CN102433439A - Method for recovering rhenium from arsenic filter cake - Google Patents

Method for recovering rhenium from arsenic filter cake Download PDF

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CN102433439A
CN102433439A CN2011104229868A CN201110422986A CN102433439A CN 102433439 A CN102433439 A CN 102433439A CN 2011104229868 A CN2011104229868 A CN 2011104229868A CN 201110422986 A CN201110422986 A CN 201110422986A CN 102433439 A CN102433439 A CN 102433439A
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rhenium
arsenic
filter cake
extraction
arsenic filter
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CN102433439B (en
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吴海国
许小龙
王智友
姚金江
李婕
肖超
刘景槐
黄彦强
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YONGXIN XINTAI SILVER INDUSTRY Co Ltd
Hunan Research Institute of Non Ferrous Metals
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YONGXIN XINTAI SILVER INDUSTRY Co Ltd
Hunan Research Institute of Non Ferrous Metals
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Abstract

The invention provides a method for recovering rhenium from an arsenic filter cake. The method comprises the following steps: entering rhenium, arsenic and sulfur into a solution by adopting one-section alkali leaching and second-section oxidization and leaching, and simultaneously enriching lead, bismuth, copper and selenium in leaching slag; in the one-section leachate, converting rhenium into perrhenate in a form of sodium thioperrhenate by adopting an oxidization method, converting sodium thioarsenate into sodium arsenate, and separating out sulfur in a form of simple substance sulfur; removing arsenic from the solution obtained by oxidization conversion by using a sulfur dioxide reduction method or lime method; carrying out rhenium enrichment on the solution obtained after arsenic is removed; treating a rhenium reextraction liquid by using a potassium chloride precipitation method to obtain crude potassium perrhenate; and refining crude potassium perrhenate to obtain potassium perrhenate. The method has short process flow, high rhenium recovery rate and low treatment cost; and by using the method, the comprehensive utilization of valuable metals in the arsenic filter cake can be realized.

Description

A kind of method that from arsenic filter cake, reclaims rhenium
Technical field
The invention belongs to Non-ferrous Metallurgy and environmental improvement technical field, relate to a kind of new method that from arsenic-containing material, reclaims rhenium, particularly the arsenic filter cake with copper smelting by pyrometallurgy acid making system output is that raw material reclaims rhenium.
Background technology
Extract the main raw material of rhenium: independent rhenium mineral are less at occurring in nature, and it mainly is present in the molybdenum glance with oxide morphology, and molybdenum glance is normal and the copper-sulphide ores symbiosis.Rhenium is enriched in copper sulfide concentrate and brings the pyrometallurgical smelting system of copper in the selecting and purchasing process of copper-sulphide ores.In the pyrometallurgical smelting process of copper, the rhenium volatilization more than 82% gets in the spent acid stoste of flue gas acid preparing system, and wherein the form of 94% above sulfide gets into arsenic filter cake.Rhenium is present in the concentrated molybdenum ore equally, and in the oxidizing roasting process of concentrated molybdenum ore, rhenium gets into flue gas with the volatilization of rhenium heptoxide form, and rhenium is enriched in the flue dust behind the flue gas dust collection.Therefore the raw material that extracts rhenium mainly contains the arsenic filter cake of concentrated molybdenum ore oxidizing roasting flue dust and pyrometallurgical smelting system output.
The typical case reclaims the technology of rhenium from arsenic filter cake: the maximum enterprise of China's rhenium output is the subordinate's of Jiangxi Copper group smeltery, Guixi at present; A spot of rhenium is contained in the main body mine of this factory; In the process of selecting and purchasing smelting, in the arsenic filter cake of the acid making system output of rhenium entering pyrometallurgical smelting.Arsenic filter cake adopts the copper sulfate displacement to leach, and makes the As in the arsenic filter cake 2S 3Be converted into H 3AsO 3, make H toward the system aerating oxygen then 3AsO 3Be converted into H 3AsO 4, the Re in the copper sulfate displacement leaching process in the arsenic filter cake 2S 7With CuSO 4Reaction generates HReO 7And entering solution after the solution that contains arsenic, rhenium is removed arsenic through sulphur dioxide reduction, adopts ion exchange method to obtain the pregnant solution of rhenium, obtains the finished product ammonium perrhenate through condensing crystal production again.
The main drawback that adopts the copper sulfate substitution method to extract rhenium has:
(1) long flow path, cost is high: because the arsenic content in the arsenic filter cake up to more than 20%, must be handled arsenic in the process of extracting rhenium, adopt the copper sulfate substitution method to extract rhenium, in the process of handling, need use copper-bath twice, generate As twice 2O 3, technical process is long, and handles ltAs 2O 3Need to consume the 2t copper powder, handle the direct processing cost of 1t arsenic filter cake and surpassed 6000 yuan.
(2) the oxidation rinsing level of residue is big, and is hard to manage: handle the above washing residue of 1t arsenic filter cake output 1.2t, the residue water cut is high, is difficult to directly return the pyrometallurgical smelting system of copper.
(3) recovery of rhenium is low: in treating processes, the recovery of rhenium is merely 88%.
Summary of the invention
To the weak point of prior art, the invention provides a kind of method that from arsenic filter cake, reclaims rhenium, this technical process is short, and the rhenium recovery is high, and effective other valuable metals of enrichment.
For realizing above-mentioned purpose, technical scheme of the present invention is:
A kind of method that from arsenic filter cake, reclaims rhenium comprises following concrete steps:
(1) earlier with adding one section leaching of alkali lye behind the arsenic filter cake ore grinding, concentration of lye is 80g/L-120g/L, and controlling liquid-solid mass ratio is 3-5: 1, and extraction temperature is controlled at 55 ℃～95 ℃, extraction time 1h～5h; Cross and filter one section leach liquor and one section leached mud;
(2) above-mentioned one section leached mud is added two sections leachings of oxygenant, oxidant concentration is 20g/L-25g/L, and controlling liquid-solid mass ratio is 2-5: 1, and control solution oxide current potential >=200mv, 55 ℃～95 ℃ of extraction temperatures, extraction time 1h～5h; Cross and filter two sections leach liquors and two sections leached muds;
(3) above-mentioned one section leach liquor is added oxygenant oxidation, oxidising process solution system terminal point control of Electric potentials >=200mv;
(4) one section leach liquor after the oxidation mixes with two sections leach liquors, adopts using sulfur dioxide reduction method or lime precipitation arsenic removal;
(5) adopt extraction process separation and concentration rhenium then, the raffinate evaporating, concentrating and crystallizing is produced saltcake;
(6) extraction liquid behind the above-mentioned rich rhenium concentrates back adding Repone K, and crystallisation by cooling is separated out rough potassium perrhenate, and rough potassium perrhenate recrystallizing and refining gets potassium perrhenate.
Ore grinding described in the step (1) is that levigate extremely-100 orders of arsenic filter cake are accounted for more than 80%.
Alkali in the step (1) in the alkali lye is selected from sodium hydroxide, sodium sulphite or yellow soda ash.
Oxygenant in step (2) and the step (3) is selected from Youxiaolin, VAL-DROP, Manganse Dioxide, potassium permanganate or ydrogen peroxide 50.
The said using sulfur dioxide reduction method of step (4) is meant and adopts sulfurous gas to make reductive agent that reduction obtains arsenus acid, makes industrial white arsenic after the arsenus acid dehydration; Said lime precipitation is meant the employing lime precipitation, control deposition pH value >=6.0, and deposition obtains the Tricalcium arsenate product, as the raw material of producing white arsenic.
PH＞6.0 of control solution in the said arsenic removal process of step (4).
In the said extraction process separation and concentration of step (5) rhenium: extraction agent adopts N235 (trialkyl mixing tertiary amine); Help the collection agent to adopt secondary octanol; Thinner is a kerosene, and the volume of organic phase consists of: the secondary octanol of 20%N235+10%+70% kerosene, reverse-extraction agent employing mass concentration are 12%～15% ammoniacal liquor.
Behind the said adding Repone K of step (6), the concentration＞5g/L of control solution Free Chlorine potassium, solution is cooled to 5 ℃, and crystallisation by cooling is separated out rough potassium perrhenate.
Do further explanation and explanation in the face of the present invention down:
Arsenic filter cake according to the invention is meant the arsenic filter cake of output in concentrated molybdenum ore oxidizing roasting flue dust and the pyrometallurgical melting.The staple of the arsenic filter cake that the present invention is used (mass content) has Re:1580-1620g/t, As:20.0%-21.5%, S:53%-55%, Se:1.8%-1.9%, Bi:2.9%-3.2%, Cu:1%-1.5%, Pb:2.5%-2.8%, and all the other are impurity.
Know-why of the present invention comprises:
(1) one section alkali soaks, and arsenic filter cake adopts sodium hydroxide, yellow soda ash, sodium sulphite to leach, and following chemical reaction mainly takes place process:
As 2S 3+6NaOH→Na 3AsS 3+Na 3AsO 3+3H 2O
3S+6NaOH→Na 2SO 3+2Na 2S+3H 2O
As 2S 3+3Na 2S→2Na 3AsS 3
As 2S 3+3Na 2CO 3→Na 3AsS 3+Na 3AsO 3+3CO 2
Re 2S 7+Na 2S→2NaReS 4
4Re 2S 7+8NaOH→7NaReS 4+NaReO 4+4H 2O
4Re 2S 7+4Na 2CO 3→7NaReS 4+NaReO 4+4CO 2
Rhenium, arsenic, sulphur are got in one section leach liquor, and valuable metals such as other element such as copper, lead, bismuth, selenium remain in one section leached mud and obtain enrichment.
(2) two sections oxidations are leached
When one section leached mud adopted ydrogen peroxide 50, VAL-DROP, hypochlorite oxidation leaching, the chemical reaction of generation was following:
Re 2S 7+28H 2O 2→2HReO 4+7H 2SO 4+20H 2O
3Re 2S 7+7NaClO 3+3H 2O→6HReO 4+7NaCl+21S↓
Re 2S 7+7NaClO+H 2O→2HReO 4+7S↓+7NaCl
Make by the oxide compound of the sulfide of the rhenium of metallic sulfide parcel and low price rhenium and be oxidized to two sections leach liquors of rhenate entering; Two sections leached muds of process output are allocated the copper anode mud treatment process into and are comprehensively reclaimed selenium, copper, lead, bismuth.
(3) one sections leach liquor oxidations
When adopting ydrogen peroxide 50, VAL-DROP, one section leach liquor of Youxiaolin processing, the main chemical reactions of generation is following:
NaReS 4+4H 2O 2→NaReO 4+4H 2O+4S↓
3NaReS 4+4NaClO 3→3NaReO 4+4NaCl+12S↓
NaReS 4+4NaClO→NaReO 4+4S+4NaCl
Make rhenium be converted into perrhenate by thioperrhenate, thioarsenous acid sodium is converted into sodium arseniate.
(4) solution dearsenification
Sodium arseniate in the solution and calcium hydroxide reaction generate the Tricalcium arsenate deposition.
4Na 3AsO 4+6Ca(OH) 2→2Ca 3(AsO 4) 2+12NaOH
(5) rhenium-containing solution extraction and back extraction
The chemical reaction that mainly takes place when adopting the rhenium in the N235 extraction solution is following:
R 3N+H ++ReO 4 -→R 3NH 4ReO 4
Load organic phases adopts the ammoniacal liquor back extraction, and it is following that chemical reaction takes place:
R 3NH 4ReO 4+NH 4OH→R 3N+NH 4ReO 4+H 2O
(6) heavy rhenium
NH 4ReO 4+KCl→KReO 4↓+NH 4Cl
Compared with prior art, advantage of the present invention is:
(1) recovery of rhenium is high: the recovery of this technology whole process rhenium can reach more than 95%;
(2) flow process is short; Cost is low: two sections leachings of this process using, leach liquor oxidation, solution dearsenification, extracting and enriching Separation of Rhenium, the heavy rhenium of Repone K, the refining potassium perrhenate that obtains of thick potassium perrhenate; Processing technological flow is short, and the direct processing cost of 1t arsenic filter cake is lower than 4000 yuan.
(3) fully utilize other valuable metals: arsenic filter cake is after two sections leachings; Valuable metals such as the copper in the arsenic filter cake, lead, bismuth, selenium are enriched in the leached mud; Its grade improves more than 2.5 times; Can allocate the ANODE SLIME TREATMENT operation of copper smelting by pyrometallurgy factory into, the comprehensive valuable metals such as wherein selenium, lead, bismuth, copper that reclaim.
Description of drawings:
Fig. 1 is a kind of concrete process flow sheet that from arsenic filter cake, reclaims the method for rhenium of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention to be done further explanation and explanation, but the invention is not restricted to the scope of embodiment, percentage composition described in the embodiment all refers to the quality percentage composition except that specifying.
Embodiment 1:
Arsenic filter cake with domestic certain copper smelting plant is a raw material; Wherein staple (mass content) has Re:1580-1620g/t, As:20.0%-21.5%, S:53%-55%, Se:1.8%-1.9%, Bi:2.9%-3.2%, Cu:1%-1.5%, Pb:2.5%-2.8%, and all the other are impurity.
One section leaching process is allocated the sodium hydroxide of material quantity 50% into, liquid-solid ratio control 3: 1,90 ℃ of extraction temperature controls, extraction time 4h.The leaching yield of one section leaching process rhenium is 94%, and the leaching yield of arsenic is 98%, and the leaching yield of selenium is 3%, and lead, bismuth, copper are enriched in the leached mud, one section leached mud that leaches output material quantity about 40%.
The Youxiaolin of one section leached mud adding 25g/L carries out two sections leachings, control liquid-solid ratio control 3: 1,60 ℃ of extraction temperature controls, extraction time 2h, control solution oxide current potential >=200mv.The leaching yield 86% of two sections leaching process rheniums, the leaching yield 85% of arsenic, the leaching yield 5% of selenium, leached mud rate are 86%.
Total leaching yield of rhenium is 99.16% in the leaching process, and the leaching yield of arsenic is 99.7%, and the leaching yield of selenium is 7.85%.Contain selenium 4.96% in two sections leached muds, cupric 3.58%, leaded 7.7%, bismuth-containing 8.75%.
One section leach liquor adds the VAL-DROP oxidation of 25g/L, the current potential >=200mv of control solution, and the retention rate of Re in solution is 98.5%, the sulphur slag sulfur-bearing 86.5% of output contains Re100g/t in the oxidising process, contains arsenic and is lower than 1%.
The oxidizing solution of rhenium-containing, arsenic adds lime, and the pH value of control solution is 8.0, and the content of As is reduced to below the 200mg/L in the heavy arsenic tail washings, and the Tricalcium arsenate slag of output contains Re less than 5g/t.
It is the secondary octanol of 20%N235+10%+70% kerosene extraction that arsenic removal rhenium-containing solution adopts the organic phase volume proportion, and it is the rich rhenium solution that 12% ammoniacal liquor back extraction obtains rhenium-containing 12～15g/L that load organic phases adopts mass concentration.Rich rhenium solution directly adds Repone K, and Repone K is excessive, and the free potassium chloride concentration is 3g/L in the solution, and solution is cooled to 5 ℃, obtains rough potassium perrhenate product, and the content of potassium perrhenate is greater than 95%.Thick potassium perrhenate obtains containing potassium perrhenate greater than 99% refining potassium perrhenate through recrystallization.
Embodiment 2:
Arsenic filter cake with domestic certain copper smelting plant is a raw material; Staple (mass content) has Re:1580-1620g/t, As:20.0%-21.5%, S:53%-55%, Se:1.8%-1.9%, Bi:2.9%-3.2%, Cu:1%-1.5%, Pb:2.5%-2.8%, and all the other are impurity.
One section leaching process is allocated the yellow soda ash of material quantity 60% into, liquid-solid ratio control 4: 1,95 ℃ of extraction temperature controls, extraction time 5h.The leaching yield of one section leaching process rhenium is 92%, and the leaching yield of arsenic is 96%, and the leaching yield of selenium is 1%, and lead, bismuth, copper are enriched in the leached mud, one section leached mud that leaches output material quantity about 45%.
One section leached mud adds about 27% ydrogen peroxide 50 and carries out two sections leachings, control liquid-solid ratio control 4: 1,80 ℃ of extraction temperature controls, extraction time 4h, control solution oxide current potential >=200mv.The leaching yield 88% of two sections leaching process rheniums, the leaching yield 84% of arsenic, the leaching yield 5% of selenium, the leached mud rate is about 82%.
Total leaching yield of rhenium is 99.04% in the leaching process, and the leaching yield of arsenic is 99.36%, and the leaching yield of selenium is 5.95%.Contain selenium 4.42% in two sections leached muds, cupric 3.12%, leaded 6.73%, bismuth-containing 7.64%.
One section leach liquor adds about 27% hydrogen peroxide oxidation, the current potential >=200mv of control solution, and the retention rate of Re in solution is 98.5%, the sulphur slag sulfur-bearing 86.5% of output in the oxidising process contains and is lower than Re100g/t, contains arsenic and is lower than 1%.
The oxidizing solution of rhenium-containing, arsenic adds lime, and the pH value of control solution is 8.0, and the content of As is reduced to below the 200mg/L in the heavy arsenic tail washings, and the Tricalcium arsenate slag of output contains Re less than 5g/t.
It is the secondary octanol of 20%N235+10%+70% kerosene extraction that arsenic removal rhenium-containing solution adopts the organic phase volume proportion, and it is the rich rhenium solution that 15% ammoniacal liquor back extraction obtains rhenium-containing 12～15g/L that load organic phases adopts mass concentration.Rich rhenium solution directly adds Repone K, and Repone K is excessive, and the free potassium chloride concentration is 3g/L in the solution, and solution is cooled to 5 ℃, obtains rough potassium perrhenate product, and the content of potassium perrhenate is greater than 95%.Thick potassium perrhenate obtains containing potassium perrhenate greater than 99% refining potassium perrhenate through recrystallization.

Claims (9)

1. a method that from arsenic filter cake, reclaims rhenium is characterized in that, comprises following concrete steps:
(1) earlier with adding one section leaching of alkali lye behind the arsenic filter cake ore grinding, concentration of lye is 80g/L-120g/L, and controlling liquid-solid mass ratio is 3-5: 1, and extraction temperature is controlled at 55 ℃～95 ℃, extraction time 1h～5h; Cross and filter one section leach liquor and one section leached mud;
(2) above-mentioned one section leached mud is added two sections leachings of oxygenant, oxidant concentration is 20g/L-25g/L, and controlling liquid-solid mass ratio is 2-5: 1, and control solution oxide current potential >=200mv, 55 ℃～95 ℃ of extraction temperatures, extraction time 1h～5h; Cross and filter two sections leach liquors and two sections leached muds;
(3) above-mentioned one section leach liquor is added oxygenant oxidation, oxidising process solution system terminal point control of Electric potentials >=200mv;
(4) one section leach liquor after the oxidation mixes with two sections leach liquors, adopts using sulfur dioxide reduction method or lime precipitation arsenic removal;
(5) adopt extraction process separation and concentration rhenium then, the raffinate evaporating, concentrating and crystallizing is produced saltcake;
(6) extraction liquid behind the above-mentioned rich rhenium concentrates back adding Repone K, and crystallisation by cooling is separated out rough potassium perrhenate, and rough potassium perrhenate recrystallizing and refining gets potassium perrhenate.
2. according to the said a kind of method that from arsenic filter cake, reclaims rhenium of claim 1, it is characterized in that ore grinding described in the step (1) is that levigate extremely-100 orders of arsenic filter cake are accounted for more than 80%.
3. according to the said a kind of method that from arsenic filter cake, reclaims rhenium of claim 1, it is characterized in that the alkali in the step (1) in the alkali lye is selected from sodium hydroxide, sodium sulphite or yellow soda ash.
4. according to the said a kind of method that from arsenic filter cake, reclaims rhenium of claim 1, it is characterized in that the oxygenant in step (2) and the step (3) is selected from Youxiaolin, VAL-DROP, Manganse Dioxide, potassium permanganate or ydrogen peroxide 50.
5. according to the said a kind of method that from arsenic filter cake, reclaims rhenium of claim 1, it is characterized in that the said using sulfur dioxide reduction method of step (4) is meant and adopts sulfurous gas to make reductive agent that reduction obtains arsenus acid, makes industrial white arsenic after the arsenus acid dehydration;
Said lime precipitation is meant the employing lime precipitation, control deposition pH value >=6.0, and deposition obtains the Tricalcium arsenate product, as the raw material of producing white arsenic.
6. according to the said a kind of method that from arsenic filter cake, reclaims rhenium of claim 1, it is characterized in that pH＞6.0 of control solution in the said arsenic removal process of step (4).
7. according to the said a kind of method that from arsenic filter cake, reclaims rhenium of claim 1; It is characterized in that in the said extraction process separation and concentration of step (5) rhenium: extraction agent adopts trialkyl mixing tertiary amine, is called for short N235; Help the collection agent to adopt secondary octanol; Thinner is a kerosene, and the volume of organic phase consists of: the secondary octanol of 20%N235+10%+70% kerosene, reverse-extraction agent employing mass concentration are 12%～15% ammoniacal liquor.
8. according to the said a kind of method that from arsenic filter cake, reclaims rhenium of claim 1, it is characterized in that, behind the said adding Repone K of step (6), the concentration＞5g/L of control solution Free Chlorine potassium, solution is cooled to 5 ℃, and crystallisation by cooling is separated out rough potassium perrhenate.
9. according to the said a kind of method that from arsenic filter cake, reclaims rhenium of claim 1; It is characterized in that; Said arsenic filter cake is meant the arsenic filter cake of output in concentrated molybdenum ore oxidizing roasting flue dust and the pyrometallurgical melting; The mass content of staple is following: Re:1580-1620g/t, As:20.0%-21.5%, S:53%-55%, Se:1.8%-1.9%, Bi:2.9%-3.2%, Cu:1%-1.5%, Pb:2.5%-2.8%, all the other are impurity.
CN2011104229868A 2011-12-16 2011-12-16 Method for recovering rhenium from arsenic filter cake Expired - Fee Related CN102433439B (en)

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CN107988487A (en) * 2017-10-30 2018-05-04 四川英创环保科技有限公司 A kind of lead skim wet oxidation decomposition technique
CN108677010A (en) * 2018-06-14 2018-10-19 中核通辽铀业有限责任公司 A kind of ground-dipping uranium extraction comprehensive recycling process
CN108929960A (en) * 2018-07-23 2018-12-04 安徽华西稀有金属材料有限公司 A method of ammonium perrhenate is prepared from rhenium-containing solution
CN109930004A (en) * 2019-04-12 2019-06-25 江西铜业股份有限公司 A kind of method of arsenic filter cake resource utilization
CN110157909A (en) * 2018-01-29 2019-08-23 安徽华晶微电子材料科技有限公司 Molybdenum metal materials industry recovery method in a kind of waste
CN112708762A (en) * 2020-11-30 2021-04-27 核工业北京化工冶金研究院 Method for preparing potassium perrhenate through back-extraction crystallization
CN114059077A (en) * 2021-10-27 2022-02-18 湖南有色金属研究院有限责任公司 Arsenic filter cake treatment method

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