CN1676638A - Metal antimony purifying method and apparatus - Google Patents
Metal antimony purifying method and apparatus Download PDFInfo
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- CN1676638A CN1676638A CNA2005100107620A CN200510010762A CN1676638A CN 1676638 A CN1676638 A CN 1676638A CN A2005100107620 A CNA2005100107620 A CN A2005100107620A CN 200510010762 A CN200510010762 A CN 200510010762A CN 1676638 A CN1676638 A CN 1676638A
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Abstract
This invention discloses metal antimony purifying method and its mechanism. The method is to fill the industrial antimony in the chlorination tower; lead chlorine in the middle of the tower, heat at the 1/3 lower part of the tower to decompose antimony pentachloride; chloride and the superfluous mental blocks in the tower react to create antimony trichloride. The antimony trichloride in the storage tank automatically flows to re-boiling equipment and steam to go into rectification 1; through reflux control valve adjust flow amount of antimony trichloride and reflux amount, and the antimony trichloride goes into the re-boiler of rectification 2; the lower output mouth of the rectification tower arch is connected by the channel with the material interface of the storage tank that has two outputting mouths connected with the computation tank of reductive tank and re-boiler of sub-grade rectification system by the tube. The upper outputting mouth is connected with the residue tank by the pipeline; orderly connect the multi-grade rectification tower and continuously bring in the superfluous hydrogen and revert it and get 99.999%, 99.9999% and 99.99999% metal antimonies.
Description
Technical Field
The method relates to a hydrometallurgical method, in particular to a method for purifying metallic antimony and a device for realizing the method. The method and the device of the invention are particularly suitable for large-scale industrial production.
Background
In the purification process of metallic antimony, because the requirements on the material of production equipment are very strict and the process conditions are complex, any method for purifying metallic antimony by a wet method is intermittent production so far, and the industrial production difficulty is high. Therefore, the prior art is always produced in small batches through the processes of chlorination → dechlorination → rectification → reduction, and the like. Hydrochloric acid is added in the rectification process to remove low-boiling-point impurities, then the antimony trichloride is extracted by rectification, the high-boiling-point impurities are remained in a rectification kettle, and the antimony trichloride is purified once every one kettle of the rectification. The rectified antimony trichloride is sent into a reduction tank, and hydrogen is introduced to reduce into metallic antimony with the purity of 99.999% -99.9999%.
The prior art has the following defects that ① production cannot be continuous and can only be discontinuous, the recovery rate of a rectification product is low, the labor intensity is high, the purification time and the temperature for removing low-boiling-point impurities and antimony trichloride in ② are difficult to master, and standard industrial production cannot be formed, the production process is operated by experience, the human factors are multiple, the stability is poor, and the product index is difficult to control, in the ③ rectification process, the phenomenon of kettle jumping caused by metal impurity chlorides is often caused, so that the equipment is damaged, particularly, the production capacity is more obvious when being expanded, and therefore, the industrialized, large-scale and continuous production is difficult to realize.
Disclosure of Invention
The invention aims to overcome the defects and provide a method for purifying metallic antimony. The method can realize the continuity of the production process, overcome human factors, further control the whole production process by adopting a computer, has safe operation, stable product quality, effectively saves energy and reduces the consumption of raw materials.
The invention provides a method for purifying metallic antimony, which comprises the following steps in sequence:
(1) crushing industrial antimony into irregular blocks with the diameter of 20-30 phi, and filling a chlorination tower; chlorine is introduced into the middle part of the chlorination tower, and the control amount is based on the principle that no spark is generated locally; part of antimony pentachloride is generated in the chlorination process: (ii) a Heating the 1/3 part at the lower section of the chlorination tower to 100-150 ℃ to decompose antimony pentachloride: (ii) a The chlorine reacts with the excessive metal blocks in the tower to generate antimony trichloride: (ii) a The obtained antimony trichloride issent into a liquid storage tank.
(2) Antimony trichloride in a liquid storage tank automatically flows into a reboiler, and is evaporated at the temperature of 200-250 ℃ to enter rectification 1; the temperature of the rectifying column is controlled to be 180-230 ℃, and the temperature of the head of the rectifying column is controlled in two sections: the temperature of the lower section is 170-210 ℃ and the temperature of the upper section is 120-180 ℃.
(3) Adjusting the ratio of the outflow quantity to the reflux quantity of the antimony trichloride to be 2: 1-6: 1 through a reflux control valve, and feeding the obtained antimony trichloride into a reboiler of a rectification unit 2.
(4) The operation method and the control conditions of the rectification 2 are the same as those of the steps (2) and (3), so that the antimony trichloride with the grade of more than 99.999 percent is obtained, and the antimony trichloride is sent to the rectification 3 for continuous rectification.
(5) The operation method and the control conditions of the rectification 3 are the same as those of the steps (2) and (3), so that the antimony trichloride with the grade of more than 99.9999 percent is obtained, and the antimony trichloride is sent to the rectification 4 for continuous rectification.
(6) The operation method and the control conditions of the rectification 4 are the same as those of the steps (2) and (3), so that the antimony trichloride with the grade of more than 99.99999 percent is obtained and is sent to a liquid storage tank.
(7) And (3) continuously feeding the antimony trichloride obtained in the steps (3), (4), (5) and (6) into a reduction tank respectively, and continuously introducing excessive hydrogen under the conditions of controlling the temperature to be 550-900 ℃ and normal pressure to reduce the antimony trichloride so as to obtain the metallic antimony with the grades of 99.999%, 99.9999% and more than 99.99999%, namely the required metallic antimony product.
The process is characterized in that an ① rectifying column is separated from a rectifying still and is changed into a reboiler, ② discontinuous production is changed into continuous production, the quality of a product is improved by utilizing a regulating reflux valve, the whole process of ③ production is controlled by computer industry, the temperature of a tower head ④ is controlled in an upper section and a lower section, ⑤ continuously produces 99.999 percent to more than 99.99999 percent of metal antimony with different purities on the same production line according to market requirements.
The device for implementing the method of the invention comprises: one chlorination tower, one liquid storage bottle, five rectifying towers, one reduction tank, one residual liquid tank and one liquid storage tank. The chlorine pipeline is connected with the air inlet in the middle of the chlorination tower in the left and right directions; the chloride outflow port of the chlorination tower is connected with the feed inlet above the liquid storage bottle by a pipeline; a discharge hole at the bottom of the liquid storage bottle is connected with a feed hole at the top of a reboiler of the rectification 1 by a pipeline; the rectifying tower comprises a tower column and a tower head, wherein the tower head is connected with the tower column by a plane flange; a feed inlet of the stripping section of the rectifying column is connected with a chloride steam outlet at the top of the reboiler by a pipeline; the liquid outflow at the bottom of the rectifying column is connected with the other port at the top of the reboiler by a pipeline; the lower liquid outlet of the rectifying tower head is connected with the feed inlet of a liquid storage tank by a pipeline, the liquid storage tank is provided with 2 discharge ports and is respectively connected with a metering tank of a reduction tank and a reboiler of a next-stage rectifying system by pipelines; an upper liquid outlet of the tower head is connected with the residual liquid tank by a pipeline; as mentioned above, the rectification 1, the rectification 2, the rectification 3 and the rectification 4 are connected by pipelines in sequence, so as to achieve the purpose of continuous rectification.
The temperature of the chlorination tower is controlled to be arranged at 1/3 part of the lower section of the tower, chlorine enters the middle part of the tower through a pipeline, and an antimony trichloride outlet is arranged at 1/3 part of the lower section of the tower. The structure is characterized in that after the metal antimony reacts with excessive chlorine, a part of antimony pentachloride is generated. Flows into the lower section of the chlorination tower, and antimony pentachloride is easily decomposed into antimony trichloride and chlorine gas at the temperature of 100-150 ℃; at the moment, chlorine gas is easy to react with excessive antimony blocks at the lower section in the tower to generate antimony trichloride, so that the dechlorination process is saved, and the utilization of equipment is improved; the chlorination and dechlorination are completed in the same device, and additional dechlorination equipment is not needed.
Compared with the prior art, the invention has the following beneficial effects:
1. the process of chlorination → rectification → reduction is adopted to produce high-purity metal antimony, and chlorination and dechlorination are completed in a chlorination tower in the chlorination process, so that the generation of antimony pentachloride is completely controlled, the rectification effect is ensured, the operation process and equipment are saved, the use efficiency of theequipment is improved, and the labor intensity is reduced.
2.① tower head temperature is controlled for one section, it must remove low boiling point chloride, then put the needed antimony trichloride distillation into liquid storage tank, it is difficult to form industrial control. ② tower column adopts single packed tower or sieve plate tower, the purification effect of metal antimony is poor, generally the purified antimony trichloride is less than 99.9999%, ③ tower column and tower kettle are directly connected into one body, and the tower kettle is spherical, and it uses external heating method, this structure needs to stop producing cleaning and leaching tower kettle, the physical property of metal impurity chloride causes 'kettle jump' phenomenon in the rectification process, which results in equipment damage.
The invention is based on the conventional organic matter rectification method, and equipment improvement is carried out after tests to form the rectification device applied at present and the rectification device is applied to the purification process of high-purity metal antimony. According to the structural characteristics, the technical problem that industrialization and scale are influenced is solved, the industrialized continuous production is realized, and the production capacity of a single set of equipment is expanded. Improves the technical index of the product and eliminates the phenomenon of kettle jumping in the production process.
3. The continuous rectification is realized by adjusting the reflux ratio to control the rectification effect in the production, so that the computer-controlled production becomes possible, the traditional manual operation and discontinuous production mode are finished, the operation is safe and reliable, the process conditions are stable, and the method makes a great breakthrough on the prior art.
4.① solves the technical problem that the high-purity antimony production can not be continuous, improves the equipment utilization rate and recovery rate, improves the equipment perfectness rate from 30-40% of discontinuous production in a laboratory to 60-80%, ② improves the equipment perfectness rate, from one time of half-year maintenance to one time of annual maintenance, ③ production capacity is greatly improved, 40 tons of antimony with 99.999% of annual production capacity of a single set of equipment, 10 tons of antimony with 99.9999% of annual production capacity, 5 tons of antimony with 99.99999, which is 10-12 times of that of the single set of equipment for discontinuous production, in the industrial process of the high-purity antimony, the technical bottle diameter is a breakthrough, particularly, the product quality is stable, the purity is improved, and the purity of 14 elements of antimony detected by a glow discharge mass spectrometer reaches more than 99.99999%.
Drawings
FIG. 1 is a schematic view of a rectification column head structure of the present invention;
FIG. 2 is a view A-A of FIG. 1;
FIG. 3 is a schematic view of a column structure of a rectifying column of the present invention;
FIG. 4 is an enlarged view of the blister of FIG. 3;
FIG. 5 is a view B-B of FIG. 4;
FIG. 6 is an enlarged view of the tray of FIG. 3;
FIG. 7 is a schematic process flow diagram of the present invention;
in fig. 1 to 6: the device comprises a tower head connecting flange 1, a tower head lower liquid receiving disc 2, a control point thermometer sleeve 3, a tower head barrel 4, a tower head inner support 5, a tower head cooling water jacket 6, a tower head upper liquid receiving disc 7, a tower head flow plug 8, a tower head cooling water inlet pipe 9, a thermometer control point sleeve 10, a tower head cooling water outlet pipe 11, a tower head emptying pipe 12, a tower head upper liquid outlet pipe 13, a tower head lower liquid outlet pipe 14, a rectifying tower barrel 15, a rectifying tower overflow pipe 16, a rectifying tower plate 17, a rectifying tower bubble cap 18 and a rectifying tower connecting flange 19.
The equipment is structurally characterized in that ① rectifying column trays are combined by a sieve plate 17 and a bubble cap 18, ② rectifying column head temperature is controlled in two sections, namely lower section and upper section, ③ rectifying column head is provided with a lower liquid receiving disc 2 and an upper liquid receiving disc 7, ④ rectifying column head is provided with a flow plug 8 above the upper liquid receiving disc;
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited to the examples.
Example 1
Crushing industrial antimony ingot No. 1 into irregular blocks with the diameter of 20-30 phi, loading the irregular blocks into a chlorination tower of 200 kg, heating the lower section of the chlorination tower to 130 ℃, continuously introducing chlorine gas at the speed of 0.5 cubic meter per hour to enable the antimony blocks to gradually generate antimony trichloride, automatically flowing the antimony trichloride to a liquid storage tank from an outlet of the chlorination tower, putting the antimony trichloride into a reboiler of a rectification 1 from the liquid storage tank at the speed of 5 liters per hour, heating the reboiler to 230 ℃, controlling the temperature of the lower section of a tower head to 210 ℃, and controlling the temperature of the upper section of the tower head to 150 ℃. Under the condition of normal pressure, continuous rectification is carried out, a reflux valve is adjusted to ensure that the ratio of the outflow quantity to the reflux quantity of the antimony trichloride is 5.5: 1, and the rectified antimony trichloride enters a reboiler of a rectification 2 through a liquid storage tank at the flow rate of 4 liters per hour. Continuing rectification under the same temperature and pressure conditions as those of the rectification 1, and adjusting a reflux valve to ensure that the ratio of the antimony trichloride flow to the reflux is 5.0: 1. And (4) allowing the rectified antimony trichloride to pass through a liquid storage tank and enter a metering tank of a reduction system for later use.
And (3) purging air in the reduction tank by using argon, heating to 850 ℃, slowly introducing hydrogen, simultaneously putting the antimony trichloride in the metering tank into the reduction tank at the flow rate of 3 liters per hour, adjusting the hydrogen amount to 1.5 cubic meters per hour, and continuously introducing the hydrogen into the reduction tank to reduce the antimony trichloride into metallic antimony. The metallic antimony 19 is removed once every 4 hours, and the purity reaches more than 99.999 percent. The results of the analysis by glow discharge mass spectrometer are shown in Table 1.
TABLE 1 rectification 2 antimony trichloride reduction results
| Name of impurity | Ag | Au* | Cd | Cu | Fe | Mg | Ni | Pb | Zn | Mn | As | S | Si | Bi |
| The content is less than or equal to PPm | 0.03 | 0.05 | 0.5 | 0.005 | 0.08 | 0.04 | 0.10 | 0.07 | 0.3 | 0.05 | 1.3 | 0.2 | 0.8 | 0.09 |
Presence of interference
Example 2
The antimony trichloride in the rectification 2 in the embodiment1 is put into a reboiler of a rectification 3 from a liquid storage tank, the control conditions of temperature and pressure are the same as those of the rectification 1, the rectification is continued, a reflux valve is adjusted to ensure that the ratio of the outflow quantity to the reflux quantity of the antimony trichloride is 3.0: 1, and the rectified antimony trichloride passes through the liquid storage tank and is put into a metering tank in a reduction system for standby.
Purging air in a reduction tank with argon, heating to 850 ℃, slowly introducing hydrogen, continuously putting antimony trichloride in a metering tank into the reduction tank at a flow rate of 1 liter per hour, adjusting the hydrogen amount to 0.6 cubic meter per hour, continuously introducing the hydrogen into the reduction tank to reduce the antimony trichloride into metallic antimony, removing the metallic antimony once every 8 hours, namely the metallic antimony is 1.4, the purity is more than 99.9999 percent, and the analysis result of a glow discharge mass spectrometer is shown in Table 2
TABLE 2 results of rectifying 3 antimony trichloride to reduce antimony
| Name of impurity | Ag | Au* | Cd | Cu | Fe | Mg | Ni | Pb | Zn | Mn | As | S | Si | Bi |
| The content is less than or equal to PPm | 0.005 | 0.03 | 0.01 | 0.01 | 0.01 | 0.05 | 0.05 | 0.05 | 0.01 | 0.01 | 0.16 | 0.08 | 0.06 | 001 |
Presence of interference
Example 3
In the embodiment 2, the antimony trichloride in the rectification 3 is put into a reboiler of a rectification 4 from a liquid storage tank, the control conditions of temperature and pressure are the same as those of the rectification 1, the rectification is continued, a reflux valve is adjusted to ensure that the ratio of the outflow quantity to the reflux quantity of the antimony trichloride is 2.0: 1, and the rectified antimony trichloride passes through the liquid storage tank and is put into a metering tank in a reduction system for standby.
The air in the reduction tank is purged by argon, the temperature is raised to 850 ℃, hydrogen is slowly introduced, and meanwhile, antimony trichloride in the metering tank is continuously put into the reduction tank at the flow rate of 0.5 liter per hour. The hydrogen amount is adjusted to 0.4 cubic meter per hour, the antimony trichloride is reduced to metallic antimony by continuously introducing into a reduction tank, the material is removed once every 8 hours to obtain the metallic antimony with the purity of more than 99.99999 percent, and the analysis result of a glow discharge mass spectrometer is shown in Table 3.
TABLE 3 results of rectifying 4 antimony trichloride to reduce antimony
| Name of impurity Balance | Ag | Au | Cd | Cu | Fe | Mg | Ni | Pb | Zn | Mn | As | S | Si | Bi |
| The content is less than or equal to PPm | 0.001 | 0.002 | 0.005 | 0.002 | 0.001 | 0.001 | 0.005 | 0.005 | 0.005 | 0.001 | 0.05 | 0.005 | 0.005 | 0.005 |
Claims (3)
1. A method for purifying metallic antimony, which comprises the following steps in sequence:
(1) crushing industrial antimony into irregular blocks with the diameter of 20-30 phi, and filling a chlorination tower; chlorine is introduced into the middle part of the chlorination tower, and part of antimony pentachloride is generated in the chlorination process; heating the 1/3 part at the lower section of the chlorination tower to 100-150 ℃ to decompose antimony pentachloride; reacting chlorine with excessive metal blocks in the tower to generate antimony trichloride; feeding the obtained antimony trichloride into a liquid storage tank;
(2) antimony trichloride in a liquid storage tank automatically flows into a reboiler, and is evaporated at the temperature of 200-250 ℃ to enter rectification 1; the temperature of the rectifying column is controlled to be 180-230 ℃, and the temperature of the head of the rectifying column is controlled in two sections: the lower section is at 170-210 ℃ and the upper section is at 120-180 ℃;
(3) adjusting the ratio of the outflow quantity to the reflux quantity of the antimony trichloride to be 2: 1-6: 1 through a reflux control valve, and feeding the obtained antimony trichloride into a reboiler of a rectification unit 2;
(4) the operation method and the control conditions of the rectification 2 are the same as those of the steps (2) and (3), so that the antimony trichloride with the grade of more than 99.999 percent is obtained, and the antimony trichloride is sent to the rectification 3 for continuous rectification;
(5) the operation method and the control conditions of the rectification 3 are the same as those of the steps (2) and (3), so that the antimony trichloride with the grade of more than 99.9999 percent is obtained, and the antimony trichloride is sent to the rectification 4 for continuous rectification;
(6) the operation method and the control conditions of the rectification 4 are the same as those of the steps (2) and (3), so that the antimony trichloride with the grade of more than 99.99999 percent is obtained and is sent into a liquid storage tank;
(7) and (3) continuously feeding the antimony trichloride obtained in the steps (3), (4), (5) and (6) into a reduction tank respectively, and continuously introducing excessive hydrogen under the conditions of controlling the temperature to be 550-900 ℃ and normal pressure to reduce the antimony trichloride so as to obtain the metallic antimony with the grades of 99.999%, 99.9999% and more than 99.99999%, namely the required metallic antimony product.
2. An apparatus for purifying metallic antimony, the apparatus comprising: a chlorination tower, a liquid storage bottle, a plurality of rectifying towers, a reduction tank, a residual liquid tank and a liquid storage tank; the chlorine pipeline is connected with the air inlet in the middle of the chlorination tower in the left and right directions; the chloride outflow port of the chlorination tower is connected with the feed inlet above the liquid storage bottle by a pipeline; a discharge hole at the bottom of the liquid storage bottle is connected with a feed hole at the top of a reboiler of the rectification 1 by a pipeline; the rectifying tower comprises a tower column and a tower head, wherein the tower head is connected with the tower column by a plane flange; a feed inlet of the stripping section of the rectifying column is connected with a chloride steam outlet at the top of the reboiler by a pipeline; the liquid outflow at the bottom of the rectifying column is connected with the other port at the top of the reboiler by a pipeline; the lower liquid outlet of the rectifying tower head is connected with the feed inlet of a liquid storage tank by a pipeline, the liquid storage tank is provided with 2 discharge ports and is respectively connected with a metering tank of a reduction tank and a reboiler of a next-stage rectifying system by pipelines; an upper liquid outlet of the tower head is connected with the residual liquid tank by a pipeline; as described above, the multistage distillation pipes are connected in sequence to realize continuous distillation.
3. The apparatus of claim 2, wherein the chlorination column is controlled in temperature at 1/3 parts of the lower section of the column, chlorine gas is introduced at the middle part of the column through a pipeline, and the outlet of antimony trichloride is provided at 1/3 parts of the lower section of the column.
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| CNB2005100107620A CN1325674C (en) | 2005-04-22 | 2005-04-22 | Metal antimony purifying method and apparatus |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101144125B (en) * | 2006-09-11 | 2010-05-12 | 昆明鸿世达高技术材料有限责任公司 | Industrialized producing method for high-purity arsenic |
| CN104962759A (en) * | 2015-08-04 | 2015-10-07 | 广东先导稀材股份有限公司 | Preparation method of antimony |
| CN107502758A (en) * | 2017-09-06 | 2017-12-22 | 长沙科力威蒸馏技术有限公司 | A kind of method for producing high-purity calcium |
| CN108300866A (en) * | 2018-04-09 | 2018-07-20 | 昆山佳鹿石英有限公司 | Arsenic purifies rectifier unit and the method using device purification arsenic |
| CN108517417A (en) * | 2018-04-09 | 2018-09-11 | 昆山佳鹿石英有限公司 | Mercury purifies rectifier unit and the method using device purification mercury |
| CN108546830A (en) * | 2018-04-13 | 2018-09-18 | 上海泰坦科技股份有限公司 | A kind of preparation method and application of antimony |
| CN117248114A (en) * | 2023-11-14 | 2023-12-19 | 昆明冶金研究院有限公司 | Short-flow system for preparing metallic antimony and method for preparing metallic antimony |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61106417A (en) * | 1984-10-31 | 1986-05-24 | Sumitomo Metal Mining Co Ltd | Distilling method of aqueous antimony chloride solution |
| JPS61106733A (en) * | 1984-10-31 | 1986-05-24 | Sumitomo Metal Mining Co Ltd | Production of high-purity antimony |
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2005
- 2005-04-22 CN CNB2005100107620A patent/CN1325674C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101144125B (en) * | 2006-09-11 | 2010-05-12 | 昆明鸿世达高技术材料有限责任公司 | Industrialized producing method for high-purity arsenic |
| CN104962759A (en) * | 2015-08-04 | 2015-10-07 | 广东先导稀材股份有限公司 | Preparation method of antimony |
| CN104962759B (en) * | 2015-08-04 | 2017-05-31 | 广东先导稀材股份有限公司 | A kind of preparation method of antimony |
| CN107502758A (en) * | 2017-09-06 | 2017-12-22 | 长沙科力威蒸馏技术有限公司 | A kind of method for producing high-purity calcium |
| CN108300866A (en) * | 2018-04-09 | 2018-07-20 | 昆山佳鹿石英有限公司 | Arsenic purifies rectifier unit and the method using device purification arsenic |
| CN108517417A (en) * | 2018-04-09 | 2018-09-11 | 昆山佳鹿石英有限公司 | Mercury purifies rectifier unit and the method using device purification mercury |
| CN108546830A (en) * | 2018-04-13 | 2018-09-18 | 上海泰坦科技股份有限公司 | A kind of preparation method and application of antimony |
| CN117248114A (en) * | 2023-11-14 | 2023-12-19 | 昆明冶金研究院有限公司 | Short-flow system for preparing metallic antimony and method for preparing metallic antimony |
| CN117248114B (en) * | 2023-11-14 | 2024-02-02 | 昆明冶金研究院有限公司 | Short-flow system for preparing metallic antimony and method for preparing metallic antimony |
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| CN1325674C (en) | 2007-07-11 |
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