb2O3 |
| CN100393921C (en) * | 2006-04-27 | 2008-06-11 | 王涛 | Method for producing grain sizes even distributed antimony trioxide in single crystal type, and equipment |
| CN112919538A (en) * | 2021-02-26 | 2021-06-08 | 广西华远金属化工有限公司 | Oxygen-enriched production process of catalyst-grade antimony trioxide |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1078502A (en) * | 1992-05-07 | 1993-11-17 | 锡矿山矿务局 | Production method for superfine antimony trioxide |
-
1997
- 1997-01-29 CN CN97107945A patent/CN1051058C/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100334002C (en) * | 2005-03-11 | 2007-08-29 | 锡矿山闪星锑业有限责任公司 | Method and its device for producing catalyst grade super high purity Sb2O3 |
| CN100393921C (en) * | 2006-04-27 | 2008-06-11 | 王涛 | Method for producing grain sizes even distributed antimony trioxide in single crystal type, and equipment |
| CN112919538A (en) * | 2021-02-26 | 2021-06-08 | 广西华远金属化工有限公司 | Oxygen-enriched production process of catalyst-grade antimony trioxide |
| CN112919538B (en) * | 2021-02-26 | 2023-04-11 | 广西华远金属化工有限公司 | Oxygen-enriched production process of catalyst-grade antimony trioxide |
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| Publication number | Publication date |
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| CN1051058C (en) | 2000-04-05 |
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Owner name: XIKUANGSHAN SHANXING ANTIMONY INDUSTRY CO., LTD. Free format text: FORMER NAME OR ADDRESS: TIN MINE MINING AFFAIRS BUREAU |
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Address after: 417502 Lengshuijiang, Hunan Province Patentee after: Tinnery Shanxing Antimony Industry LLC Address before: 417502 Lengshuijiang, Hunan Province Patentee before: Tin Mine Mining Affairs Bureau |
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Granted publication date: 20000405 |
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