CN110042258A - Stibium fire smelting reverberatory furnace refines deferrization process - Google Patents

Stibium fire smelting reverberatory furnace refines deferrization process Download PDF

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Publication number
CN110042258A
CN110042258A CN201910491731.3A CN201910491731A CN110042258A CN 110042258 A CN110042258 A CN 110042258A CN 201910491731 A CN201910491731 A CN 201910491731A CN 110042258 A CN110042258 A CN 110042258A
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iron
reverberatory furnace
antimony
furnace
phosphate
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游先银
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DONGGANG ANTIMONY PRODUCT Co Ltd HUNAN PROV
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DONGGANG ANTIMONY PRODUCT Co Ltd HUNAN PROV
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Priority to CN201910491731.3A priority Critical patent/CN110042258A/en
Publication of CN110042258A publication Critical patent/CN110042258A/en
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B30/00—Obtaining antimony, arsenic or bismuth
    • C22B30/02—Obtaining antimony
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/10—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses stibium fire smelting reverberatory furnaces to refine deferrization process, which includes the following steps: step 1: iron content antimony raw material being added in reverberatory furnace carry out arsenic removal, except lead is handled first；Step 2: arsenic removal, except after lead processing operation, substance inside reverberatory furnace is in the iron antimony fusant of molten state, then tapping total amount is calculated according to iron content in reverberatory furnace inner molten antimony iron liquid, except the dosage of the ammonium dihydrogen phosphate of iron needed for calculating according to the total amount of iron.The iron in antimony liquid can be controlled to 50ppm by this method hereinafter, this method is used as iron removing reagent using ammonium di-hydrogen phosphate, it will not be to bring new impurity into antimony liquid, method is easy to operate, and the scum of generation is not belonging to solid waste, is easy to sell or processing.It is operated by practice, ammonium di-hydrogen phosphate de-ferrous effect is good, and production antimony slab can achieve No. zero antimony slab standard, has satisfactorily resolved influence of the iron tramp element to star metal product quality in antimony smelting.

Description

Stibium fire smelting reverberatory furnace refines deferrization process
Technical field
The present invention relates to metal refining techniques field, specially stibium fire smelting reverberatory furnace refines deferrization process.
Background technique
Always contain some other metal impurities from the crude metal that ore or concentrate melting obtain, in most cases, this A little impurity have bad influence to metal.Therefore, to obtain purer metal must remove as much as possible these impurity.In addition, Some noble metals (such as gold, silver) are also present in lead bullion crude metal frequently as impurity, by your gold extracted in these crude metal Category is also a task of Nonferrous Metallurgical Process.Since liquation refining method and device therefor are simple, and refining efficiency is also suitable Height, therefore be widely used in the production practices of nonferrous metallurgy, so-called liquate refer to melt in molten condition or slowly cold But during, separate liquid phase or solid phase.In cooling metal alloy, other than eutectic composition, liquate phenomenon can be all generated. This phenomenon is very harmful for foundry industry, because liquate phenomenon destroys the uniformity of alloy-steel casting each section composition, Cause the inconsistent of casting each section property.
But liquate phenomenon is but widely used in coloured crude metal refining, as the desilver of lead bullion liquate, crude zinc liquate remove iron Except lead, thick tin liquate are except iron etc., due to stibium by wet method smelting process, part iron in ore and yin, yang pole plate is made to be dissolved in electrolysis In liquid, therefore a large amount of ferrous ion and iron ion (Fe3+) being generated in the electrolytic solution, being reacted by electrodeposition, iron ion enters In cathode antimony, cause ferro element in cathode antimony exceeded, by assay, cathode antimony iron content is up to 7000ppm, even more Height, and national standard No.1 antimony slab requires iron to be no more than 100ppm.Therefore, in order to ensure the quality of antimony slab and antimony product, cathode is used When the iron content antimony material production antimony slab such as antimony, it must carry out handling except iron during reverberatory furnace molten refined, by impurity in antimony slab The content of iron is reduced within national standard allowed band, and traditional reverberatory refining arsenic removal, lead can not remove the iron in antimony liquid, iron Presence seriously affect the quality of antimony slab, will also hinder wet method electrolysis industrial expansion.
Summary of the invention
The purpose of the present invention is to provide stibium fire smelting reverberatory furnaces to refine deferrization process, has the excellent of good iron removal effect Point solves the problems, such as that above-mentioned background technique is previously mentioned.
It to achieve the above object, should the invention provides the following technical scheme: stibium fire smelting reverberatory furnace refines deferrization process Technique includes the following steps:
Step 1: iron content antimony raw material is added in reverberatory furnace carries out arsenic removal, except lead is handled first；
Step 2: arsenic removal, except after lead processing operation, the substance inside reverberatory furnace is in the iron antimony fusant of molten state, then root Tapping total amount is calculated according to iron content in reverberatory furnace inner molten antimony iron liquid, the di(2-ethylhexyl)phosphate of iron is removed needed for calculating according to the total amount of iron The dosage of hydrogen ammonium；
Step 3: the ventilation equipment of reverberatory furnace are closed, and in order to reduce the oxidation of antimony, reduce oxygen content, then will be in reverberatory furnace The temperature in portion is heated between 850-950 degrees Celsius, and ammonium dihydrogen phosphate is then added into reverberatory furnace by the furnace roof of reverberatory furnace；
Step 4: using cast iron connecting pipe to high pressure draught is passed through by air blower inside reverberatory furnace, wind pressure is in 6 kilograms of pressure More than, four Furnace doors of reverberatory furnace are then opened respectively, are passed through Furnace door using long trivet and are protruded into reverberatory furnace Portion is stirred the antimony liquid of molten state, so that iron ion is sufficiently reacted with phosphate, the operating temperature setting of reverberatory furnace at this time Between 900-950 degrees Celsius, blasting time was set as between 40-50 minutes；
Step 5: closing air blower, cast iron connecting pipe removed, and floats at this point, can be precipitated one layer on the surface of antimony iron fusant Then dross is slowly moved to the slag notch of reverberatory furnace by slag using long trivet, then by manually being clawed；
Step 6: taking out part antimony liquid in reverberatory furnace, the iron-content in assay antimony liquid, if iron-content is excessively high, three times Continue to detect iron content in antimony liquid after repeating the above steps, until iron content reaches standard, stop to reflection stove heating, It is 30-50 minutes cooling to material under the blowing effect of air blower, material can be taken out and carry out subsequent process operation.
Preferably, the furnace roof connection setting charging hopper of the reverberatory furnace.
Preferably, it is Fe that the dosage of the ammonium dihydrogen phosphate, which calculates the chemical equation of basis,3++PO3-=FePO4、Fe2++ PO3-=Fe3(PO4)2、Fe3++HPO2-=Fe2(HPO4)3、Fe3++H2PO-=Fe(H2PO4)3One or more of combination.
Preferably, single packet quality of the ammonium dihydrogen phosphate is 25kg/ packet, and the amount being added every time is no more than 1.5 tons, list The amount of secondary addition is no more than 60 packets, and in the case where the content of iron is high, ammonium dihydrogen phosphate is refined using multiple batches of.
Preferably, the dross is phosphatic one or more kinds of mixing such as ferric phosphate, ferrous phosphate, primary iron phosphate Object has part for the simple substance antimony of precipitation.
Preferably, the boiling point of ferric phosphate is generated in the technique in 158 degrees centigrades, readily volatilized, operator exists Special mask is worn during work.
Preferably, the temperature for repeating reaction in the step 6 three times is respectively 850-1000 degrees Celsius, 800-950 is Celsius It spends and 800-900 degrees Celsius.
Compared with prior art, beneficial effects of the present invention are as follows:
1, the present invention reacts production ferric phosphate, ferrous phosphate, biphosphate with phosphate anion using iron ion under molten condition The phosphate such as iron, ferric phosphate are white or greyish white powder crystal, and relative density is in 1.13-1.59g/cm3Between, the boiling point of ferric phosphate It is volatile at 158 DEG C or so, to achieve the purpose that antimony iron separates, the iron in antimony liquid is controlled to 50ppm or less and (is much higher than National standard No.1 antimony slab, 100ppm standard).This method uses ammonium di-hydrogen phosphate as iron removing reagent, will not be new to bring into antimony liquid Impurity, method is easy to operate, and the scum of generation is not belonging to solid waste, is easy to sell or handle.It is operated by practice, ammonium di-hydrogen phosphate De-ferrous effect is good, production antimony slab can achieve No. zero antimony slab standard, satisfactorily resolved antimony smelt in iron tramp element to star metal The influence of product quality.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described, Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all Belong to the scope of protection of the invention.
Embodiment one:
The present invention provides a kind of technical solution: stibium fire smelting reverberatory furnace refines deferrization process, has the advantages of good iron removal effect, Solve the problems, such as that above-mentioned background technique is previously mentioned.
It to achieve the above object, should the invention provides the following technical scheme: stibium fire smelting reverberatory furnace refines deferrization process Technique includes the following steps:
Step 1: iron content antimony raw material is added in reverberatory furnace carries out arsenic removal, except lead is handled first；
Step 2: arsenic removal, except after lead processing operation, the substance inside reverberatory furnace is in the iron antimony fusant of molten state, then root According in reverberatory furnace inner molten antimony iron liquid iron content calculate tapping total amount, according to chemical equation be Fe3++PO3-=FePO4、 Fe2++PO3-=Fe3(PO4)2、Fe3++HPO2-=Fe2(HPO4)3And Fe3++H2PO-=Fe(H2PO4)3, calculated according to the total amount of iron The dosage of the required ammonium dihydrogen phosphate except iron；
Step 3: the ventilation equipment of reverberatory furnace are closed, and in order to reduce the oxidation of antimony, reduce oxygen content, then will be in reverberatory furnace The temperature in portion is heated to 850 degrees Celsius, and ammonium dihydrogen phosphate, the phosphoric acid are then added into reverberatory furnace by the furnace roof of reverberatory furnace Single packet quality of ammonium dihydrogen is 25kg/ packet, and the amount being added every time is no more than 1.5 tons, and the amount that single is added is no more than 60 packets, In the case that the content of iron is high, ammonium dihydrogen phosphate is refined using multiple batches of；
Step 4: using cast iron connecting pipe to high pressure draught is passed through by air blower inside reverberatory furnace, wind pressure is in 6 kilograms of pressure More than, four Furnace doors of reverberatory furnace are then opened respectively, are passed through Furnace door using long trivet and are protruded into reverberatory furnace Portion is stirred the antimony liquid of molten state, so that iron ion is sufficiently reacted with phosphate, the operating temperature setting of reverberatory furnace at this time It is 900 degrees Celsius, blasting time is set as 40 minutes；
Step 5: closing air blower, cast iron connecting pipe removed, and floats at this point, can be precipitated one layer on the surface of antimony iron fusant Slag, the dross are phosphatic one or more kinds of mixtures such as ferric phosphate, ferrous phosphate, primary iron phosphate, have the part to be Then dross is slowly moved to the slag notch of reverberatory furnace by the simple substance antimony of precipitation using long trivet, then by manually being taken off Out；
Step 6: taking out part antimony liquid in reverberatory furnace, the iron-content in assay antimony liquid, stops to reflection stove heating, It is 30 minutes cooling to material under the blowing effect of air blower, material can be taken out and carry out subsequent process operation.
It is 45ppm according to iron content in the obtained antimony slab of the present embodiment.
Embodiment two: the present embodiment and the distinguishing characteristics of embodiment one are:
Stibium fire smelting reverberatory furnace refines deferrization process, which includes the following steps:
Step 1: iron content antimony raw material is added in reverberatory furnace carries out arsenic removal, except lead is handled first；
Step 2: arsenic removal, except after lead processing operation, the substance inside reverberatory furnace is in the iron antimony fusant of molten state, then root According in reverberatory furnace inner molten antimony iron liquid iron content calculate tapping total amount, according to chemical equation be Fe3++PO3-=FePO4、 Fe2++PO3-=Fe3(PO4)2、Fe3++HPO2-=Fe2(HPO4)3And Fe3++H2PO-=Fe(H2PO4)3, calculated according to the total amount of iron The dosage of the required ammonium dihydrogen phosphate except iron；
Step 3: the ventilation equipment of reverberatory furnace are closed, and in order to reduce the oxidation of antimony, reduce oxygen content, then will be in reverberatory furnace The temperature in portion is heated to 950 degrees Celsius, and ammonium dihydrogen phosphate, the phosphoric acid are then added into reverberatory furnace by the furnace roof of reverberatory furnace Single packet quality of ammonium dihydrogen is 25kg/ packet, and the amount being added every time is no more than 1.5 tons, and the amount that single is added is no more than 60 packets, In the case that the content of iron is high, ammonium dihydrogen phosphate is refined using multiple batches of；
Step 4: high pressure draught is passed through by air blower to inside reverberatory furnace using cast iron connecting pipe, wind pressure is pressed at 6 kilograms Then power opens four Furnace doors of reverberatory furnace respectively, pass through Furnace door using long trivet and protrude into the inside of reverberatory furnace The antimony liquid of molten state is stirred, so that iron ion is sufficiently reacted with phosphate, the operating temperature of reverberatory furnace at this time is set as 950 degrees Celsius, blasting time is set as 50 minutes；
Step 5: closing air blower, cast iron connecting pipe removed, and floats at this point, can be precipitated one layer on the surface of antimony iron fusant Slag, the dross are phosphatic one or more kinds of mixtures such as ferric phosphate, ferrous phosphate, primary iron phosphate, have the part to be Then dross is slowly moved to the slag notch of reverberatory furnace by the simple substance antimony of precipitation using long trivet, then by manually being taken off Out；
Step 6: taking out part antimony liquid in reverberatory furnace, the iron-content in assay antimony liquid, stops to reflection stove heating, It is 50 minutes cooling to material under the blowing effect of air blower, material can be taken out and carry out subsequent process operation.
It is 40ppm according to iron content in the obtained antimony slab of the present embodiment.
Embodiment three: the present embodiment and the distinguishing characteristics of embodiment one and embodiment two are:
Stibium fire smelting reverberatory furnace refines deferrization process, which includes the following steps:
Step 1: iron content antimony raw material is added in reverberatory furnace carries out arsenic removal, except lead is handled first；
Step 2: arsenic removal, except after lead processing operation, the substance inside reverberatory furnace is in the iron antimony fusant of molten state, then root According in reverberatory furnace inner molten antimony iron liquid iron content calculate tapping total amount, according to chemical equation be Fe3++PO3-=FePO4、 Fe2++PO3-=Fe3(PO4)2、Fe3++HPO2-=Fe2(HPO4)3And Fe3++H2PO-=Fe(H2PO4)3, calculated according to the total amount of iron The dosage of the required ammonium dihydrogen phosphate except iron；
Step 3: the ventilation equipment of reverberatory furnace are closed, and in order to reduce the oxidation of antimony, reduce oxygen content, then will be in reverberatory furnace The temperature in portion is heated to 900 degrees Celsius, and ammonium dihydrogen phosphate, the phosphoric acid are then added into reverberatory furnace by the furnace roof of reverberatory furnace Single packet quality of ammonium dihydrogen is 25kg/ packet, and the amount being added every time is no more than 1.5 tons, and the amount that single is added is no more than 60 packets, In the case that the content of iron is high, ammonium dihydrogen phosphate is refined using multiple batches of；
Step 4: using cast iron connecting pipe to high pressure draught is passed through by air blower inside reverberatory furnace, wind pressure is in 6 kilograms of pressure More than, four Furnace doors of reverberatory furnace are then opened respectively, are passed through Furnace door using long trivet and are protruded into reverberatory furnace Portion is stirred the antimony liquid of molten state, so that iron ion is sufficiently reacted with phosphate, the operating temperature setting of reverberatory furnace at this time It is 920 degrees Celsius, blasting time is set as 25 minutes；
Step 5: closing air blower, cast iron connecting pipe removed, and floats at this point, can be precipitated one layer on the surface of antimony iron fusant Slag, the dross are phosphatic one or more kinds of mixtures such as ferric phosphate, ferrous phosphate, primary iron phosphate, have the part to be Then dross is slowly moved to the slag notch of reverberatory furnace by the simple substance antimony of precipitation using long trivet, then by manually being taken off Out；
Step 6: taking out part antimony liquid in reverberatory furnace, the iron-content in assay antimony liquid, stops to reflection stove heating, It is 30-50 minutes cooling to material under the blowing effect of air blower, material can be taken out and carry out subsequent process operation.
It is 48ppm according to iron content in the obtained antimony slab of the present embodiment.
In summary: the iron in antimony liquid can be controlled to 50ppm or less by this method and (be much higher than national standard No.1 antimony Ingot, 100ppm standard).This method, as iron removing reagent, will not be to bring new impurity in antimony liquid into using ammonium di-hydrogen phosphate, method behaviour Make simply, the scum of generation is not belonging to solid waste, is easy to sell or handle.It is operated by practice, ammonium di-hydrogen phosphate de-ferrous effect is good Good, production antimony slab can achieve No. zero antimony slab standard, satisfactorily resolved antimony smelt in iron tramp element to star metal product quality It influences.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment Intrinsic element.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding And modification, the scope of the present invention is defined by the appended.

Claims (7)

1. stibium fire smelting reverberatory furnace refines deferrization process, it is characterised in that: the technique includes the following steps:
Step 1: iron content antimony raw material is added in reverberatory furnace carries out arsenic removal, except lead is handled first；
Step 2: arsenic removal, except after lead processing operation, the substance inside reverberatory furnace is in the iron antimony fusant of molten state, then root Tapping total amount is calculated according to iron content in reverberatory furnace inner molten antimony iron liquid, the di(2-ethylhexyl)phosphate of iron is removed needed for calculating according to the total amount of iron The dosage of hydrogen ammonium；
Step 3: the ventilation equipment of reverberatory furnace are closed, and in order to reduce the oxidation of antimony, reduce oxygen content, then will be in reverberatory furnace The temperature in portion is heated between 850-950 degrees Celsius, and ammonium dihydrogen phosphate is then added into reverberatory furnace by the furnace roof of reverberatory furnace；
Step 4: using cast iron connecting pipe to high pressure draught is passed through by air blower inside reverberatory furnace, wind pressure is in 6 kilograms of pressure More than, four Furnace doors of reverberatory furnace are then opened respectively, are passed through Furnace door using long trivet and are protruded into reverberatory furnace Portion is stirred the antimony liquid of molten state, so that iron ion is sufficiently reacted with phosphate, the operating temperature setting of reverberatory furnace at this time Between 900-950 degrees Celsius, blasting time was set as between 40-50 minutes；
Step 5: closing air blower, cast iron connecting pipe removed, and floats at this point, can be precipitated one layer on the surface of antimony iron fusant Then dross is slowly moved to the slag notch of reverberatory furnace by slag using long trivet, then by manually being clawed；
Step 6: taking out part antimony liquid in reverberatory furnace, the iron-content in assay antimony liquid, if iron-content is excessively high, three times Continue to detect iron content in antimony liquid after repeating the above steps, until iron content reaches standard, stop to reflection stove heating, It is 30-50 minutes cooling to material under the blowing effect of air blower, material can be taken out and carry out subsequent process operation.
2. stibium fire smelting reverberatory furnace according to claim 1 refines deferrization process, it is characterised in that: the reverberatory furnace Furnace roof connection setting charging hopper.
3. stibium fire smelting reverberatory furnace according to claim 1 refines deferrization process, it is characterised in that: the biphosphate The chemical equation that the dosage of ammonium calculates basis is Fe3++PO3-=FePO4、Fe2++PO3-=Fe3(PO4)2、Fe3++HPO2-=Fe2 (HPO4)3And Fe3++H2PO-=Fe(H2PO4)3One or more of combination.
4. stibium fire smelting reverberatory furnace according to claim 1 refines deferrization process, it is characterised in that: the biphosphate Single packet quality of ammonium is 25kg/ packet, and the amount being added every time is no more than 1.5 tons, and the amount that single is added is no more than 60 packets, in iron In the case that content is high, ammonium dihydrogen phosphate is refined using multiple batches of.
5. stibium fire smelting reverberatory furnace according to claim 1 refines deferrization process, it is characterised in that: the dross is phosphorus Phosphatic one or more kinds of mixtures such as sour iron, ferrous phosphate, primary iron phosphate, have part for the simple substance antimony of precipitation.
6. stibium fire smelting reverberatory furnace according to claim 1 refines deferrization process, it is characterised in that: produced in the technique The boiling point of raw ferric phosphate is in 158 degrees centigrades, and readily volatilized, operator wears dedicated port in the process of work Cover.
7. stibium fire smelting reverberatory furnace according to claim 1 refines deferrization process, it is characterised in that: in the step 6 Repeating the temperature of reaction three times is respectively 850-1000 degrees Celsius, 800-950 degrees Celsius and 800-900 degrees Celsius.
CN201910491731.3A 2019-06-06 2019-06-06 Stibium fire smelting reverberatory furnace refines deferrization process Pending CN110042258A (en)

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CN201910491731.3A CN110042258A (en) 2019-06-06 2019-06-06 Stibium fire smelting reverberatory furnace refines deferrization process

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CN201910491731.3A CN110042258A (en) 2019-06-06 2019-06-06 Stibium fire smelting reverberatory furnace refines deferrization process

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113564384A (en) * 2021-07-23 2021-10-29 湖南辰州矿业有限责任公司 Production method of refined antimony with ultralow arsenic content

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113564384A (en) * 2021-07-23 2021-10-29 湖南辰州矿业有限责任公司 Production method of refined antimony with ultralow arsenic content

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