CN105349777A - Method for conducting microwave low temperature activation and ultrasonic coupling coupling leaching on oxygen vulcanization mixed ore - Google Patents

Method for conducting microwave low temperature activation and ultrasonic coupling coupling leaching on oxygen vulcanization mixed ore Download PDF

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Publication number
CN105349777A
CN105349777A CN201510675047.2A CN201510675047A CN105349777A CN 105349777 A CN105349777 A CN 105349777A CN 201510675047 A CN201510675047 A CN 201510675047A CN 105349777 A CN105349777 A CN 105349777A
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oxygen
ore
temperature
composite ore
ultrasonic wave
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CN105349777B (en
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彭金辉
杨坤
李世伟
张利波
马爱元
陈伟恒
谢峰
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Kunming University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/12Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
    • C22B3/14Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions containing ammonia or ammonium salts
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Engineering & Computer Science (AREA)
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  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention relates to a method for conducting microwave low-temperature activation and ultrasonic coupling leaching on oxygen vulcanization mixed ore, and belongs to the technical field of microwave metallurgy. The method comprises the steps that firstly, the oxygen vulcanization mixed ore and activator are uniformly mixed after being smashed, and a mixed material is obtained; the activator is Na2O2 or Na2CO3, and the added quantity of the activator is 5-40% of the mass of the oxygen vulcanization mixed ore; secondly, the obtained mixed material is transferred into a microwave oven to be continuously heated after being heated to the temperature of 50-150 DEG C in tradition, then is heated to the final temperature which is lower than the kindling point of the oxygen vulcanization mixed ore at 0-300 DEG C , the mixed material is subjected to low-temperature activation for 2-60 min, and the activated material is obtained; and finally, the obtained activated material is subjected to ultrasonic wave enhancing leaching, and leaching liquor is obtained. The method for conducting microwave low-temperature activation and ultrasonic coupling leaching on the oxygen vulcanization mixed ore has the characteristics of being high in processing efficiency, friendly to environment, and high in resource recovery rate.

Description

A kind of microwave low-temperature activation-ultrasonic wave-coupled leaches the method for oxygen sulfuration composite ore
Technical field
The present invention relates to the method that a kind of microwave low-temperature activation-ultrasonic wave-coupled leaches oxygen sulfuration composite ore, belong to microwave metallurgical technical field.
Background technology
Along with rapid development of economy, nonferrous metal resource demand is increasing, and traditional tractable sulphide ores resource reduces day by day, can not meet this demand; Therefore must utilize the non-traditional resources such as burning ore deposit, composite ore, metallurgical slag dirt, competitively carry out the research effectively utilizing non-ferrous metal non-traditional resources both at home and abroad for this reason.
Metallurgical industry in modern times is over more than 100 year, and the non-ferrous metal tradition selecting and smelting technologies such as copper nickel zinc are mainly for the treatment of sulphide ores.But the difficult Mineral resources such as current China copper nickel zinc, based on the oxidase complex ore deposit of many metal many ore deposits phase and composite ore, adopt traditional selecting and smelting technology high efficiency separation to extract.The great demand of country that this patent utilizes around strategic non-ferrous metal non-traditional resources high-efficiency cleaning, for non-traditional complicated Metallurgical resources, there is many metals, many ore deposits phase, character feature that basic gangue content is high, devise the short route of metal simultaneous extraction more than new technology path.
Summary of the invention
For above-mentioned prior art Problems existing and deficiency, the invention provides the method that a kind of microwave low-temperature activation-ultrasonic wave-coupled leaches oxygen sulfuration composite ore.Present method has that processing efficiency is high, environmental friendliness, and the feature that resource recovery is high, the present invention is achieved through the following technical solutions.
Microwave low-temperature activation-ultrasonic wave-coupled leaches a method for oxygen sulfuration composite ore, and its concrete steps are as follows:
(1) mix after first oxygen sulfuration composite ore and activator being pulverized and obtain mixture, activator is Na 2o 2or Na 2cO 3, the add-on of activator is 5 ~ 40% of oxygen sulfuration composite ore quality;
(2) after mixture step (1) obtained is 50 ~ 150 DEG C by traditional heating to temperature, then transfer in microwave oven and continue heating, be heated to outlet temperature and obtain activating material lower than point of ignition oxygen sulfuration composite ore 0 ~ 300 DEG C of low-temperature activation 2 ~ 60min;
(3) activation material step (2) obtained adopts intensified by ultrasonic wave to leach and obtains leach liquor.
In described step (1), oxygen sulfuration composite ore is oxygen-sulfur mixed copper ore or oxysulphied zinc ore.
In intensified by ultrasonic wave leaching process in described step (3): extraction temperature is 25 ~ 50 DEG C, rotating speed is 200 ~ 600rpm, and extraction time is 0.5 ~ 2h, and ultrasonic power is 500 ~ 3000W.
In described step (3), leaching agent is compound coordination leach liquor, and compound coordination leach liquor is the mixing leaching agent of the arbitrary proportion of oronain and ammoniacal liquor.
The invention has the beneficial effects as follows: the present invention is directed to non-traditional complicated Metallurgical resources composition complicated, leach the present situation of route blank, have studied the activator that a kind of wave absorbtion that adulterates in mineral is good, utilize microwave to carry out low-temperature activation, and utilize ultrasonic wave to carry out the new non-traditional complicated Metallurgical resources treatment process of Strengthen education.Leaching efficiency is high, environmental friendliness, and handling object resource is extensive, is a kind of new technology with wide range of industrial applications prospect.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention;
Fig. 2 is different activator Na 2o 2under content, the leaching yield of zinc in oxysulphied zinc ore.In oxysulphied zinc ore, the grade of zinc is 35.04wt%, and microwave heating temperature is 600 DEG C, and soaking time is 10min.Leach liquid level oronain solution: c (NH 3) t=7.5mol/L, c (NH 3h 2o): c (NH 4cl)=1:1, ultrasonic power is 2000W, and leaching condition is: 40 DEG C, 500rpm, liquid-solid ratio 10:1, total ammonia density 7.5mol/L; C (NH 4 +)/C (NH 3)=1:1.As can be seen from the figure along with Na 2o 2the increase of content, in the complicated zinc ore of oxysulphied, the leaching yield of zinc increases gradually.Work as Na 2o 2when content is oxysulphied zinc ore quality 25%, the leaching yield of zinc can reach 82.06%.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1
As shown in Figure 1, this microwave low-temperature activation-ultrasonic wave-coupled leaches the method for oxygen sulfuration composite ore, and its concrete steps are as follows:
(1) mix after first 500g oxygen sulfuration composite ore and activator being pulverized and obtain mixture, activator is Na 2o 2, the add-on of activator is 5% of oxygen sulfuration composite ore quality; Wherein oxygen sulfuration composite ore is oxysulphied zinc ore, and the grade of zinc is 35.04wt%;
(2) after mixture step (1) obtained is 50 DEG C by traditional heating to temperature, then transfer in microwave oven and continue heating (microwave power is set as 500W), be heated to outlet temperature and obtain activating material lower than point of ignition oxygen sulfuration composite ore 0 DEG C of (800 DEG C) low-temperature activation 2min;
(3) activation material step (2) obtained is that the ratio of 1:10ml/g adds c (NH with liquid-solid ratio 3) tthe oronain compound coordination leaching agent of=5mol/L is wherein the NH of concentration 1:1 in oronain compound coordination leaching agent 3h 2o and NH 4cl mixture is 25 DEG C at extraction temperature, and rotating speed is 200rpm, and extraction time is 0.5h, and ultrasonic power is adopt intensified by ultrasonic wave to leach under 500W condition to obtain leach liquor.
In the leach liquor that the present embodiment prepares, the leaching yield of zinc can reach 60.73%.
Embodiment 2
As shown in Figure 1, this microwave low-temperature activation-ultrasonic wave-coupled leaches the method for oxygen sulfuration composite ore, and its concrete steps are as follows:
(1) mix after first 500g oxygen sulfuration composite ore and activator being pulverized and obtain mixture, activator is Na 2o 2, the add-on of activator is 20% of oxygen sulfuration composite ore quality; Wherein oxygen sulfuration composite ore is oxygen sulfuration mixed copper ore, and the grade of copper is 24.48wt%;
(2) after mixture step (1) obtained is 100 DEG C by traditional heating to temperature, then transfer in microwave oven and continue heating (microwave power is set as 3000W), be heated to outlet temperature and obtain activating material lower than point of ignition oxygen sulfuration composite ore 150 DEG C of low-temperature activation 30min;
(3) activation material step (2) obtained is that the ratio of 1:10ml/g adds c (NH with liquid-solid ratio 3) tthe oronain compound coordination leaching agent of=10mol/L is wherein the NH of concentration 1:1 in oronain compound coordination leaching agent 3h 2o and NH 4cl mixture is 40 DEG C at extraction temperature, and rotating speed is 400rpm, and extraction time is 2h, and ultrasonic power is adopt intensified by ultrasonic wave to leach under 3000W condition to obtain leach liquor.
In the leach liquor that the present embodiment prepares, the leaching yield of copper can reach 80.12%.
Embodiment 3
As shown in Figure 1, this microwave low-temperature activation-ultrasonic wave-coupled leaches the method for oxygen sulfuration composite ore, and its concrete steps are as follows:
(1) mix after first 500g oxygen sulfuration composite ore and activator being pulverized and obtain mixture, activator is Na 2o 2, the add-on of activator is 20% of oxygen sulfuration composite ore quality; Wherein oxygen sulfuration composite ore is oxygen sulfuration mixing zinc ore, and the grade of zinc is 35.42wt%;
(2) after mixture step (1) obtained is 150 DEG C by traditional heating to temperature, then transfer in microwave oven and continue heating (microwave power is set as 800W), be heated to outlet temperature and obtain activating material lower than point of ignition oxygen sulfuration composite ore 150 DEG C of (650 DEG C) low-temperature activation 30min;
(3) activation material step (2) obtained is that the ratio of 1:7.5ml/g adds c (NH with liquid-solid ratio 3) tthe oronain compound coordination leaching agent of=7.5mol/L is wherein the NH of concentration 1:1 in oronain compound coordination leaching agent 3h 2o and NH 4cl mixture is 50 DEG C at extraction temperature, and rotating speed is 600rpm, and extraction time is 1h, and ultrasonic power is adopt intensified by ultrasonic wave to leach under 1000W condition to obtain leach liquor.
In the leach liquor that the present embodiment prepares, the leaching yield of zinc can reach 61.26%.
Embodiment 4
As shown in Figure 1, this microwave low-temperature activation-ultrasonic wave-coupled leaches the method for oxygen sulfuration composite ore, and its concrete steps are as follows:
(1) first get 6 parts of 500g oxygen sulfuration composite ore, mix after adding the activator pulverizing of oxygen sulfuration composite ore quality 0%, 5%, 10%, 15%, 20%, 25% respectively and obtain mixture, activator is Na 2o 2; Wherein oxygen sulfuration composite ore is oxygen sulfuration mixing zinc ore, and the grade of zinc is 35.04wt%;
(2) after mixture step (1) obtained is 150 DEG C by traditional heating to temperature, then transfer in microwave oven and continue heating (microwave power is set as 800W), be heated to outlet temperature and obtain activating material lower than point of ignition oxygen sulfuration composite ore 200 DEG C of (600 DEG C) low-temperature activation 10min;
(3) activation material step (2) obtained is that the ratio of 1:10ml/g adds c (NH with liquid-solid ratio 3) tthe oronain compound coordination leaching agent of=7.5mol/L is wherein the NH of concentration 1:1 in oronain compound coordination leaching agent 3h 2o and NH 4cl mixture is 50 DEG C at extraction temperature, and rotating speed is 600rpm, and extraction time is 1h, and ultrasonic power is adopt intensified by ultrasonic wave to leach under 1000W condition to obtain leach liquor.
In the leach liquor that the present embodiment prepares, the leaching yield of zinc as shown in Figure 2, works as Na 2o 2when content is oxysulphied zinc ore quality 25%, leach 0.75h, the leaching yield of zinc can reach 82.06%.
Simultaneous test
By 500g oxygen sulfuration composite ore (35.04wt%) with 25% Na 2o 2after mixing, be placed in retort furnace and be heated to 600 DEG C, insulation 10min, obtain activating material.In the activation material of gained, add c (NH 3) tthe oronain compound coordination leaching agent of=7.5mol/L, and carry out agitation leach, be the NH of concentration 1:1 in oronain compound coordination leaching agent 3h 2o and NH 4cl coordination forms, and activation material is 1:10 with the liquid-solid ratio that mixes of leaching agent, and extraction temperature is 50 DEG C, and rotating speed is 600rpm, and extraction time is 0.75h, and ultrasonic power is 1000W, and final zinc leaching rate is 30.56%.
Embodiment 5
As shown in Figure 1, this microwave low-temperature activation-ultrasonic wave-coupled leaches the method for oxygen sulfuration composite ore, and its concrete steps are as follows:
(1) mix after first 500g oxygen sulfuration composite ore and activator being pulverized and obtain mixture, activator is Na 2cO 3, the add-on of activator is 20% of oxygen sulfuration composite ore quality; Wherein oxygen sulfuration composite ore is oxygen sulfuration mixing zinc ore, and the grade of zinc is 35.23wt%;
(2) after mixture step (1) obtained is 150 DEG C by traditional heating to temperature, then transfer in microwave oven and continue heating (microwave power is set as 800W), be heated to outlet temperature and obtain activating material lower than point of ignition oxygen sulfuration composite ore 150 DEG C of (650 DEG C) low-temperature activation 30min;
(3) activation material step (2) obtained is that the ratio of 1:5ml/g adds c (NH with liquid-solid ratio 3) tthe oronain compound coordination leaching agent of=10mol/L is wherein the NH of concentration 5:1 in oronain compound coordination leaching agent 3h 2o and NH 4cl mixture is 40 DEG C at extraction temperature, and rotating speed is 400rpm, and extraction time is 0.5h, and ultrasonic power is adopt intensified by ultrasonic wave to leach under 2000W condition to obtain leach liquor.
In the leach liquor that the present embodiment prepares, the leaching yield of zinc can reach 72.42%.
Embodiment 5
As shown in Figure 1, this microwave low-temperature activation-ultrasonic wave-coupled leaches the method for oxygen sulfuration composite ore, and its concrete steps are as follows:
(1) mix after first 500g oxygen sulfuration composite ore and activator being pulverized and obtain mixture, activator is Na 2cO 3, the add-on of activator is 40% of oxygen sulfuration composite ore quality; Wherein oxygen sulfuration composite ore is oxygen sulfuration mixing zinc ore, and the grade of zinc is 35.23wt%;
(2) after mixture step (1) obtained is 100 DEG C by traditional heating to temperature, then transfer in microwave oven and continue heating (microwave power is set as 800W), be heated to outlet temperature and obtain activating material lower than point of ignition oxygen sulfuration composite ore 300 DEG C of (500 DEG C) low-temperature activation 60min;
(3) activation material step (2) obtained is that the ratio of 1:10ml/g adds c (NH with liquid-solid ratio 3) tthe oronain compound coordination leaching agent of=10mol/L is wherein the NH of concentration 10:1 in oronain compound coordination leaching agent 3h 2o and NH 4cl mixture is 35 DEG C at extraction temperature, and rotating speed is 500rpm, and extraction time is 1.5h, and ultrasonic power is adopt intensified by ultrasonic wave to leach under 2000W condition to obtain leach liquor.
In the leach liquor that the present embodiment prepares, the leaching yield of zinc can reach 85.56%.
Below by reference to the accompanying drawings the specific embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the ken that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.

Claims (4)

1. microwave low-temperature activation-ultrasonic wave-coupled leaches a method for oxygen sulfuration composite ore, it is characterized in that concrete steps are as follows:
(1) mix after first oxygen sulfuration composite ore and activator being pulverized and obtain mixture, activator is Na 2o 2or Na 2cO 3, the add-on of activator is 5 ~ 40% of oxygen sulfuration composite ore quality;
(2) after mixture step (1) obtained is 50 ~ 150 DEG C by traditional heating to temperature, then transfer in microwave oven and continue heating, be heated to outlet temperature and obtain activating material lower than point of ignition oxygen sulfuration composite ore 0 ~ 300 DEG C of low-temperature activation 2 ~ 60min;
(3) activation material step (2) obtained adopts intensified by ultrasonic wave to leach and obtains leach liquor.
2. microwave low-temperature activation according to claim 1-ultrasonic wave-coupled leaches the method for oxygen sulfuration composite ore, it is characterized in that: in described step (1), oxygen sulfuration composite ore is oxygen-sulfur mixed copper ore or oxysulphied zinc ore.
3. microwave low-temperature activation according to claim 1-ultrasonic wave-coupled leaches the method for oxygen sulfuration composite ore, it is characterized in that: in the intensified by ultrasonic wave leaching process in described step (3): extraction temperature is 25 ~ 50 DEG C, rotating speed is 200 ~ 600rpm, extraction time is 0.5 ~ 2h, and ultrasonic power is 500 ~ 3000W.
4. the microwave low-temperature activation according to claim 1 or 3-ultrasonic wave-coupled leaches the method for oxygen sulfuration composite ore, it is characterized in that: in described step (3), leaching agent is compound coordination leach liquor, and compound coordination leach liquor is the mixing leaching agent of the arbitrary proportion of oronain and ammoniacal liquor.
CN201510675047.2A 2015-10-19 2015-10-19 A kind of method that microwave low-temperature activation ultrasonic wave-coupled leaches oxygen vulcanization composite ore Expired - Fee Related CN105349777B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112662893A (en) * 2020-12-14 2021-04-16 成都大川锂电科技有限公司 Method for leaching lithium ore by microwave-ultrasonic coupling

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Publication number Priority date Publication date Assignee Title
CN1401801A (en) * 2002-04-12 2003-03-12 昆明理工大学 Preparation of active zinc oxide from zinc dross by ultrasonic-microwave process
CN103352127A (en) * 2013-04-07 2013-10-16 昆明理工大学 Method for recovering zinc from zinc flue dust leaching residue through ultrasonic wave assistance
CN103352116A (en) * 2013-04-07 2013-10-16 昆明理工大学 Method for recovering zinc from high iron and high lead leaching residue through microwave-ultrasonic wave combination

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Publication number Priority date Publication date Assignee Title
CN1401801A (en) * 2002-04-12 2003-03-12 昆明理工大学 Preparation of active zinc oxide from zinc dross by ultrasonic-microwave process
CN103352127A (en) * 2013-04-07 2013-10-16 昆明理工大学 Method for recovering zinc from zinc flue dust leaching residue through ultrasonic wave assistance
CN103352116A (en) * 2013-04-07 2013-10-16 昆明理工大学 Method for recovering zinc from high iron and high lead leaching residue through microwave-ultrasonic wave combination

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112662893A (en) * 2020-12-14 2021-04-16 成都大川锂电科技有限公司 Method for leaching lithium ore by microwave-ultrasonic coupling

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