CN100334002C - Method and its device for producing catalyst grade super high purity Sb2O3 - Google Patents
Method and its device for producing catalyst grade super high purity Sb2O3 Download PDFInfo
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Abstract
The present invention discloses a method and a device for producing catalyst grade super high purity Sb2O3. The production method of the present invention is characterized in that the compressed air of 0.1 to 0.8MPa is sprayed to the surface of antimony liquid from the top of an antimony oxide furnace, and one of the following two modes is used, wherein one mode comprises that each position of a reaction area of a furnace chamber is heated to more than 1100 DEG C in a mode that partial heat quantity is supplied by the indirect heating of an electrical heating element, and the center temperature of the reaction area is more than 1200 DEG C; the other mode comprises that the fume of the furnace chamber is led in a high-temperature gasifying reaction chamber so that Sb2O3 fume is rapidly heated to 1100 to 1600 DEG C; then, the high-temperature antimony trioxide fume is cooled by a quenching mixing device, and dust is collected by a cloth bag to obtain an Sb2O3 product. The used production device is the improved antimony oxide furnace. Compared with the publicly known plasma production method and the device thereod, the product produced by the present inveniton reduces energy consumption by more than 70%, has furnace yield of 6 to 15 t/d and reduces production cost by more than 30%. The present invention has the advantages of simple and convenient operation, easy control of technological parameters, stable and reliable product quality, etc.
Description
Technical field
The present invention relates to a kind of production method and device thereof of catalyst grade super high purity Sb 2 O 3, especially relate to a kind of pyrogenic process production method and device thereof of catalyst grade super high purity Sb 2 O 3.
Background technology
Antimonous oxide is as the catalyzer of polyester polycondensation reaction process, removes and requires the product purity height, do not contain high price four weisspiessglanzs, require that also high catalytic activity is arranged and in ethylene glycol high solvability, require the whiteness height of product, the b value is low, cubic content height.Be used for the antimonous oxide of electronic ceramics, fluorescent material industry, then require the purity height, foreign matter content is low.
Catalyst grade super high purity Sb 2 O 3 mainly adopts thermal process to be prepared at present, as Chinese invention patent 92103430.x disclosed " plasma antimony oxide furnace with reflection type dual-reaction chamber ", adopt metallic antimony in the first reaction chamber voloxidation, enter second reaction chamber and plasma flow effect, the gasiform antimonous oxide through water jacket and air quenched, obtains the catalyst grade antimonous oxide in the exit.Chinese invention patent 88103221.2 disclosed " plasma method is produced the antimonous oxide ultrafine powder ", be to be raw material with the antimonous oxide, with the DC arc plasma high-temperature generator is under the thermal source, with antimonous oxide gasification cooling, obtain superfine antimony trioxide, if raw material adopts the lower antimonous oxide of impurity, its products obtained therefrom can satisfy the service requirements of catalyst grade super high purity Sb 2 O 3.But these two kinds of processing methodes all have stove day output low (1-2t/d), product energy consumption height, shortcoming such as product yield is low.
Chinese invention patent 85102489 disclosed " a kind of stibium trioxide stove of reverberatory furnace structure ", it is the raw material production antimonous oxide with the metallic antimony, utilize the exothermic oxidation reaction of antimony, process is carried out 950-1000 ℃ of self-heating, contain four weisspiessglanzs of 0.1-0.2% in the product, do not meet the requirement of catalyst grade super high purity Sb 2 O 3.
The method and the device of No. 00126692.6 disclosed production stibium trioxide of Chinese invention patent application, only heating unit is installed at furnace roof, and heating unit is exposed in the interior oxidizing atmosphere of burner hearth, under the high temperature oxidation condition in stove, the easy loss of heating unit, and enter product with flue gas, thus product is polluted, do not meet the requirement of catalyst grade super high purity Sb 2 O 3.
Disclosed method for producing particle diantimony trioxide of Chinese invention patent ZL97107945.5 and device, the product that obtains meets the requirement of catalyst grade super high purity Sb 2 O 3, but because of what utilize is the stibium trioxide stove of traditional reverberatory furnace structure, the secondary air feed pipe of antimony oxidizing reaction is positioned at the high temperature combustors bottom, the easy burn through of air feed pipe causes complicated operation.
Summary of the invention
Purpose of the present invention is intended to overcome the defective that above-mentioned prior art exists, provide a kind of energy consumption low, the output height, product direct yield height, production cost are low, easy and simple to handle, the production method of the catalyst grade super high purity Sb 2 O 3 of stable and reliable product quality and device thereof.
The production method of catalyst grade super high purity Sb 2 O 3 of the present invention may further comprise the steps: (1) drops into metallic antimony after stibium trioxide stove furnace temperature is risen to 700 ℃ in stove, makes it fusing; (2) adopt the mode of pressurized air from the liquid top blast, spray into the pressurized air of 0.1-0.8MPa to antimony liquid surface, make the antimony voloxidation, and by being installed in the electrical heating element in stibium trioxide stove furnace roof, the furnace wall, indirect heating supply part heat, temperature in the burner hearth conversion zone is brought up to more than 1100 ℃, and conversion zone central authorities temperature is more than 1200 ℃; (3) in stibium trioxide stove high-temperature flue gas top reaction compartment exit, by a flue gas quenching equipment, control high temperature antimonous oxide flue gas total amount is 1 with the ratio of quench air amount: 2-10 (preferred 1: 6-8), make the quenching of high temperature antimonous oxide flue gas be cooled to 60-300 ℃, products obtained therefrom bag collection systematic collection promptly gets full cubic crystal model, high purity, high whiteness, hangs down the catalyst grade super high purity Sb 2 O 3 product of b value.
The production method of catalyst grade super high purity Sb 2 O 3 of the present invention also can adopt following steps: (1) drops into metallic antimony after stibium trioxide stove furnace temperature is risen to 700 ℃ in stove, makes it fusing; (2) adopt the mode of pressurized air from the liquid top blast, spray into the pressurized air of 0.1-0.8MPa to antimony liquid surface, make the antimony voloxidation, flue gas is imported a high-temperature gasification reaction chamber, by burning to this reaction chamber fueling, make the antimonous oxide flue gas be warmed up to 1100-1600 ℃ (preferred temperature is 1200-1400 ℃) rapidly, and form a kind of equally distributed gaseous phase through this high-temperature gasification reaction chamber; (3) in high-temperature gasification reaction chamber exit, carry out quenching with a large amount of cooling airs, the high-temperature flue gas total amount of control trioxygen-containingization two antimony is 1 with the ratio of cooling air volume: 2-10 (preferred 1: 6-8), make it be cooled to 60-300 ℃ in moment, products obtained therefrom bag collection systematic collection promptly gets full cubic crystal model, high purity, high whiteness, hangs down the catalyst grade super high purity Sb 2 O 3 product of b value.
Use the production method of the present invention's catalyst grade super high purity Sb 2 O 3, the modified version stibium trioxide stove with following structure that should select the present invention for use is as production equipment, described stibium trioxide furnace body top is provided with movable installation can spray into compressed-air actuated nozzle to antimony liquid surface, the internal diameter in the same way doubly apart from 1-12 at nozzle and flue gas top reaction compartment center to this pyroreaction chamber, jet exit can be regulated in the 20-400mm scope apart from antimony liquid surface distance, furnace roof and tail end inwall are separately installed with heating unit, (purpose is to prevent heating unit oxidation loss under the high temperature oxidation condition to be respectively equipped with the thermostable heat-conductive plate that heating unit and burner hearth are separated between heating unit and the burner hearth, prolong heating unit work-ing life, and prevent loss thing polluted product), the furnace roof surface coverage has the heat insulating layer, the outlet of high-temperature flue gas top reaction compartment is provided with quenching mixer, one side of quenching mixer is a blast inlet on the cooling air, what the bottom of quenching mixer and high-temperature flue gas top reaction compartment closely linked to each other is the high-temperature flue gas import, the quenching mixer opposite side is the chilling mixing zone, the chilling mixing zone is streamlined expansion, blast inlet under the cooling air is arranged under it, and chilling mixing zone cross section maximum links to each other with the cooled flue gas outlet pipe.
Use the production method of the present invention's catalyst grade super high purity Sb 2 O 3, the modified version stibium trioxide stove with following structure that also can select the present invention for use is as production equipment, comprise the stibium trioxide furnace body, the body of heater top is provided with movable installation can spray into compressed-air actuated nozzle to antimony liquid surface, the internal diameter in the same way doubly apart from 1-12 at nozzle and center, pyroreaction chamber, flue gas top to this pyroreaction chamber, jet exit can be regulated in the 20-400mm scope apart from antimony liquid surface distance, the burner hearth smoke outlet is provided with the high-temperature gasification reaction chamber, 1-4 burner of inwall distribution that this reaction chamber is made with refractory materials, but this burner and a cover independently fuel of fuel metering and air feed rate link to each other with air supply system, high-temperature flue gas outlet end at the high-temperature gasification reaction chamber is provided with a quenching mixer, one side of quenching mixer is a blast inlet on the cooling air, what the bottom of quenching mixer and high-temperature gasification reaction chamber closely linked to each other is the high-temperature flue gas import, the quenching mixer opposite side is the chilling mixing zone, the chilling mixing zone is streamlined expansion, blast inlet under the cooling air is arranged under it, chilling mixing zone cross section maximum links to each other with the cooled flue gas outlet pipe, stibium trioxide stove one end is provided with fiery chamber, is used for the molten antimony of baker and blow-on.
Production method and device thereof with known plasma method catalyst grade super high purity Sb 2 O 3 compare, use the present invention to produce catalyst grade super high purity Sb 2 O 3, energy consumption reduces more than 70%, furnace output can reach 6-15t/d, production cost can reduce more than 30%, and have advantages such as easy and simple to handle, stable and reliable product quality.
Description of drawings
Fig. 1 is the structural representation of production equipment stibium trioxide stove one embodiment of the present invention;
Fig. 2 is the structural representation of another embodiment of production equipment stibium trioxide stove of the present invention.
Embodiment
The invention will be further described below in conjunction with drawings and Examples.
With reference to Fig. 1, this stibium trioxide stove embodiment comprises body of heater 1a, described body of heater 1a top is provided with movable installation can spray into compressed-air actuated nozzle 3 to antimony liquid surface, furnace roof and tail end inwall are separately installed with heating unit 5,15, heating unit 5,15 and burner hearth 2 between be respectively equipped with heating unit 5, the 15 thermostable heat-conductive plates of being separated with burner hearth 24,14 (purpose is to prevent heating unit 5, oxidation loss under 15 hot conditionss, prolong element work-ing life, and prevent loss thing polluted product), the furnace roof surface coverage has heat insulating layer 6,13 outlets of high-temperature flue gas top reaction compartment are provided with quenching mixer 9, one side of quenching mixer 9 is blast inlets 7 on the cooling air, what the bottom of quenching mixer 9 and high-temperature flue gas top reaction compartment 13 closely linked to each other is high-temperature flue gas import 8, quenching mixer 9 opposite sides are chilling mixing zone 11, chilling mixing zone 11 is streamlined expansion, blast inlet 12 under the cooling air is arranged under it, chilling mixing zone 11 cross section maximums link to each other with cooled flue gas outlet pipe 10, are provided with charging opening 16 at stibium trioxide stove one end.
In said apparatus, nozzle 3 outlets can be regulated in the 20-400mm scope apart from antimony liquid surface distance, fire-resistant heat-conducting plate 4,14 is a refractory materials, and heating unit 5,15 is a globars, and 8 times of the distances at nozzle 3 and flue gas top reaction compartment 13 centers are to the internal diameter in the same way of this reaction chamber 13.
With reference to Fig. 2, this stibium trioxide stove embodiment comprises body of heater 1b, described body of heater 1b top is provided with movable the installation and sprays into compressed-air actuated nozzle 3 to antimony liquid surface, the burner hearth exhanst gas outlet is provided with high-temperature gasification reaction chamber 17, the inwall 18 distribution 1-4 burner 20 that these gasification reactor chamber 17 usefulness refractory materialss are made, but fuel that burner 20 is required and air by a cover independently the plenum system 19 of fuel metering and air feed rate supply with, high-temperature flue gas outlet end at high-temperature gasification reaction chamber 17 is provided with quenching mixer 9, one side of quenching mixer 9 is blast inlets 7 on the cooling air, what the bottom of quenching mixer 9 and high-temperature gasification reaction chamber 17 closely linked to each other is high-temperature flue gas import 8, quenching mixer 9 opposite sides are chilling mixing zone 11, chilling mixing zone 11 is streamlined expansion, blast inlet 12 under the cooling air is arranged under it, chilling mixing zone 11 cross section maximums link to each other with cooled flue gas outlet pipe 10, stibium trioxide stove 1b one end has a fiery chamber 21, is used for the molten antimony of baker and blow-on.
In said apparatus, nozzle 3 can be regulated in the 20-400mm scope apart from antimony liquid surface distance, and 6 times of the distances at nozzle 3 outlet and high-temperature gasification reaction chamber 17 centers are to the internal diameter in the same way of this high-temperature gasification reaction chamber 17.
Be the embodiment of production method of the present invention below:
Embodiment 1: production equipment adopts stibium trioxide stove shown in Figure 1, with the metallic antimony is raw material, its chemical ingredients is Sb 99.89%, Pb 0.05%, and As 0.02%, and Fe 0.011%, after by heating unit 5,15 furnace temperature being risen to 700 ℃, drop into the metallic antimony fusing in burner hearth 2, when treating that fusion antimony liquid reaches more than 2 tons in the stove, the pressurized air that sprays into 0.1-0.8MPa to antimony liquid surface makes the antimony voloxidation; Thereby spray into the compressed air require on antimony liquid surface and carry out supplementary heating with heating unit 5,15 by regulating the compressed air pressure adjusting, the antimonous oxide flue-gas temperature is brought up to more than 1200 ℃, when flue gas leaves pyroreaction chamber 13 and enters quenching mixer 9, control high temperature antimonous oxide flue gas total amount is 1: 6 with the ratio of quench air amount, per hour in stove, drop into metallic antimony 300kg, products obtained therefrom bag collection systematic collection, per hour get antimonous oxide product 340kg, the physical and chemical index detected result of 10 tons of products of one of them lot number is as follows:
Sb
2O
3 99.90％ As?0.018％
Pb 0.032％ Fe?0.0015％
EG dissolving transmittance 98.8% dissolving with hydrochloric acid turbidity 3.6ppm
Whiteness 98.1% b value 0.95
Mean particle size 0.61 μ m cubic 99.2%.
Embodiment 2: used metallic antimony chemical ingredients is Sb 99.96%, and Pb 0.005%, and As 0.0048%, and Fe 0.011%, and all the other conditions are with embodiment 1, and the physical and chemical index detected result of its products obtained therefrom is as follows:
Sb
2O
3?99.94％ As 0.0041％
Pb 0.004.3％ Fe 0.0010％
EG dissolving transmittance 99.1% dissolving with hydrochloric acid turbidity 3.9ppm
Whiteness 98.5% b value 0.90
Mean particle size 0.58 μ m cubic 99.3%
Embodiment 3: production equipment adopts stibium trioxide stove shown in Figure 2, with the metallic antimony is raw material, its chemical ingredients is Sb 99.90%, As 0.03%Pb 0.04%, Fe 0.014%, when rising to furnace temperature more than 700 ℃ by fiery chamber 21 usefulness cokes, dropping into metallic antimony melts, when treating that fusion antimony liquid reaches more than 2 tons in the stove, the pressurized air that sprays into 0.1-0.8MPa to antimony liquid surface makes the antimony voloxidation, stopping fiery chamber 21 simultaneously heats up, by regulating compressed air pressure, thereby regulate the compressed air require that sprays into antimony liquid surface, the reaction in furnace temperature is brought up to more than 1100 ℃, with liquefied petroleum gas (LPG) or other fuel, the temperature of keeping in the gasification reactor chamber 17 is 1300-1500 ℃, when flue gas leaves gasification reactor chamber 17 and enters quenching mixer 9, control high temperature antimonous oxide flue gas total amount is 1: 8 with the ratio of quench air total amount, per hour in stove, drop into metallic antimony 350kg, products obtained therefrom bag collection systematic collection, per hour obtain antimonous oxide product 397kg, the physical and chemical index detected result of its representative product is:
Sb
2O
3?99.91％ As?0.022％
Pb 0.029％ Fe?0.0010％
EG dissolution rate transmittance 99.0% dissolving with hydrochloric acid turbidity 5.2ppm
Whiteness 98.4% b value 0.92
Mean particle size 0.31 μ m cubic 99.5%.
Embodiment 4: be raw material with the metallic antimony, its chemical ingredients is Sb 99.95%, and As 0.005%, Pb0.0046%, and Fe 0.018%, and the gasification reaction chambers temp is 1200-1400 ℃, and all the other are with embodiment 3, and the physical and chemical index detected result of products obtained therefrom is:
Sb
2O
3 99.95％ As?0.0047％
Pb 0.0040％ Fe?0.0009％
EG dissolving transmittance 98.9% dissolving with hydrochloric acid turbidity 4.6ppm
Whiteness 98.9% b value 0.89
Mean particle size 0.41 μ m cubic 99.2%.
Claims (6)
1, a kind of catalyst grade super high purity Sb 2 O 3 production method is characterized in that, may further comprise the steps:
(1) stibium trioxide stove furnace temperature is risen to 700 ℃ after, in stove, drop into metallic antimony, make it the fusing; (2) pressurized air that sprays into 0.1-0.8MPa to antimony liquid surface makes the antimony voloxidation, and by being installed in the electrical heating element in stibium trioxide stove furnace roof, the furnace wall, indirect heating supply part heat is brought up to whole burner hearth reaction zone temperature more than 1100 ℃, and burner hearth central authorities temperature is more than 1200 ℃; (3) in stibium trioxide stove high-temperature flue gas top reaction compartment exit, by the flue gas quenching equipment, control high temperature antimonous oxide flue gas total amount is 1 with the ratio of quench air amount: 2-10 makes the quenching of high temperature antimonous oxide flue gas be cooled to 60-300 ℃, products obtained therefrom bag collection systematic collection.
2, catalyst grade super high purity Sb 2 O 3 production method according to claim 1 is characterized in that, the high-temperature flue gas total amount of described antimonous oxide is 1 with the ratio of cooling air volume: 6-8.
3, a kind of catalyst grade super high purity Sb 2 O 3 production method is characterized in that, may further comprise the steps: (1) drops into metallic antimony after stibium trioxide stove furnace temperature is risen to 700 ℃ in stove, makes it fusing; (2) spray into the pressurized air of 0.1-0.8MPa to antimony liquid surface, make the antimony voloxidation, the antimonous oxide flue gas is imported a high-temperature gasification reaction chamber, by burning to this reaction chamber fueling, make the antimonous oxide flue gas be warmed up to 1100-1600 ℃ rapidly, and form a kind of equally distributed gaseous phase through this high-temperature gasification reaction chamber; (3) in high-temperature gasification reaction chamber exit, by the flue gas quenching equipment, control high temperature antimonous oxide flue gas total amount is 1 with the ratio of cooling air volume: 2-10 makes high temperature antimonous oxide flue gas moment be cooled to 60-300 ℃, products obtained therefrom bag collection systematic collection.
4, catalyst grade super high purity Sb 2 O 3 production method according to claim 3, it is characterized in that, make the antimonous oxide flue gas be warmed up to 1200-1400 ℃ rapidly through described high-temperature gasification chamber, the high-temperature flue gas total amount of described antimonous oxide is 1 with the ratio of cooling air volume: 6-8.
5, a kind of enforcement claim 1 or 3 described catalyst grade super high purity Sb 2 O 3 production method stibium trioxide stoves, comprise body of heater, it is characterized in that, the body of heater top is provided with movable the installation and sprays into compressed-air actuated nozzle to antimony liquid surface, the internal diameter in the same way doubly apart from 1-12 at nozzle and center, pyroreaction chamber, flue gas top to this pyroreaction chamber, jet exit is regulated in the 20-400mm scope apart from antimony liquid surface distance, furnace roof and tail end inwall are separately installed with heating unit, be respectively equipped with the thermostable heat-conductive plate that heating unit and burner hearth are separated between heating unit and the burner hearth, the furnace roof surface coverage has the heat insulating layer, the outlet of high-temperature flue gas top reaction compartment is provided with quenching mixer, one side of quenching mixer is a blast inlet on the cooling air, what the bottom of quenching mixer and high-temperature flue gas top reaction compartment closely linked to each other is the high-temperature flue gas import, the quenching mixer opposite side is the chilling mixing zone, the chilling mixing zone is streamlined expansion, blast inlet under the cooling air is arranged under it, and chilling mixing zone cross section maximum links to each other with the cooled flue gas outlet pipe.
6, a kind of enforcement claim 1 or 3 described catalyst grade super high purity Sb 2 O 3 production method stibium trioxide stoves, comprise body of heater, it is characterized in that, the body of heater top is provided with movable the installation and sprays into compressed-air actuated nozzle to antimony liquid surface, nozzle and high-temperature gasification reaction chamber center, flue gas top apart from 1-12 doubly to this high-temperature gasification reaction chamber internal diameter in the same way, jet exit is regulated in the 20-400mm scope apart from antimony liquid surface distance, the burner hearth smoke outlet is provided with the high-temperature gasification reaction chamber, 1-4 burner of inwall distribution that this reaction chamber is made with refractory materials, burner and one overlaps independently, and the fuel of fuel metering and air feed rate links to each other with air supply system, high-temperature flue gas outlet end at the high-temperature gasification reaction chamber is provided with a quenching mixer, one side of quenching mixer is a blast inlet on the cooling air, what the bottom of quenching mixer and high-temperature gasification reaction chamber closely linked to each other is the high-temperature flue gas import, the quenching mixer opposite side is the chilling mixing zone, the chilling mixing zone is streamlined expansion, blast inlet under the cooling air is arranged under it, chilling mixing zone cross section maximum links to each other with the cooled flue gas outlet pipe, and stibium trioxide stove one end is provided with the fiery chamber that is used for baker and the molten antimony of blow-on.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101559980B (en) * | 2009-05-19 | 2012-12-05 | 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 |
| CN102602995B (en) * | 2012-04-05 | 2014-07-23 | 广西华锑科技有限公司 | Production method of large-particle-size antimonous oxide |
| CN102616847B (en) * | 2012-04-05 | 2014-03-26 | 广西华锑科技有限公司 | Method for preparing catalyst grade antimony trioxide |
| CN104355332B (en) * | 2014-10-20 | 2017-01-11 | 郑香萍 | Preparation device of antimony trioxide for polyester |
| CN104591280B (en) * | 2015-01-15 | 2016-05-11 | 益阳市华昌锑业有限公司 | A kind of natural gas is smelted preparation technology and the device of antimony oxide |
| CN106698513B (en) * | 2017-01-09 | 2018-03-02 | 上海深化实业有限公司 | A kind of preparation method of antimony oxide superfine powder |
| 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 |
| CN113277555B (en) * | 2021-05-18 | 2022-05-20 | 湖南娄底华星锑业有限公司 | Preparation method of high-purity antimony trioxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1172769A (en) * | 1997-01-29 | 1998-02-11 | 锡矿山矿务局 | Method for producing particle diantimony trioxide and its device |
| CN1354137A (en) * | 2000-11-17 | 2002-06-19 | 刘伯龙 | Method for producing antimony white and its special equipment |
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2005
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1172769A (en) * | 1997-01-29 | 1998-02-11 | 锡矿山矿务局 | Method for producing particle diantimony trioxide and its device |
| CN1354137A (en) * | 2000-11-17 | 2002-06-19 | 刘伯龙 | Method for producing antimony white and its special equipment |
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