CN102602995B - Production method of large-particle-size antimonous oxide - Google Patents
Production method of large-particle-size antimonous oxide Download PDFInfo
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- CN102602995B CN102602995B CN201210097318.7A CN201210097318A CN102602995B CN 102602995 B CN102602995 B CN 102602995B CN 201210097318 A CN201210097318 A CN 201210097318A CN 102602995 B CN102602995 B CN 102602995B
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Abstract
The invention discloses a production method of large-particle-size antimonous oxide, which adopts a reflection-type antimony white furnace for melting. The production method comprises the following steps in sequence: (a) increasing the temperature of the antimony white furnace (1) to be 1000 DEG C by a diesel burner, and then putting metallic antimony in the furnace so as to melt the metallic antimony into antimony liquid; (b) blowing top-blown wind and side-blown wind to the antimony liquid surface respectively through wind pipes (2) arranged on the top and the walls of the antimony white furnace (1) so as to oxidize antimony for volatilization, introducing furnace gas into a reaction room (3) to conduct oxidation reaction; (c) guiding high-temperature furnace gas out from the reaction room (3), then introducing the high-temperature furnace gas into a circular multi-baffle crystallizer (6), and simultaneously, blowing cooling air to the circular multi-baffle crystallizer (6) so as to control the crystallization temperature to be 500-600 DEG C; and (d) cooling crystalline particles by a cooling tower (5) again, and finally, collecting finished products by a dust collector (7). According to the method, the working procedures are simple, the process is short, the degree of automation is high, the production and the operation can be controlled stably, and the direct recovery rate of the product is high.
Description
Technical field
The invention belongs to pyrogenic process and produce the method field of antimonous oxide, related in particular to the production method of the large particle diameter antimonous oxide that a kind of production capacity is high, direct yield is high.
Background technology
Weisspiessglanz is a kind of high-performance refractory synergistic additive, is widely used in the fields such as electronic apparatus, automobile, weaving, communication, military project.Large particle diameter (less colored power weisspiessglanz) is the weisspiessglanz high-end product that a kind of median size is greater than 2.1 μ m, because its flame retarding efficiency is high, consumption is few, the addition impact of performance on material and look female is little, non-other fire retardants of cost performance can be equal to, be exclusively used in dark color or colorful flame-retardant plastics, resin, textiles, therefore the international market price of this product is more much higher than the price of common weisspiessglanz.
At present, domestic pyrogenic process is produced large particle diameter antimonous oxide technique, and general method is that Horizontal type grain coarsening device is installed on stibium trioxide stove reaction chamber, then isolates qualified coarse particle antimony trioxide production method [97107946.3] through winnowing extension set.There is certain shortcoming in this method: while adopting Horizontal type cooling crystallizer, coarse particles crystal, than the great duct bottom that is easily deposited on, forms even blocking pipe of fouling, cause producing and interrupt, cause production process many, production capacity is low, direct yield is low, and production cost is high, equipment complexity.Therefore, people begin one's study and improve the production method of antimonous oxide, if Chinese Patent Application No. is 200610018991.1 to disclose a kind of monocrystalline type, the uniform antimonous oxide production method of size distribution and device thereof, it is the method that adopts reflective stibium trioxide stove to smelt, antimony reflective stibium trioxide stove through fusing after, air is blasted to the antimony liquid level of melting in burner hearth, make antimony be oxidized to antimonous oxide furnace gas, then cooling, crystallization, discharge from furnace gas export pipe, the process trapping by dust collecting system again, it is characterized in that: after the furnace gas that is oxidized to antimonous oxide is drawn, first pass through air-cooled reactor, follow in crystallizer through three grades of cooling and crystallizations, then discharge from furnace gas export pipe, obtain monocrystalline type with dust collecting system trapping again, size distribution is even and be unimodal, median size 0.2 ~ 3.5 μ m, principal constituent Sb
20
399.6%, the senior antimonous oxide that 325 screen residues are less than 0.003%, whiteness is greater than 98.5%.But being still after this improvement do not reach existing production requirement.
Summary of the invention
The object of the invention is to, for existing deficiency, provides a kind of production method of large particle diameter antimonous oxide.
To achieve these goals, the present invention has adopted following technical scheme: a kind of production method of large particle diameter antimonous oxide is the method that adopts reflective stibium trioxide stove to smelt, and it is characterized in that, the method comprises the following steps successively:
(1) with diesel fuel burner, the furnace temperature of stibium trioxide stove is risen to after 1000 DEG C, in stove, drop into metallic antimony, make it to be fused into antimony liquid, and keep the temperature of antimony liquid between 900～1000 DEG C;
(2) airduct arranging on the furnace roof by stibium trioxide stove, furnace wall blasts respectively top blast wind and cross air blow to antimony liquid, makes antimony voloxidation, maintains furnace temperature at 1100～1200 DEG C simultaneously; Antimony steam and airborne oxygen continue oxidizing reaction occurs after entering reaction chamber, and keep the temperature of reaction chamber at 1080～1200 DEG C;
(3) high-temperature furnace gas from reaction chamber out, enter circular many baffle plates crystallizer, blast cooling air by intake stack to many baffle plates of circle crystallizer simultaneously, crystallization control temperature is at 500～600 DEG C;
(4) crystalline particle is cooling through cooling tower again, and finally collecting median size with dust-precipitator is that 2.1～4.5 μ m and size distribution are unimodal, principal constituent Sb
2o
3the antimonous oxide that ratio is greater than 99.6%, 325 screen residues are less than 0.003%, colourity L value is greater than 98.
The air pressure of described top blast wind is 0.4～0.6MPa, and airshed is 200～400m
3/ h; The air pressure of described cross air blow is 0.4～0.6MPa, and airshed is 80～200m
3/ h; The described airshed that blasts cooling air to many baffle plates of circle crystallizer is 500～1000m
3/ h.
Described many baffle plates of circle crystallizer internal derangement diagonal angle is provided with baffle plate, and the obliquity of baffle plate is 45 °.
1 airduct is installed on the furnace roof of described stibium trioxide stove, 4 airducts are installed on furnace wall.
Described intake stack is arranged on the junction of reaction chamber and circular many baffle plates crystallizer.
Advantage of the present invention:
1, production method of the present invention has that production capacity is large, product direct yield is high, cost is low, operation quick-reading flow sheets is short, level of automation is high, production operation control stable, raw material is adaptable, the large particle diameter antimonous oxide product that can produce different size, has significant economic benefit.
2, being installed on furnace roof airduct is one, and the airduct of furnace wall is 4, and top blast can make temperature maintenance everywhere in stibium trioxide stove evenly, fluctuate and be not more than 50 DEG C with side-blown combination, uniform distribution of temperature field in reaction chamber, and antimony steam is fully oxidized.
3, the present invention does not need winnowing to divide device separation circuit, adopt many baffle plates of circle crystallizer of original creation, make in stove high temperature oxidation antimony gas out crystallizer, form turbulent area during through 4 grades of choked flow baffle plates, thereby increasing nucleus produces quantity and extends crystallization time, the temperature of controlling well in crystallizer is at 500～600 DEG C, nucleus can fully be grown up, finally reach the antimonous oxide of 2.1～4.5 μ m, through further cooling, finally catch and obtain large particle diameter (less colored power) antimonous oxide product by bagroom, be that coarse particle antimony trioxide production method and device output thereof described in [97107946.3] patent is large more than 1.7 times than publication number, cost is low by 40～60%, quality is better and stable, there is obvious economic benefit.
Brief description of the drawings
Fig. 1 is the structural representation of the device that uses in method of the present invention.
Reference numeral: stibium trioxide stove 1, airduct 2, reaction chamber 3, baffle plate 4, cooling tower 5, circular many baffle plates crystallizer 6, dust-precipitator 7, intake stack 8.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further described.
Embodiment 1: No. two antimony slabs taking Sb content as 98.66%, as raw material, are produced 18.2 tons of large particle diameter antimonous oxide products daily, and median size 2.5 μ m and size distribution are unimodal, principal constituent Sb
2o
3the step of the production method of the antimonous oxide product that be 99.65%, 325 screen residues is less than 0.003%, colourity L value is 98.7 is:
1. first with diesel fuel burner, the furnace temperature of the stibium trioxide stove (1) of 6m2 is risen to after 1000 DEG C, in stove, drop into metallic antimony, make it to be fused into antimony liquid, and keep the temperature of antimony liquid at 900 DEG C;
2. 4 airducts (2) that arrange on 1 airduct (2) arranging on the furnace roof by stibium trioxide stove (1) and furnace wall blast respectively top blast wind and cross air blow to antimony liquid level, make antimony voloxidation, maintain furnace temperature at 1100 DEG C simultaneously; Antimony steam and airborne oxygen enter reaction chamber (3) to be continued oxidizing reaction occurs afterwards, and keeps the temperature of reaction chamber (3) at 1080 DEG C; The air pressure of top blast wind is 0.4MPa, and airshed is 200m
3/ h; The air pressure of described cross air blow is 0.4MPa, and airshed is 80m
3/ h;
3. high-temperature furnace gas from reaction chamber (3) out, enter dislocation diagonal angle and many baffle plates of circle crystallizer (6) of 45 ° of 4 baffle plates of installation (4) that tilt, blast cooling air by intake stack (8) to many baffle plates of circle crystallizer (6), the airshed of cooling air is 500m simultaneously
3/ h, crystallization control temperature is at 500 DEG C;
4. crystalline particle is cooling through cooling tower (5) again, finally uses dust-precipitator (7) to collect finished product.
Embodiment 2: No. two antimony slabs taking Sb content as 98.66%, as raw material, are produced 20.1 tons of large particle diameter antimonous oxide products daily, and median size 3.4 μ m and size distribution are unimodal, principal constituent Sb
2o
3the step of the production method of the antimonous oxide product that be 99.67%, 325 screen residues is less than 0.003%, colourity L value is 98.4 is:
1. first with diesel fuel burner, the furnace temperature of the stibium trioxide stove (1) of 6m2 is risen to after 1000 DEG C, in stove, drop into metallic antimony, make it to be fused into antimony liquid, and keep the temperature of antimony liquid at 950 DEG C;
2. 4 airducts (2) that arrange on 1 airduct (2) arranging on the furnace roof by stibium trioxide stove (1) and furnace wall blast respectively top blast wind and cross air blow to antimony liquid level, make antimony voloxidation, maintain furnace temperature at 1150 DEG C simultaneously; Antimony steam and airborne oxygen enter reaction chamber (3) to be continued oxidizing reaction occurs afterwards, and keeps the temperature of reaction chamber (3) at 1140 DEG C; The air pressure of top blast wind is 0.5MPa, and airshed is 300m
3/ h; The air pressure of described cross air blow is 0.5MPa, and airshed is 150m
3/ h;
3. high-temperature furnace gas from reaction chamber (3) out, enter dislocation diagonal angle and many baffle plates of circle crystallizer (6) of 45 ° of 4 baffle plates of installation (4) that tilt, blast cooling air by intake stack (8) to many baffle plates of circle crystallizer (6), the airshed of cooling air is 800m simultaneously
3/ h, crystallization control temperature is at 550 DEG C;
4. crystalline particle is cooling through cooling tower (5) again, finally uses dust-precipitator (7) to collect finished product.
Embodiment 3: No. two antimony slabs taking Sb content as 98.66%, as raw material, are produced 19.7 tons of large particle diameter antimonous oxide products daily, and median size 4.5 μ m and size distribution are unimodal, principal constituent Sb
2o
3the step of the production method of the antimonous oxide product that be 99.61%, 325 screen residues is less than 0.003%, colourity L value is 98.1 is:
1. first with diesel fuel burner, the furnace temperature of the stibium trioxide stove (1) of 6m2 is risen to after 1000 DEG C, in stove, drop into metallic antimony, make it to be fused into antimony liquid, and keep the temperature of antimony liquid at 1000 DEG C;
2. 4 airducts (2) that arrange on 1 airduct (2) arranging on the furnace roof by stibium trioxide stove (1) and furnace wall blast respectively top blast wind and cross air blow to antimony liquid level, make antimony voloxidation, maintain furnace temperature at 1200 DEG C simultaneously; Antimony steam and airborne oxygen enter reaction chamber (3) to be continued oxidizing reaction occurs afterwards, and keeps the temperature of reaction chamber (3) at 1200 DEG C; The air pressure of top blast wind is 0.6MPa, and airshed is 400m3/h; The air pressure of described cross air blow is 0.6MPa, and airshed is 200m
3/ h;
3. high-temperature furnace gas from reaction chamber (3) out, enter dislocation diagonal angle and many baffle plates of circle crystallizer (6) of 45 ° of 4 baffle plates of installation (4) that tilt, blast cooling air by intake stack (8) to many baffle plates of circle crystallizer (6), the airshed of cooling air is 500m simultaneously
3/ h, crystallization control temperature is at 600 DEG C;
4. crystalline particle is cooling through cooling tower (5) again, finally uses dust-precipitator (7) to collect finished product.
Claims (4)
1. a production method for large particle diameter antimonous oxide, is the method that adopts reflective stibium trioxide stove to smelt, and it is characterized in that, the method comprises the following steps successively:
1. with diesel fuel burner, the furnace temperature of stibium trioxide stove (1) is risen to after 1000 DEG C, in stove, drop into metallic antimony, make it to be fused into antimony liquid, and keep the temperature of antimony liquid between 900～1000 DEG C;
2. the airduct (2) arranging on the furnace roof by stibium trioxide stove (1), furnace wall blasts respectively top blast wind and cross air blow to antimony liquid level, makes antimony voloxidation, maintains furnace temperature at 1100～1200 DEG C simultaneously; Antimony steam and airborne oxygen enter reaction chamber (3) to be continued oxidizing reaction occurs afterwards, and keeps the temperature of reaction chamber (3) at 1080～1200 DEG C;
3. high-temperature furnace gas from reaction chamber (3) out, enter circular many baffle plates crystallizer (6), blast cooling air by intake stack (8) to many baffle plates of circle crystallizer (6) simultaneously, crystallization control temperature is at 500～600 DEG C; Described many baffle plates of circle crystallizer (6) internal derangement diagonal angle is provided with baffle plate (4), and the obliquity of baffle plate (4) is 45 °;
4. crystalline particle is cooling through cooling tower (5) again, and finally using dust-precipitator (7) to collect median size is that 2.1～4.5 μ m and size distribution are unimodal, principal constituent Sb
2o
3the antimonous oxide that ratio is greater than 99.6%, 325 screen residues are less than 0.003%, colourity L value is greater than 98.
2. the production method of large particle diameter antimonous oxide according to claim 1, is characterized in that: the air pressure of described top blast wind is 0.4～0.6MPa, and airshed is 200～400m
3/ h; The air pressure of described cross air blow is 0.4～0.6MPa, and airshed is 80～200m
3/ h; The described airshed that blasts cooling air to many baffle plates of circle crystallizer (6) is 500～1000m
3/ h.
3. the production method of large particle diameter antimonous oxide according to claim 1, is characterized in that: 1 airduct (2) is installed on the furnace roof of described stibium trioxide stove (1), 4 airducts (2) are installed on furnace wall.
4. the production method of large particle diameter antimonous oxide according to claim 1, is characterized in that: described intake stack (8) is arranged on the junction of reaction chamber (3) and circular many baffle plates crystallizer (6).
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| CN201210097318.7A CN102602995B (en) | 2012-04-05 | 2012-04-05 | Production method of large-particle-size antimonous oxide |
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| CN103508490B (en) * | 2013-08-23 | 2014-12-17 | 湖南辰州矿业股份有限公司 | Multi-functional upper expanding device for producing antimony trioxide |
| CN110483027B (en) * | 2019-08-26 | 2022-01-28 | 湖南辰州矿业有限责任公司 | Refractory air duct for producing antimony oxide and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101559980A (en) * | 2009-05-19 | 2009-10-21 | 广西日星金属化工有限公司 | Method for producing catalyst level antimony oxide and special antimony white furnace thereof |
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| CN1339612A (en) * | 2000-08-18 | 2002-03-13 | 夏延波 | Process for directly producing super fine antimony trioxide by volatilizing smelting in blast furnace and its special equipment |
| 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 |
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| CN101559980A (en) * | 2009-05-19 | 2009-10-21 | 广西日星金属化工有限公司 | Method for producing catalyst level antimony oxide and special antimony white furnace thereof |
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