CN103771357A - Oxidizing furnace for preparing selenium dioxide with crude selenium and method for preparing selenium dioxide - Google Patents
Oxidizing furnace for preparing selenium dioxide with crude selenium and method for preparing selenium dioxide Download PDFInfo
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- CN103771357A CN103771357A CN201410040626.5A CN201410040626A CN103771357A CN 103771357 A CN103771357 A CN 103771357A CN 201410040626 A CN201410040626 A CN 201410040626A CN 103771357 A CN103771357 A CN 103771357A
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Abstract
The invention relates to the field of refining selenium dioxide with crude selenium, and particularly relates to an oxidizing furnace for preparing selenium dioxide with crude selenium. The oxidizing furnace comprises an oxidizing furnace body, wherein the oxidizing furnace body is provided with an oxygen inlet and a furnace door and is internally provided with an oxygen coil pipe and a feed tray, the oxygen coil pipe is arranged at the upper part in the oxidizing furnace body, the oxygen inlet of the oxygen coil pipe is butt jointed with the oxygen inlet, the oxygen coil pipe is provided with dozens of oxygen outlets, the feed tray is arranged at the bottom in the oxidizing furnace body and is an opening rectangular vessel, the length of the oxygen coil pipe is matched with that of the feed tray, the width of the feed tray is matched with that of the furnace door, and the furnace door is used as a port for putting into and taking out the feed tray. The invention also relates to a method for preparing the selenium dioxide. The new production technology of once feeding substitutes for the previous method of continuously feeding in batches, the grade product rate of SeO299 grade selenium dioxide product is improved to be over 95% from 50%, and the recovery rate of selenium is improved from 90% and stabilized to be over 96%.
Description
Technical field
The invention belongs to chemical industry melting equipment, relate to thick selenium refining tin anhydride field, be specifically related to the oxidized still that a kind of thick selenium is prepared tin anhydride, also relate to the method for preparing tin anhydride, be intended to improve the quality product of tin anhydride.
Background technology
In smart selenium production process, tin anhydride is a kind of work in-process, but the producer that buys smart selenium product conventionally smart selenium can be oxidized be again prepared into tin anhydride as additive for actual suitability for industrialized production.Along with the continuous increase of market to tin anhydride consumption, many Jing Xi manufacturer sells tin anhydride as product, adopt dioxygen oxidation method directly directly to prepare tin anhydride from thick selenium.The thick selenium of most domestic is prepared tin anhydride producer and is used oxidized still system device to carry out oxidation refining.The ultimate principle of the refining tin anhydride dioxygen oxidation method refining of thick selenium is: volatile different according to the oxide compound of selenium and oxide impurity, having oxygen to exist and the condition of heating under, selenium is easily oxidized the volatile tin anhydride of generation; And in thick selenium, most of impurity remains in slag at oxygen exists and the next generation of heating condition is difficult to volatilize Cadmium oxide, arsenic powder etc., so just can reach the object that makes its separation, its sepn process is carried out in oxidized still.At present, in tin anhydride refining is produced, the factor that affects tin anhydride grade is a lot, as oxidizing temperature, oxygen flow, oxidization time, thick selenium grade and thick selenium feed way etc.We find production practice by for many years, adopt continuous charging mode, with oxidized still oxide purification tin anhydride, exist the finished product tin anhydride quality of output unstable, impurity element is higher and the rubescent blackout of tin anhydride etc. problem, the normal production and production marketing of serialization that directly has influence on tin anhydride.
Summary of the invention
The object of the present invention is to provide a kind of thick selenium to prepare the oxidized still of tin anhydride, the present invention also provides the method that uses this oxidized still to prepare tin anhydride; To solve in existing thick selenolite gas oxidation style explained hereafter, the unsettled technical problem of tin anhydride quality.
For this reason, the present invention adopts following technical scheme: a kind of thick selenium is prepared the oxidized still of tin anhydride, comprises oxidation body of heater, and oxidation body of heater is provided with oxygen intake and fire door; It is characterized in that: in oxidation body of heater, be provided with oxygen coil pipe and loading tray; Oxygen coil pipe is positioned at oxidation body of heater internal upper part, and oxygen coil pipe oxygen feeder docks with oxygen intake, and oxygen coil pipe is provided with dozens of paranasal sinuses, and loading tray is positioned at oxidation body of heater inner bottom part.
Loading tray is uncovered rectangular vessel, and the length of oxygen coil pipe and the length of loading tray are suitable; The width of loading tray and the width of fire door are suitable, and fire door is as the putting into of loading tray, conveying end.
Prepare a method for tin anhydride, with the refining tin anhydride of thick selenolite gas oxidation style, use oxidized still, boiler tube and cooling cylinder as equipment; It is characterized in that inserting in loading tray and evenly dividing disposable thick selenium pending every stove, the loading tray that thick selenium is housed is put into oxidation bottom of furnace body from fire door; By the preparation of following technology condition: furnace body temperature is that 540 ℃～560 ℃ or furnace tube temperature are 460 ℃～480 ℃, and oxygen flow is 16L/min; Thick selenium treatment capacity: 13kg/ stove class, 13 kilograms of the thick selenium treatment capacities of every 8 hours every stoves; The number of times of coming out of the stove: the 1 time/stove 8h of class.Scarfing cinder 1 time weekly.
In thick selenium smelting process, often with metal and nonmetal because heating is melted, and then generate its oxide compound steam and volatilize.At a certain temperature, the vapour pressure of different metal element varies in size, thereby their volatilization degree is also different, and dioxygen oxidation is just based on to be controlled at certain temperature, and selenium is different from the volatilization degree of various impurity elements.Basic object of the present invention is to improve tin anhydride quality product, take thick selenolite gas oxidation style as ultimate principle, refining its improvement of tin anhydride is mainly: loading tray and oxygen coil pipe are set in existing oxidized still, remove the loading hopper at oxidized still top, and entering, exporting fire door as loading tray; The charging process that adopts thick selenium once to feed in raw material; Boiler tube and cooling cylinder etc. are not improved, keep prior art.Controlling oxidized still oxidizing temperature is 540 ℃～560 ℃, and selenium is most of at this temperature generates volatile tin anhydride gas with oxygen, reclaims the refining tin anhydride of preparation through condensation, and its physical specification is white needle-like crystals.In thick selenium, most high boiling impurity is non-volatile at this temperature.The particularly oxide compound of these elements, its volatilization temperature is all much higher than the volatilization temperature of tin anhydride.Therefore under oxidizing temperature, impurity and oxide compound thereof remain in the oxidation sludge in oxidized still, so just can reach the object that tin anhydride is separated.
The present invention adopts once the method for continuous charging in batches before reinforced new production process method replacement in thick selenium oxide purification tin anhydride process, to improve the quality product of tin anhydride.Continuous charging method is for to divide the thick selenium of per tour 10kg raw material four times in batches, and each 2.5kg, added once and add from the loading hopper of oxidized still furnace roof every 2 hours; In former production practice, adopt continuous charging method in batches, upwards the selenium steam of volatilization influences each other when we find that thick selenium material enters oxidation stage and in hopper chassis, hinder after material volatilization and the contacting of oxygen, make to contain monomer selenium in the tin anhydride of output, cause product tin anhydride rubicundity, blackout, the tin anhydride qualification rate that per tour is produced only can reach 50%.We,, through test of many times, improve and adopt once after the reinforced mode of production oxidized still, have guaranteed the abundant oxidation of material in oxidized still, effectively reduce the foreign matter content in product tin anhydride, and the qualification rate of tin anhydride is increased to more than 95%.
The present invention changes continuous charging pattern into every 8 hours and disposable thick 13kg selenium is joined in oxidized still loading tray, strengthen feeding quantity, make 8 hours thick selenium treatment capacities of split run bring up to 13kg/ stove class by 10kg/ stove class, and greatly improved up-to-standard rate and the selenium recovery of tin anhydride product.
In People's Republic of China's non-ferrous metal industry standard (tin anhydride part) YS/T 651-2007, stipulate that tin anhydride quality product requires as shown in table 1.
Adopt after reinforced in batches new production process, through the actual production practice more than 1 year, prove greatly to have improved the quality product of tin anhydride.The SeO of tin anhydride
299 trade mark percentages of product all remain on more than 95%, and tin anhydride product meets the regulation of YS/T 651-2007, and selenium recovery is stabilized in more than 96%, have obtained good effect, and the method has high promotional value.Before this, the tin anhydride that original production method is produced, its SeO
299 trade mark percentages of product are only 50% left and right, and selenium recovery is only up to 90%, and through equipment improvement and Technology lifting, the up-to-standard rate of tin anhydride product is increased to more than 95% by 50%, and selenium recovery is by 90% raising and be stabilized in more than 96%.
Accompanying drawing explanation
Fig. 1 be improve before oxidized still and the structural representation of boiler tube and cooling cylinder,
Fig. 2 is the structural representation of oxidized still of the present invention and boiler tube and cooling cylinder,
Fig. 3 is the structural representation of oxygen coil pipe,
Fig. 4 is the left view of Fig. 3,
Fig. 5 is Fig. 3 A-A sectional view,
Fig. 6 is the structural representation of loading tray,
Fig. 7 is the left view of Fig. 6,
Fig. 8 is the vertical view of Fig. 6.
In figure: 1-fire door, 2-oxygen intake, 3-oxidation body of heater, 4-loading hopper, 5-body of heater thermometer hole, 6-pipe connecting, 7-boiler tube, 8-expect clearly flange, 9-cooling cylinder, 10-expect clearly hole, 11-discharge port, 12-oxygen coil pipe, 1201-oxygen feeder, 1202-paranasal sinuses, 13-loading tray, the angle between the vertical medullary ray of the medullary ray of b-paranasal sinuses and coil pipe, the length of L-oxygen coil pipe, the length of L1-loading tray, the width of W-loading tray, the height of H-loading tray.
Embodiment
Oxidized still embodiment is as shown in Figure 2: a kind of thick selenium is prepared the oxidized still of tin anhydride, comprises oxidation body of heater 3, and oxidation body of heater 3 is provided with oxygen intake 2 and fire door 1; In oxidation body of heater 3, be provided with oxygen coil pipe 12 and loading tray 13; Oxygen coil pipe 12 is positioned at oxidation body of heater 3 internal upper parts, referring to Fig. 3, Fig. 4 and Fig. 5: oxygen coil pipe oxygen feeder 1201 docks with oxygen intake 2, oxygen coil pipe 12 is provided with dozens of paranasal sinuses 1202, two adjacent paranasal sinuses 1202 interval 20mm, paranasal sinuses 1202 is positioned at tiltedly below of oxygen coil pipe 12, angle b between the vertical medullary ray of the medullary ray of paranasal sinuses and coil pipe is 45 degree, and loading tray 13 is positioned at oxidation body of heater 3 inner bottom parts.
Add referring to Fig. 6 to Fig. 8: loading tray 13 is uncovered rectangular vessel, and the length L of oxygen coil pipe and the length L of loading tray 1 are suitable; The width W of loading tray and the width of fire door are suitable, fire door 1 is as the putting into of loading tray, conveying end, thick selenium material is directly added by loading tray from oxidized still left side fire door, oxygen does not directly spray in oxidized still, but spray from the paranasal sinuses 1202 that oxygen coil pipe is offered in stove, make oxygen directly spray to loading tray 13 to oblique lower 45 degree, greatly strengthened oxidation effectiveness, and promoted oxygen utilization rate.
Loading tray adopts the thick stainless steel plate of 4mm to be welded; The length L 1 of loading tray is 500mm; The width W of loading tray is 260mm, and the height H of loading tray is 100mm.
A kind of method of preparing tin anhydride of embodiment of the method, with the refining tin anhydride of thick selenolite gas oxidation style, using oxidized still, boiler tube and cooling cylinder is equipment; Insert in loading tray and evenly divide disposable thick selenium pending every stove, the loading tray that thick selenium is housed is put into oxidation bottom of furnace body from fire door; By the preparation of following technology condition: furnace body temperature is that 540 ℃～560 ℃ or furnace tube temperature are 460 ℃～480 ℃, and oxygen flow is 16L/min; Thick selenium treatment capacity: 13kg/ stove class, the number of times of coming out of the stove: the 1 time/stove 8h of class.Scarfing cinder 1 time weekly.
Oxidation furnace structure before improvement is as shown in Figure 1: oxidized still system before comprises oxidation body of heater 3, boiler tube 7 and clear material flange 8, pipe connecting 6 will be oxidized body of heater 3 tops and be communicated with boiler tube 7 tops, boiler tube 7 bottoms are communicated with cooling cylinder 9 tops, oxidation body of heater 3 tops are provided with loading hopper 4, oxidation body of heater 3 tops are also provided with body of heater thermometer hole 5, oxidation body of heater 3 left upper portion are provided with oxygen intake 2, bottom is provided with fire door 1, and cooling cylinder 9 tops are provided with expects clearly that flange 8, right upper portion are provided with and expect that clearly hole 10, bottom, right side are provided with discharge port 11.Reinforced by adding body of heater from top loading hopper, oxygen directly sprays in oxidized still oxidation reinforced by left side oxygen intake, thus thick selenium material from loading hopper add while entering oxidation stage with hopper chassis the selenium steam that upwards volatilizees influence each other, hinder after material volatilization and the contacting of oxygen, after the volatilization of part selenium simple substance, directly enter into cooling cylinder by boiler tube, make to contain monomer selenium in the tin anhydride of output, cause product tin anhydride rubicundity, blackout, if condensation reclaim tin anhydride as intermediate material for the preparation of selenium ingot, can after purification, reduction, the further removal of impurities of operation such as washing, if but the tin anhydride that condensation is reclaimed is directly off quality as production marketing.
Claims (5)
1. thick selenium is prepared an oxidized still for tin anhydride, comprises oxidation body of heater, and oxidation body of heater is provided with oxygen intake and fire door; It is characterized in that: in oxidation body of heater (3), be provided with oxygen coil pipe (12) and loading tray (13); Oxygen coil pipe (12) is positioned at oxidation body of heater (3) internal upper part, and oxygen coil pipe oxygen feeder (1201) docks with oxygen intake (2), and oxygen coil pipe (12) is provided with dozens of paranasal sinuses (1202), and loading tray (13) is positioned at oxidation body of heater (3) inner bottom part.
2. a kind of thick selenium as claimed in claim 1 is prepared the oxidized still of tin anhydride, it is characterized in that: two adjacent paranasal sinuses (1202) interval 20mm, paranasal sinuses (1202) is positioned at tiltedly below of oxygen coil pipe (12), and the angle (b) between the vertical medullary ray of the medullary ray of paranasal sinuses and coil pipe is 45 degree.
3. a kind of thick selenium as claimed in claim 1 or 2 is prepared the oxidized still of tin anhydride, it is characterized in that: loading tray (13) is uncovered rectangular vessel, and the length (L) of oxygen coil pipe is suitable with the length (L1) of loading tray; The width (W) of loading tray is suitable with the width of fire door.
4. a kind of thick selenium as claimed in claim 3 is prepared the oxidized still of tin anhydride, it is characterized in that: the length (L1) of loading tray is 500mm, and the width (W) of loading tray is 260mm, and the height (H) of loading tray is 100mm.
5. prepare a method for tin anhydride, with the refining tin anhydride of thick selenolite gas oxidation style, use oxidized still, boiler tube and cooling cylinder as equipment; It is characterized in that inserting in loading tray and evenly dividing disposable thick selenium pending every stove, the loading tray that thick selenium is housed is put into oxidation bottom of furnace body from fire door; By the preparation of following technology condition: furnace body temperature is that 540 ℃～560 ℃ or furnace tube temperature are 460 ℃～480 ℃, and oxygen flow is 16L/min; Thick selenium treatment capacity: 13kg/ stove class, the number of times of coming out of the stove: the 1 time/stove 8h of class.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410040626.5A CN103771357B (en) | 2014-01-28 | 2014-01-28 | Thick selenium is prepared the oxidized still of tin anhydride and is prepared the method for tin anhydride |
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| CN201410040626.5A CN103771357B (en) | 2014-01-28 | 2014-01-28 | Thick selenium is prepared the oxidized still of tin anhydride and is prepared the method for tin anhydride |
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| CN103771357B CN103771357B (en) | 2015-09-30 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104477860A (en) * | 2015-01-14 | 2015-04-01 | 盐城市科强电器有限公司 | Selenium oxidation production device |
| CN104743526A (en) * | 2015-03-27 | 2015-07-01 | 大冶有色金属有限责任公司 | Refining process of crude selenium |
| CN111689478A (en) * | 2020-06-11 | 2020-09-22 | 黄湛明 | Preparation method and preparation system of high-purity nano selenium powder |
| CN112173450A (en) * | 2020-09-04 | 2021-01-05 | 广东长信精密设备有限公司 | Recycling equipment for industrial selenium-depleted material |
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| CN101987725A (en) * | 2009-08-07 | 2011-03-23 | 铜陵有色金属集团控股有限公司 | Method and equipment for producing selenium dioxide by using crude selenium as raw material |
| CN202208640U (en) * | 2011-09-14 | 2012-05-02 | 江西铜业股份有限公司 | Selenium oxide generating device |
| CN203699912U (en) * | 2014-01-28 | 2014-07-09 | 白银有色集团股份有限公司 | Oxidation furnace for preparing selenium dioxide from coarse selenium |
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2014
- 2014-01-28 CN CN201410040626.5A patent/CN103771357B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101987725A (en) * | 2009-08-07 | 2011-03-23 | 铜陵有色金属集团控股有限公司 | Method and equipment for producing selenium dioxide by using crude selenium as raw material |
| CN202208640U (en) * | 2011-09-14 | 2012-05-02 | 江西铜业股份有限公司 | Selenium oxide generating device |
| CN203699912U (en) * | 2014-01-28 | 2014-07-09 | 白银有色集团股份有限公司 | Oxidation furnace for preparing selenium dioxide from coarse selenium |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104477860A (en) * | 2015-01-14 | 2015-04-01 | 盐城市科强电器有限公司 | Selenium oxidation production device |
| CN104477860B (en) * | 2015-01-14 | 2016-06-01 | 盐城市科强电器有限公司 | A kind of selenolite production equipment |
| CN104743526A (en) * | 2015-03-27 | 2015-07-01 | 大冶有色金属有限责任公司 | Refining process of crude selenium |
| CN111689478A (en) * | 2020-06-11 | 2020-09-22 | 黄湛明 | Preparation method and preparation system of high-purity nano selenium powder |
| CN111689478B (en) * | 2020-06-11 | 2022-01-28 | 黄湛明 | Preparation method and preparation system of high-purity nano selenium powder |
| CN112173450A (en) * | 2020-09-04 | 2021-01-05 | 广东长信精密设备有限公司 | Recycling equipment for industrial selenium-depleted material |
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| CN103771357B (en) | 2015-09-30 |
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