CN102560150B - Efficient lead removing agent for fire refining antimony and preparation method and application of efficient lead removing agent - Google Patents
Efficient lead removing agent for fire refining antimony and preparation method and application of efficient lead removing agent Download PDFInfo
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- CN102560150B CN102560150B CN2012100313098A CN201210031309A CN102560150B CN 102560150 B CN102560150 B CN 102560150B CN 2012100313098 A CN2012100313098 A CN 2012100313098A CN 201210031309 A CN201210031309 A CN 201210031309A CN 102560150 B CN102560150 B CN 102560150B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to an efficient lead removing agent for fire refining antimony and a preparation method and application of the efficient lead removing agent. The efficient lead removing agent for fire refining antimony is condensed phosphoric acid; the condensed phosphoric acid is prepared by the following steps: adding 85% industrial phosphoric acid to an autoclave; then adding phosphorus pentaoxide with the weight of 25-50% of the weight of the industrial phosphoric acid; reacting for 2-4h under the conditions of 100-120 DEG C and 0.1-0.3MPa, wherein the weight of the active ingredient phosphorus pentaoxide is 69-85%. In the application, the weight ratio of the efficient lead removing agent to the lead in antimony liquid is (4-1.8):1. The efficient lead removing agent is applied by the steps of adding the efficient lead removing agent to the surface of molten metal of an antimony-refining reverbaratory furnace of a temperature of 700-1,000 DEG C, blowing gas for agitation, reacting for 60-80min, and fishing out the floating slag. The preparation method provided by the invention is simple in process, short in flow and easy to operate and does not generate the three wastes or pollution; compared with the traditional lead removing agent, the dosage is reduced by more than 30%, the slag rate is decreased, the metal recycling rate is improved, and the efficiency and environmental friendliness are realized.
Description
Technical field
The present invention relates to efficient deleading agent of the pyrorefining of antimony in the non-ferrous metal metallurgy and its preparation method and application.
Background technology
Have and be attended by plumbous impurity element in the coloured gold raw materials for metallurgy usually, in smelting the course of processing, in order to reach the quality products specification of quality, must carry out deleading handles, original deleading agent is solid powdery, its main component is primary ammonium phosphate, when refining lead-removing, deleading agent is joined fusion antimony liquid surface in the metallurgical furnace, blast gas stirring, but this pressed powder deleading agent contains ammonia and moisture, when deleading agent fusing reaction, a large amount of toxic and harmfuls be can produce, and sb oxide flue dust, severe operational environment carried, and surrounding enviroment are polluted, also caused the loss of metal simultaneously.And the deleading quantity of slag is big, and lead-in-dreg is low, and the deleading agent consumption is big, and the metal direct yield is low, deficiency in economic performance.A kind of liquid deleading agent of use is also arranged, but moisture content wherein is too high, generally reach about 15%, in use one is to exist certain danger, when adding deleading agent in the high temperature antimony liquid in fusion, cause that easily antimony liquid splashes, add excessive velocities and can cause the blast of high temperature stove that operator in serious harm; The 2nd, a large amount of moisture evaporations reduces furnace temperature, needs the additional heat consumes energy, and Hui Fa moisture carries away sb oxide simultaneously, has caused the loss of metal; The 3rd, deleading efficient is lower, and the metal direct yield is low, same deficiency in economic performance.
Summary of the invention
The object of the present invention is to provide a kind of raw material sources convenient, production cost is lower, less investment, and production capacity is big, environment-friendly high-efficiency, efficient deleading agent of the antimony regulus that is used for non-ferrous metal metallurgy that the Metal smelting rate of recovery is high, refining bismuth, copper metallurgy pyrorefining and its preparation method and application.
Efficient deleading agent of the present invention is polycondensation phosphoric acid; Its effective constituent phosphorus pentoxide content is 69%～85%.
Described polycondensation phosphoric acid is tripolyphosphate, four polyphosphoric acids or polyphosphoric acid.
Its preparation method may further comprise the steps:
PHOSPHORIC ACID TECH.GRADE with 85% adds in the autoclave, add industrial phosphoric acid weight 25%～50% Vanadium Pentoxide in FLAKES again, at 100～120 ℃, react 2～4h under 0.1～0.3MPa condition, the polycondensation phosphoric acid that generates, its effective constituent phosphorus pentoxide content is 69%～85%.
The effective constituent of described polycondensation phosphoric acid is looked the difference in phosphorus pentoxide content, polymerization temperature, pressure, reaction times, is respectively tripolyphosphate, four polyphosphoric acids or polyphosphoric acid.
Its chemical equation is:
P
2O
5＋H
2O＝2HPO
3
HPO
3＋H
2O＝H
3PO
4
P
2O
5＋3H
2O＝2H
3PO
4
P
2O
5＋2H
2O＝H
4P
2O
7
The application of efficient deleading agent: the amount ratio according to lead content in efficient deleading agent and the antimony liquid is: 4～1.8:1.Efficient deleading agent product is joined the surface of metal melting liquid of the antimony regulus reverberatory furnace of 700 ℃～1000 ℃ of temperature, blast gas stirring again, react and pull scum silica frost out after 60～80 minutes and get final product.
Advantage of the present invention: production technique of the present invention is simple, and flow process is short, and processing ease is grasped, and does not have " three wastes " output and pollution, with traditional deleading agent relatively, consumption reduces more than 30%, the slag rate reduces, metal recovery rate improves, and has realized efficiently, environmental protection.
Embodiment
Be described in further detail below in conjunction with the present invention of embodiment:
Embodiment 1: condensation method is produced efficient deleading agent:
Industrial phosphoric acid 3000Kg with 85% and Vanadium Pentoxide in FLAKES 800Kg put into 5000 liters of autoclaves and heat up, at 100～120 ℃, react 2.5h under 0.1～0.3MPa condition, after the fast cooling step-down, namely obtain efficient deleading agent product 3758Kg, effective constituent phosphorus pentoxide content 70.43%.
Embodiment 2:
Industrial phosphoric acid 2500Kg with 85% and Vanadium Pentoxide in FLAKES 996Kg put into 5000 liters of autoclaves and heat up, at 100～120 ℃, react 3h under 0.1～0.3MPa condition, after the fast cooling step-down, namely obtain efficient deleading agent product 3465Kg, effective constituent phosphorus pentoxide content 73.16%.
Embodiment 3:
Industrial phosphoric acid 2000Kg with 85% and Vanadium Pentoxide in FLAKES 2000Kg put into 5000 liters of autoclaves and heat up, at 100～120 ℃, react 3.5h under 0.1～0.3MPa condition, after the fast cooling step-down, namely obtain efficient deleading agent product 3880Kg, effective constituent phosphorus pentoxide content 83.28%.
Embodiment 4: the application of efficient deleading agent
Get the efficient deleading agent product 590Kg that embodiment 1 obtains, join in the antimony regulus reverberatory furnace, needle antimony is leaded 0.55% before the refining, and 50 tons of antimony liquid gross weights are stirred reaction in air blast under 750 ℃ of temperature and pulled scum silica frost out after 60 minutes, star metal liquid leaded 0.14%, the cooling ingot casting gets 48.50 tons of star metals, and the heavy 750Kg of scum silica frost contains antimony 19.95%, leaded 25.49%, the antimony metal rate of recovery 97.0%.
Embodiment 5: the application of efficient deleading agent
Get the efficient deleading agent product 410Kg that embodiment 1 obtains, join in the antimony regulus reverberatory furnace, needle antimony is leaded 0.16% before the refining, and 53 tons of antimony liquid gross weights are stirred reaction in air blast under 850 ℃ of temperature and pulled scum silica frost out after 70 minutes, star metal liquid leaded 0.005%, the cooling ingot casting gets 51.15 tons of star metals, and the heavy 545Kg of scum silica frost contains antimony 33.93%, leaded 15.01%, the antimony metal rate of recovery 96.50%.
Embodiment 6:
Get the efficient deleading agent product 1200Kg that embodiment 1 obtains, join in the antimony regulus reverberatory furnace, needle antimony is leaded 0.85% before the refining, and 52 tons of antimony liquid gross weights are stirred reaction in air blast under 800 ℃ of temperature and pulled scum silica frost out after 65 minutes, star metal liquid leaded 0.05%, the cooling ingot casting gets 50.00 tons of star metals, and the heavy 1505Kg of scum silica frost contains antimony 13.29%, leaded 26.75%, the antimony metal rate of recovery 96.15%.
Embodiment 7:
Get the efficient deleading agent product 520Kg that embodiment 2 obtains, join in the antimony regulus reverberatory furnace, needle antimony is leaded 0.56% before the refining, and 50 tons of antimony liquid gross weights are stirred reaction in air blast under 750 ℃ of temperature and pulled scum silica frost out after 60 minutes, star metal liquid leaded 0.13%, the cooling ingot casting gets 48.45 tons of star metals, and the heavy 650Kg of scum silica frost contains antimony 23.85%, leaded 32.05%, the antimony metal rate of recovery 96.90%.
Embodiment 8: get the efficient deleading agent product 430Kg that embodiment 2 obtains, join in the antimony regulus reverberatory furnace, needle antimony is leaded 0.19% before the refining, and 52 tons of antimony liquid gross weights are stirred reaction in air blast under 800 ℃ of temperature and pulled scum silica frost out after 70 minutes, star metal liquid leaded 0.003%, the cooling ingot casting gets 50.07 tons of star metals, and the heavy 560Kg of scum silica frost contains antimony 34.46%, leaded 16.99%, the antimony metal rate of recovery 96.28%.
Embodiment 9:
Get the efficient deleading agent product 1100Kg that embodiment 2 obtains, join in the antimony regulus reverberatory furnace, needle antimony is leaded 0.75% before the refining, and 53 tons of antimony liquid gross weights are stirred reaction in air blast under 750 ℃ of temperature and pulled scum silica frost out after 60 minutes, star metal liquid leaded 0.03%, the cooling ingot casting gets 51.06 tons of star metals, and the heavy 1375Kg of scum silica frost contains antimony 17.45%, leaded 26.83%, the antimony metal rate of recovery 96.35%.
Embodiment 10:
Get the efficient deleading agent product 390Kg that embodiment 3 obtains, join in the antimony regulus reverberatory furnace, needle antimony is leaded 0.55% before the refining, and 50 tons of antimony liquid gross weights are stirred reaction in air blast under 750 ℃ of temperature and pulled scum silica frost out after 60 minutes, star metal liquid leaded 0.14%, the cooling ingot casting gets 48.50 tons of star metals, and the heavy 480Kg of scum silica frost contains antimony 31.25%, leaded 41.42%, the antimony metal rate of recovery 97.0%.
Embodiment 11:
Get the efficient deleading agent product 280Kg that embodiment 3 obtains, join in the antimony regulus reverberatory furnace, needle antimony is leaded 0.18% before the refining, and 53 tons of antimony liquid gross weights are stirred reaction in air blast under 850 ℃ of temperature and pulled scum silica frost out after 70 minutes, star metal liquid leaded 0.005%, the cooling ingot casting gets 51.30 tons of star metals, and the heavy 420Kg of scum silica frost contains antimony 40.47%, leaded 21.98%, the antimony metal rate of recovery 96.8%.
Embodiment 12:
Get the efficient deleading agent product 1000Kg that embodiment 3 obtains, join in the antimony regulus reverberatory furnace, needle antimony is leaded 0.85% before the refining, and 52 tons of antimony liquid gross weights are stirred reaction in air blast under 800 ℃ of temperature and pulled scum silica frost out after 65 minutes, star metal liquid leaded 0.05%, the cooling ingot casting gets 50.18 tons of star metals, and the heavy 1258Kg of scum silica frost contains antimony 14.46%, leaded 31.91%, the antimony metal rate of recovery 96.50%.
Claims (4)
1. the efficient deleading agent of a pyrorefining antimony is characterized in that, is polycondensation phosphoric acid; Its effective constituent phosphorus pentoxide content is 69%～85%.
2. the efficient deleading agent of pyrorefining antimony according to claim 1 is characterized in that, described polycondensation phosphoric acid is tripolyphosphate, four polyphosphoric acids or polyphosphoric acid.
3. the preparation method of the efficient deleading agent of a pyrorefining antimony, it is characterized in that, the phosphoric acid of technical grade 85% is added in the autoclave, the Vanadium Pentoxide in FLAKES that adds PHOSPHORIC ACID TECH.GRADE weight 25%～50% again, at 100～120 ℃, 0.1 react 2～4h under the～0.3MPa condition, generate polycondensation phosphoric acid, its effective constituent phosphorus pentoxide content is 69%～85%.
4. the preparation method of the efficient deleading agent of pyrorefining antimony according to claim 3, it is characterized in that, described polycondensation phosphoric acid is looked the difference in phosphorus pentoxide content, polymerization temperature, pressure, reaction times, is respectively tripolyphosphate, four polyphosphoric acids or polyphosphoric acid.
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| CN110791666A (en) * | 2019-12-18 | 2020-02-14 | 益阳生力材料科技股份有限公司 | Bismuth removing agent for antimony smelting and refining |
| CN113737020B (en) * | 2021-09-10 | 2022-09-13 | 广西万仕智稀贵金属科技有限公司 | Method for deeply removing cadmium in crude antimony refining process |
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2012
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| CN1123335A (en) * | 1994-11-25 | 1996-05-29 | 刘伯龙 | Lead-removing method for ammonium salt refined by antimony affination process |
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