CN1168664C - Method for controlling grain size in preparation of antimony trioxide by using lead antimony alloy - Google Patents
Method for controlling grain size in preparation of antimony trioxide by using lead antimony alloy Download PDFInfo
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- CN1168664C CN1168664C CNB011363568A CN01136356A CN1168664C CN 1168664 C CN1168664 C CN 1168664C CN B011363568 A CNB011363568 A CN B011363568A CN 01136356 A CN01136356 A CN 01136356A CN 1168664 C CN1168664 C CN 1168664C
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Abstract
The present invention relates to a method for controlling grain size in the preparation of antimony trioxide by lead antimony alloy. The method is characterized in that after air is heated by a heater 8, the air is evenly filled in the metal liquid face in a furnace by an air box 4, an air matching plate 7 and an air guide pipe 3 so that an alloy fused body containing 10-90% of Pb, and 90 to 10% of Sb is directly heated; metallic antimony is volatilized and oxidized under the condition that the temperature of the fused body is stabilized below 700 DEG C; the antimony trioxide which is obtained by oxidation can be cooled and crystallized at regulable hollow cavity temperature (150 to 550 DEG C) to obtain the antimony trioxide of which the average particle size is in a range of 0.3 to 5 mu m.
Description
The present invention relates to domain of inorganic chemistry, particularly, the present invention relates to a kind of method of control size size when preparing antimonous oxide with lead antimony alloy.
In the prior art, people adopt the method and apparatus of oxidation jamesonite to produce antimonous oxide usually, the chemical index of the antimonous oxide that this method is produced meets or exceeds tradition is produced antimonous oxide with star metal level, but the particle size of antimonous oxide is uncontrollable, can only form the very thin product of a kind of granularity naturally.And the very thin antimonous oxide applicable narrow range in flame retardant area of granularity, consumption is also little, has restricted the development of existing antimonous oxide production technology.Therefore, in order to satisfy flame retardant area to the requirement of antimonous oxide and the development of promotion antimonous oxide industry, people need the antimonous oxide product of various size ranges, need objectively the method for prior art is improved.The present invention proposes for solving such problem just.
The purpose of this invention is to provide a kind of by operating the method for controlling the high purity Sb 2 O 3 that obtains various sizes.
For achieving the above object, the present invention has increased by a cover heating unit, air is heated, the temperature of air is controlled to heat by well heater, warm air directly heats alloy melt, utilize antimony, the plumbous characteristic different with vapour pressure with the fusing point of other alloy, metallic antimony volatilization oxidation, the antimonous oxide that oxidation obtains is at cavity (cavity: be meant liquid metal liquid level top, divide the airduct outer wall, the space that air distribution plate and body of heater surround, the cavity temperature is the temperature of liquid metal ullage space) middle crystallisation by cooling, the cavity temperature can be regulated and control, the cavity temperature that can regulate and control is controlled in the 150-550 ℃ of scope, obtain the antimonous oxide of mean sizes in 0.3～5 mu m range, realize controllability the antimonous oxide globule size.Same set of device can be adjusted and give hot device as required, reaches corresponding crystallisation by cooling temperature condition, produces the antimonous oxide (being stibium trioxide) of multiple granularity specification.
Technical process of the present invention is simple, and facility investment is little, and industrial being easy to realize, is applicable to that lead antimony alloy that any ratio, any method obtain produces the antimonous oxide of various granularity specifications.Be further described below in conjunction with accompanying drawing:
Description of drawings:
Accompanying drawing 1 is the process flow sheet of the inventive method, and wherein 1 is the heat supply chamber, the 2nd, and dog-house, the 3rd, guide duct, the 4th, gas tank, the 5th, induced exhaust, the 6th, dust chamber, the 7th, air distribution plate, the 8th, well heater, the 9th, crucible oxidized still body of heater, the 10th, delivery pipe, the 11st, cavity.
The crucible type oxidized still that accompanying drawing 1 has been described controlled globule size is produced the synoptic diagram of antimonous oxide.Oxidized still has a crucible oxidized still body of heater 9, and the air distribution plate 7 that has guide duct 3 is installed in this stove, and its top is gas tank 4, and the gas tank right side is a well heater 8; The oxidized still bottom fills alloy melt; Alloy melt top is the cavity 11 of crystallisation by cooling; Air distribution plate 7 is equipped with induced exhaust 5 and passes gas tank 4, communicates with dust chamber 6 through citation damper; Guide duct 3 on the air distribution plate 7 is communicated with gas tank 4 and melt liquid upper surface; Gas tank 4 is communicated with well heater 8 again; Body of heater 9 has alloy input port or slag removing hole 2; The body of heater bottom has delivery pipe 10, is used to discharge the low antimony alloy melt.
Accompanying drawing 1 has been described process implementing process of the present invention, and lead antimony alloy is melted in dog-house 2 is put into the crucible oxidized still, and this alloy is handled through arsenic removal, and it is low to contain arsenic, generally contains between Sb90-10%, the Pb10-90%; Heat supply chamber 1 links to each other with crucible type oxidized still body of heater 9, and indirect heating crucible formula oxidized still body of heater 9 when blow-on and handling failure is for ordinary production is offered help; Through the warm air direct heating alloy melt of guide duct 3, under warm air and reaction heat acting in conjunction, make the alloy melt temperature-stable below 700 ℃; Air enters well heater 8 heating from the air channel, enter bellows 4 then, distributes to guide duct 3 through air distribution plate 7, evenly blasts air or the oxygen-rich air of pressure at 900-5000Pa from well heater 8 alloy surface in stove, makes alloy melt be in relative static conditions; Adjust the heat of giving of well heater 8, the cavity temperature of burner hearth is remained between 150-550 ℃, can obtain the antimonous oxide crystalline powder of granularity mean sizes at 0.3～5 μ m.The inventor is through discovering antimonous oxide crystalline cavity temperature and its granular relevant, cavity temperature height, the crystalline powder granularity that obtains is big, the cavity temperature is low, and the crystalline powder granularity that obtains is little, can obtain the different antimonous oxide of granularity by control cavity temperature.Control cavity temperature is at 150-550 ℃, preferred 250-500 ℃, can obtain the granularity mean sizes at 0.3～5 μ m, antimonous oxide in preferred 0.5～3 mu m range, therefore, can be according to actual needs, by regulating a certain temperature section of cavity temperature in the said temperature scope, obtain the antimonous oxide of required mean particle size, realize controllability the antimonous oxide globule size.Regularly remove the alloy surface coverture from dog-house 2, to keep the bright and clean of alloy surface; When Sb content less than 10% the time, stop oxygen blast, from delivery pipe 10 beginning blowings, i.e. the low stibium crude lead of discharging, and passing on potroom, to extract electricity plumbous, anode sludge fusion is cast and is recycled into oxidized still behind the alloy and blows antimony; Meanwhile control the citation damper of induced exhaust 5 places dresses, according to conventional methods, the mixed gas of burner hearth is introduced bagroom 6, obtain meeting the antimonous oxide of national 0 grade standard, i.e. stibium trioxide through collection with controlled underbalance.
Compared with prior art, method of the present invention has the following advantages:
1, by regulation and control cavity temperature, obtain the antimonous oxide crystalline powder of different mean particle sizes, realize controllability to the antimonous oxide granularity;
2, need the equipment of increase few, controlled variable is also few, and operation is easily gone, and can realize automatization or semi-automation;
3, thermo-efficiency height, throughput can improve more than 15%, and quality product is more stable, and cost reduces about 10%;
4, same set of device can be produced the product of multiple granularity specification, and market adaptability is strong, and the finished product appreciate more than 10% than the product of original single grain size category.
Further specify the present invention below by embodiment.The preparation method who it should be understood that the embodiment of the invention is only used for illustrating the present invention, rather than limitation of the present invention, and the simple modifications to preparation method of the present invention under design prerequisite of the present invention all belongs to the scope of protection of present invention.Except as otherwise noted, the percentage ratio among the present invention all is weight percentage.In addition, unit " T " is " ton ".
Below with 7.2M
2The crucible type oxidized still be example, use method of the present invention and produce varigrained antimonous oxide.Wherein, when oxidized still contains the alloy of Sb＜35%, 100 tons of monthly output stibium trioxides; Suitably keep Sb when 35-55%, 150 tons of monthly output stibium trioxides.Concrete experimental data is as follows:
Embodiment 1:
Alloy ingredient after the refining arsenic removal (%):
Element: Pb Sb As Ag
Content: 58.31 41.67 0.02 1.8Kg/T
The antimonous oxide index that the cloth bag powder gathers dust: (150-180 ℃ of cavity temperature)
Element: Sb
2O
3PbO As whiteness (Wr) mean particle size 325 order percent of pass
Content: 99.68% 0.08% 0.031% 95.3 0.35 μ m 100%
Lead bullion composition (%):
Element: Pb Sb Ag
Content: 89.62 10.1 2.77Kg/T
Embodiment 2:
Alloy ingredient after the refining arsenic removal (%):
Element: Pb Sb As Ag
Content: 44.47 55.31 0.02 2.0Kg/T
The antimonous oxide index that the cloth bag powder gathers dust: (300-320 ℃ of cavity temperature)
Element: Sb
2O
3PbO As whiteness (Wr) mean particle size 325 order percent of pass
Content: 99.63% 0.085% 0.03% 94.5 0.63 μ m 100%
Lead bullion composition (%):
Element: Pb Sb Ag
Content: 89.72 9.87 3.2Kg/T
Embodiment 3:
Alloy ingredient after the refining arsenic removal (%):
Element: Pb Sb As Ag
Content: 35.47 64.31 0.02 2.5Kg/T
The antimonous oxide index that the cloth bag powder gathers dust: (460-480 ℃ of cavity temperature)
Element: Sb
2O
3PbO As whiteness (Wr) mean particle size 325 order percent of pass
Content: 99.65% 0.093% 0.032% 93.5 2.51 μ m 100%
Lead bullion composition (%):
Element: Pb Sb Ag
Content: 87.23 12.12 4.1Kg/T
Claims (3)
1. one kind prepares granularity control method in the antimonous oxide with lead antimony alloy, this method heats air through well heater (8) after, evenly blast to stove inner metal liquid face by bellows (4), air distribution plate (7) and guide duct (3), make alloy melt be subjected to direct heating, under melt temperature is stabilized in condition below 700 ℃, with the metallic antimony oxidation of volatilizing, the antimonous oxide that oxidation obtains crystallisation by cooling in cavity, the cavity temperature that can regulate and control is controlled between 150-550 ℃, obtains mean particle size antimonous oxide in the 0.3-5 mu m range.
2. according to the process of claim 1 wherein that lead antimony alloy contains Pb10-90%, Sb90-10%.
3. according to the method for claim 2, wherein the cavity temperature is controlled between 250-500 ℃, obtains mean particle size antimonous oxide in the 0.5-3.5 mu m range.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011363568A CN1168664C (en) | 2001-10-11 | 2001-10-11 | Method for controlling grain size in preparation of antimony trioxide by using lead antimony alloy |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011363568A CN1168664C (en) | 2001-10-11 | 2001-10-11 | Method for controlling grain size in preparation of antimony trioxide by using lead antimony alloy |
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| CN1412118A CN1412118A (en) | 2003-04-23 |
| CN1168664C true CN1168664C (en) | 2004-09-29 |
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| CNB011363568A Expired - Fee Related CN1168664C (en) | 2001-10-11 | 2001-10-11 | Method for controlling grain size in preparation of antimony trioxide by using lead antimony alloy |
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| CN102616846B (en) * | 2012-04-05 | 2014-09-24 | 广西华锑科技有限公司 | Gas-phase cooling crystallization device for antimony white furnace |
| CN113720867B (en) * | 2021-10-11 | 2024-01-30 | 昆明理工大学 | Method for preparing antimony trioxide standard sample of scanning electron microscope |
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