CN103771357B - Thick selenium is prepared the oxidized still of tin anhydride and is prepared the method for tin anhydride - Google Patents
Thick selenium is prepared the oxidized still of tin anhydride and is prepared the method for tin anhydride Download PDFInfo
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- CN103771357B CN103771357B CN201410040626.5A CN201410040626A CN103771357B CN 103771357 B CN103771357 B CN 103771357B CN 201410040626 A CN201410040626 A CN 201410040626A CN 103771357 B CN103771357 B CN 103771357B
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Abstract
The present invention relates to thick selenium refining tin anhydride field, be specifically related to the oxidized still that thick selenium prepares tin anhydride, comprise oxidation body of heater, oxidation body of heater is provided with oxygen intake and fire door; Oxygen coil pipe and loading tray is provided with in oxidation body of heater; 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, the length of oxygen coil pipe and the length of loading tray suitable; The width of loading tray and the width of fire door suitable, fire door is as the putting into of loading tray, conveying end.The invention still further relates to the method preparing tin anhydride, adopt the method for continuous charging in batches before once reinforced new production process method replacement, the SeO of tin anhydride product
299 trade mark percentages of product are increased to more than 95% by 50%, and selenium recovery improves by 90% and is stabilized in more than 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 prepares tin anhydride, also relate to the method preparing tin anhydride, be intended to the quality product improving tin anhydride.
Background technology
In smart selenium production process, tin anhydride is a kind of work in-process, but smart selenium can be oxidized and is prepared into tin anhydride and is used in actual suitability for industrialized production as additive by producer usually again that buy smart selenium product.Along with market is to the continuous increase of tin anhydride consumption, tin anhydride is sold as product by many Jing Xi manufacturers, namely adopts 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 that thick selenium refines the refining of tin anhydride dioxygen oxidation method is: according to the oxide compound of selenium and the volatile different of oxide impurity, and under the condition having oxygen existence and heating, selenium is easily oxidized and generates volatile tin anhydride; And in thick selenium, most of impurity remains in slag at oxygen exists and under heating condition, then generation is difficult to volatilize Cadmium oxide, arsenic powder etc., so just can reach the object making it be separated, its sepn process is carried out in oxidized still.At present, in tin anhydride refining is produced, the factor affecting tin anhydride grade is a lot, as oxidizing temperature, oxygen flow, oxidization time, thick selenium grade and thick selenium feed way etc.By production practice for many years, we find, adopt continuous charging mode, with oxidized still oxide purification tin anhydride, the finished product tin anhydride quality that there is output is unstable, impurity element is higher and the rubescent blackout of tin anhydride etc. problem, and the serialization directly having influence on tin anhydride is normally produced and production marketing.
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 using this oxidized still to prepare tin anhydride; To solve in existing thick selenolite gas oxidation style explained hereafter, the technical problem of tin anhydride quality instability.
For this reason, the present invention adopts following technical scheme: a kind of thick selenium prepares 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, the length of oxygen coil pipe and the length of loading tray suitable; The width of loading tray and the width of fire door suitable, fire door is as the putting into of loading tray, conveying end.
Prepare a method for tin anhydride, refine tin anhydride with thick selenolite gas oxidation style, use oxidized still, boiler tube and cooling cylinder as equipment; It is characterized in that disposable for thick selenium pending for every stove inserting in loading tray also evenly to divide, the loading tray that thick selenium is housed is put into oxidation bottom of furnace body from fire door; Prepare by following technology condition: furnace body temperature is 540 DEG C ~ 560 DEG C or furnace tube temperature is 460 DEG C ~ 480 DEG C, and oxygen flow is 16L/min; Thick selenium treatment capacity: 13kg/ stove class, the i.e. thick selenium treatment capacity 13 kilograms of every 8 hours every stoves; To come out of the stove number of times: 1 time/stove class 8h.Scarfing cinder 1 time weekly.
In thick selenium smelting process, often with metal with nonmetally to melt due to heating, and then generate its oxide vapor and volatilize.At a certain temperature, the vapour pressure of different metal element varies in size, and thus their volatilization degree is also different, and under dioxygen oxidation is just based on and controls certain temperature, selenium is different from the volatilization degree of various impurity element.Basic object of the present invention improves tin anhydride quality product, refine its improvement of tin anhydride with thick selenolite gas oxidation style for ultimate principle to be mainly: in existing oxidized still, arrange loading tray and oxygen coil pipe, eliminate the loading hopper at oxidized still top, and using fire door as the entering of loading tray, export; Adopt the charging process that thick selenium once feeds in raw material; Boiler tube and cooling cylinder etc. are not improved, keeps prior art.Controlled oxidization stove oxidizing temperature is 540 DEG C ~ 560 DEG C, and selenium at this temperature major part and oxygen generates volatile tin anhydride gas, and reclaim the refining tin anhydride of preparation through condensation, its physical specification is white needle-like crystals.In thick selenium, most high boiling impurity is then non-volatile at such a 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 then remain in the oxidation sludge in oxidized still, so just can reach the object making tin anhydride be separated.
The present invention adopts the method for continuous charging in batches before once 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 divide the thick selenium of per tour 10kg raw material four times in batches, each 2.5kg, adds once add from the loading hopper of oxidized still furnace roof every 2 hours; In former production practice, adopt continuous charging method in batches, the selenium steam upwards volatilized when we find that thick selenium material enters oxidation stage and in hopper chassis influences each other, hinder material to volatilize afterwards and the contact of oxygen, make in the tin anhydride of output containing monomer selenium, cause product tin anhydride rubicundity, blackout, the tin anhydride qualification rate that per tour is produced only can reach 50%.We are through test of many times, give to improve and after adopting the once reinforced mode of production to oxidized still, and ensure that fully oxidized in oxidized still of material, effectively reduce the foreign matter content in product tin anhydride, the qualification rate of tin anhydride is increased to more than 95%.
Continuous charging pattern is changed into every 8 hours and disposablely joins in oxidized still loading tray by thick for 13kg selenium by the present invention, increase feeding quantity, make split run 8 hours thick selenium treatment capacities bring up to 13kg/ stove class by 10kg/ stove class, and substantially increase up-to-standard rate and the selenium recovery of tin anhydride product.
Defining tin anhydride quality product in People's Republic of China's non-ferrous metal industry standard (tin anhydride part) YS/T 651-2007 requires as shown in table 1.
After adopting new production process reinforced in batches, through the actual production practice more than 1 year, prove the quality product substantially increasing 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%, achieve good effect, and the method has high promotional value.Before this, i.e. the tin anhydride of original production method production, its SeO
299 trade mark percentages of product are only about 50%, and selenium recovery, only up to 90%, promotes through equipment improvement and Technology, and the up-to-standard rate of tin anhydride product is increased to more than 95% by 50%, and selenium recovery improves by 90% and is stabilized in more than 96%.
Accompanying drawing explanation
Fig. 1 is oxidized still before improving and the structural representation of boiler tube and cooling cylinder thereof,
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 flange clearly, 9-cooling cylinder, 10-expect hole clearly, 11-discharge port, 12-oxygen coil pipe, 1201-oxygen feeder, 1202-paranasal sinuses, 13-loading tray, the angle between the medullary ray of b-paranasal sinuses and the vertical medullary ray of 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 prepares 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; Oxygen coil pipe 12 and loading tray 13 is provided with in oxidation body of heater 3; Oxygen coil pipe 12 is positioned at oxidation body of heater 3 internal upper part, see 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 oxygen coil pipe 12 tiltedly below, angle b between the medullary ray of paranasal sinuses and the vertical medullary ray of coil pipe is 45 degree, and loading tray 13 is positioned at oxidation body of heater 3 inner bottom part.
Add see Fig. 6 to Fig. 8: loading tray 13 is uncovered rectangular vessel, and the length L of oxygen coil pipe and the length L1 of loading tray is suitable; The width W of loading tray and the width of fire door suitable, fire door 1 is as the putting into of loading tray, conveying end, thick selenium material is directly added from fire door on the left of oxidized still by loading tray, oxygen does not directly spray in oxidized still, but spray from the paranasal sinuses 1202 that oxygen coil pipe in stove is offered, make oxygen directly spray to loading tray 13 to oblique lower 45 degree, greatly strengthen oxidation effectiveness, and improve oxygen utilization rate.
Loading tray adopts the thick stainless steel plate of 4mm to be welded; The length L1 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 preparing tin anhydride of embodiment of the method, refines tin anhydride with thick selenolite gas oxidation style, uses oxidized still, boiler tube and cooling cylinder to be equipment; Disposable for thick selenium pending for every stove inserting in loading tray is also evenly divided, the loading tray that thick selenium is housed is put into oxidation bottom of furnace body from fire door; Prepare by following technology condition: furnace body temperature is 540 DEG C ~ 560 DEG C or furnace tube temperature is 460 DEG C ~ 480 DEG C, and oxygen flow is 16L/min; Thick selenium treatment capacity: 13kg/ stove class, number of times of coming out of the stove: 1 time/stove class 8h.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 expects flange 8 clearly, pipe connecting 6 will be oxidized body of heater 3 top and be communicated with boiler tube 7 top, boiler tube 7 bottom is communicated with cooling cylinder 9 top, oxidation body of heater 3 top is provided with loading hopper 4, oxidation body of heater 3 top is also provided with body of heater thermometer hole 5, oxidation body of heater 3 left upper portion is provided with oxygen intake 2, bottom is provided with fire door 1, and cooling cylinder 9 top is provided with material flange 8, right upper portion clearly and is provided with material hole 10, bottom right side clearly and is provided with discharge port 11.Reinforced by adding in 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 enter oxidation stage time and hopper chassis the selenium steam that upwards volatilizees influence each other, hinder material to volatilize afterwards and the contact of oxygen, part selenium simple substance is direct after volatilizing enters into cooling cylinder by boiler tube, make in the tin anhydride of output containing monomer selenium, cause product tin anhydride rubicundity, blackout, if condensation reclaim tin anhydride as intermediate material for the preparation of selenium ingot, can in purification afterwards, reduction, the further removal of impurities of operation such as washing, but if the tin anhydride that condensation is reclaimed is directly as production marketing, off quality.
Claims (4)
1. thick selenium prepares 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 prepares the oxidized still of tin anhydride, it is characterized in that: two adjacent paranasal sinuses (1202) interval 20mm, paranasal sinuses (1202) is positioned at oxygen coil pipe (12) tiltedly below, and the angle (b) between the medullary ray of paranasal sinuses and the vertical medullary ray of coil pipe is 45 degree.
3. a kind of thick selenium as claimed in claim 1 or 2 prepares 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 prepares 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.
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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 true CN103771357B (en) | 2015-09-30 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN104743526B (en) * | 2015-03-27 | 2016-08-17 | 大冶有色金属有限责任公司 | A kind of thick selenium process for refining |
| CN111689478B (en) * | 2020-06-11 | 2022-01-28 | 黄湛明 | Preparation method and preparation system of high-purity nano selenium powder |
| CN112173450B (en) * | 2020-09-04 | 2022-08-09 | 江苏先导微电子科技有限公司 | 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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Patent Citations (3)
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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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| 延长二氧化硒氧化炉内胆使用寿命的措施;侯琼英 等;《技术改造》;20101231(第6期);第43-46页 * |
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