CN1412118A - 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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- CN1412118A CN1412118A CN 01136356 CN01136356A CN1412118A CN 1412118 A CN1412118 A CN 1412118A CN 01136356 CN01136356 CN 01136356 CN 01136356 A CN01136356 A CN 01136356A CN 1412118 A CN1412118 A CN 1412118A
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Abstract
The method for controlling grain size of antimony troxide being in course of its preparation by using lead-anitmony alloy is characterized by implementing the following steps: using heater to heat air, utilizing air box, air-distributing palte and air tube to uniformly blow the hot air into the metal liquid surface in the furnace to directly heat alloy melt body containing 10-90% of Pb and 90-10% of Sb, under the condition of that the melt temp. is stabilized below 700 deg.C making metal antimony volatilize and oxidate, cooling and crystallizing the obtained antimony trioxide in the adjustable and controllable hollow cavity temp. (150-550 deg.C) so as to obtain the antimony trioxide whose average grain size is in range of 0.3-5 mirometers.
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.
Accompanying drawing 1 has been described the crucible type oxidation furnace of controlled granule size and has been produced showing of antimony oxide Intention. Oxidation furnace has a crucible oxidation furnace body of heater 9, is equipped with in this stove to have guide duct 3 Air distribution plate 7, its top are gas tank 4, and the gas tank right side is heater 8; The oxidation furnace bottom fills Alloy melt; Alloy melt top is the cavity 11 of crystallisation by cooling; Air distribution plate 7 is equipped with air inducing Pipe 5 passes gas tank 4, communicates with dust chamber 6 through citation damper; Guide duct 3 on the air distribution plate 7 Be communicated with gas tank 4 and melt liquid upper surface; Gas tank 4 is communicated with heater 8 again; Body of heater 9 is opened Ladle refining mouth or breast hole 2 are arranged; Lower portion of furnace body has delivery pipe 10, is used for the low antimony of discharging and closes The gold melt.
Accompanying drawing 1 has been described process implementing process of the present invention, and lead-antimony alloy is thrown through dog-house 2 Enter in the crucible oxidation furnace to melt, this alloy is processed through arsenic removal, and it is low to contain arsenic, generally contains Sb90-10%, between the Pb10-90%; Link to each other with crucible type oxidation furnace body of heater 9 for hot cell 1, opening Indirect heating crucible formula oxidation furnace body of heater 9 when stove and handling failure is for ordinary production is offered help; Hot-air through guide duct 3 directly heats alloy melt, in hot-air and reaction heat acting in conjunction Lower, make the alloy melt temperature stabilization below 700 ℃; Air enters heater 8 heating from the air channel, Enter then bellows 4, distribute to guide duct 3 through air distribution plate 7, close in from heater 8 to stove Gold surface evenly blasts pressure at air or the oxygen-enriched air of 900-5000Pa, makes alloy melt Be in relative static conditions; Adjust the heat of giving of heater 8, the cavity temperature of burner hearth is kept Between 150-550 ℃, can obtain the granularity average-size in three oxidations of 0.3～5 μ m Two antimony crystalline powders. The inventor finds through research, the cavity temperature of antimony oxide crystallization With its granular relevant, cavity temperature height, the crystalline powder granularity that obtains is big, and the cavity temperature is low, The crystalline powder granularity that obtains is little, can obtain three different oxygen of granularity by control cavity temperature Change two antimony. Control cavity temperature preferred 250-500 ℃, can get at 150-550 ℃ Arrive the granularity average-size at 0.3～5 μ m, three oxidations in preferred 0.5～3 mu m range Two antimony, therefore, can be according to actual needs, by regulating the cavity temperature in the said temperature scope In a certain temperature section, obtain the antimony oxide of required particle mean size, realize three oxidations two The controllability of antimony granule size. Regularly remove the alloy surface covering from dog-house 2, to keep Alloy surface bright and clean; When Sb content less than 10% the time, stop oxygen blast, from delivery pipe 10 Blowing, i.e. the low stibium crude lead of discharging, and passing on potroom, to extract electricity plumbous, earth of positive pole melting is cast Be recycled into oxidation furnace behind the alloy and blow antimony; Meanwhile control the citation damper of induced duct 5 places dress, root According to conventional method, with controlled underbalance the mist of burner hearth is introduced bagroom 6, through receiving Collection obtains meeting the antimony oxide of national 0 grade standard, i.e. stibium trioxide.
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: the antimonous oxide index that 58.31 41.67 0.02 1.8Kg/T cloth bag powder gather 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 compositions (%): 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: the antimonous oxide index that 44.47 55.31 0.02 2.0Kg/T cloth bag powder gather 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 compositions (%): 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: the antimonous oxide index that 35.47 64.31 0.02 2.5Kg/T cloth bag powder gather 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 compositions (%): 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 |
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| 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 true CN1412118A (en) | 2003-04-23 |
| CN1168664C 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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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616846A (en) * | 2012-04-05 | 2012-08-01 | 广西华锑科技有限公司 | Gas-phase cooling crystallization device for antimony white furnace |
| CN113720867A (en) * | 2021-10-11 | 2021-11-30 | 昆明理工大学 | Method for preparing antimony trioxide standard sample of scanning electron microscope |
-
2001
- 2001-10-11 CN CNB011363568A patent/CN1168664C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616846A (en) * | 2012-04-05 | 2012-08-01 | 广西华锑科技有限公司 | Gas-phase cooling crystallization device for antimony white furnace |
| 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 |
| CN113720867A (en) * | 2021-10-11 | 2021-11-30 | 昆明理工大学 | Method for preparing antimony trioxide standard sample of scanning electron microscope |
| 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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| CN1168664C (en) | 2004-09-29 |
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