CN1181925C - Scandium extraction method of river channel sedimentation - Google Patents
Scandium extraction method of river channel sedimentation Download PDFInfo
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- CN1181925C CN1181925C CNB031353541A CN03135354A CN1181925C CN 1181925 C CN1181925 C CN 1181925C CN B031353541 A CNB031353541 A CN B031353541A CN 03135354 A CN03135354 A CN 03135354A CN 1181925 C CN1181925 C CN 1181925C
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Abstract
The present invention relates to a scandium extraction method for river channel deposited sand. The present invention is characterized in that the deposited sand with the diameter smaller than 2mm is used as raw material; titanaugite ore concentrate is separated from the deposited sand by the techniques of grading, gravity separation, magnetic separation, electrostatic separation, etc.; scandium products are extracted through the techniques of leaching, extraction, phase inversion, purification, etc. The present invention uses the deposited sand of the river channel of the Yangtse River as, can changing wastes into valuables and can save mineral resources; after the three-gorge reservoir is formed, the deposited sand in the river channel of the Chongqing section of the Yangtse River is sufficient; the present invention has the advantages of no limitation, wide distribution, low cost and obvious economic benefit; the present invention has an obvious competitive advantage in markets; the present invention can not destroy ecological environment and is favorable for environment protection; after the scandium is extracted, the deposited sand is clean, is used for construction industry for increasing the quality of concrete and is also favorable for engineering construction.
Description
Technical field
The present invention relates to a kind of extracting method, especially a kind of method of from river course silt sand, extracting the scandium product to scandium.
Background technology
Scandium is one of the basic material of 21 century advanced material, also is one of rising star's element that changes conventional industries, and its scope of application is in rising stage and expansionary phase, and it is mainly used in high-tech areas such as Aero-Space.At present, compose of scandium is stored in the natural mineral more, and the mineral matter in the Nature is limited, present stage, the common method of extracting scandium from mineral is: test portion preliminary treatment-magnetic separation or (electric separation)-scandium concentrate-hydrochloric acid adding consolvent leaching-extraction-pickling-back extraction-oxalic acid are made with extra care-roasting-scandium oxide, because mineral resources are limited, mineral resources are non-renewable, and this method expense height that from mineral, extracts scandium, cause the scandium product to be unfavorable for the competition in market.In addition, this scandium extracting method is destroyed ecological environment easily to the digging of mineral products, also can cause certain pollution to environment in process of production.
Along with domestic high-grade continuous exhaustion that contains the scandium natural minerals, the scandium product price is high again, is absolutely necessary and produce scandium, and this has proposed a new problem for the brainstrust that extracts scandium.
Summary of the invention
The method for extracting scandium that the purpose of this invention is to provide a kind of river course silt sand extracts scandium from the silt sand of rivers, turn waste into wealth, and the scandium resource is fully used, and reduces the scandium product price, enlarges range of application.
Concrete scheme of the present invention is: a kind of method for extracting scandium of river course silt sand, it is characterized in that the cut-off footpath is a raw material less than 2mm silt sand, and carry out as follows:
(1). from silt sand, select the scandium concentrate
Be 80 purpose vibratory sieve classifications with sieve aperture earlier, again with spiral concentrator and spiral chute gravity treatment+80 orders and-80 purpose silt sand respectively, wherein on the sieve+80 purpose silt sand enter spiral concentrator ,-80 purpose silt sand enter spiral chute under the sieve, 37.5% the mine tailing of skimming; To contain the scandium grade in order improving, to guarantee monomer dissociation, gravity concentrate is merged into the closed cycle into ball milling and spiral classifier formation, and the control granularity is 200 orders, sends into the low intensity magnetic separation machine, and magnetic product is an iron ore concentrate; Nonmagnetic portion is through high-gradient magnetic separation, 50.81% the mine tailing of can skimming, and concentrate is through hydroclone classification, and the control granularity is 400 orders, and 400 orders enter table concentration; Gravity tailings discards, and the chats Returning process enters electric separation behind the concentrate drying; Electrostatic separation tailing is incorporated the shaking table chats into, and concentrate then is the scandium concentrate.
(2), from the scandium concentrate, extract scandium
(A), the leaching of scandium
Be finely ground to-320 purpose scandium concentrate, add hydrochloric acid in the titanium reactor, concentration is 22.8%, and liquid-solid ratio is 2.5: 1, adds 7
#Cosolvent 30～50g/t, 88 ℃～95 ℃ of extraction temperatures stirred 8.5～10.5 hours.
(B), extraction stoste produces
Get immersion liquid 200ml and be heated to 90 ℃, add Na
2SO
49～12g stirred 20 minutes, added NaClO again
34～5.5g continues to stir 20 minutes, uses Na then
2CO
3Adjust PH=2.3, at this moment solution is salmon pink, constantly stirs about 2～3 hours, leaves standstill back filtration about 1 hour, and filtrate is the used stoste of extraction.
(C), the extraction of scandium
Get stoste 1000ml, adjust PH=1.26, add 48～50ml tbp and 3～5ml kerosene, stirred 3 minutes, leave standstill and abandoned water in 20 minutes, wash 2～4 times, stirred 3 minutes at every turn, leave standstill and abandoned water in 20 minutes, then carry out secondary and strip, add hydrochloric acid 42～56ml of 5% at every turn, vibrated 1～2 minute, left standstill 30 minutes, and told extract.
(D), the phase inversion of scandium
The oxalic acid that adds extraction liquid measure 10～18% stirs in extract, adjusts PH=4.5 with NaOH, leaves standstill filtration, and filter residue is the head product of scandium.
(E), the purification of scandium
Adopt above-mentioned steps (A), (B), (C) once more and (D) handle head product, filter residue is put into cabinet-type electric furnace again and carried out the high temperature ashing, temperature is controlled at below 1000 ℃, when product is white powder, promptly gets scandium oxide.
(F), metal scandium produces
With step (5) gained purity be 87.27% thick scandium with the reduction of vacuum metallurgy equipment, can make metal scandium.
The silt of river course described in the present invention sand has through the mineral that chemical analysis mainly contains: ilmenite, titanomagnetite, scandium, hornblend, plagioclase, chlorite, quartz, calcite, mica etc., and the scandium amount that contains of each mineral sees the following form 1:
Essential mineral contains scandium amount (g/t) in the table 1 river course silt sand
| Mineral name | Ilmenite | Titanomagnetite | Scandium | Hornblend | Plagioclase | Chlorite | Quartzy | Calcite | Mica |
| Contain the scandium amount | 101 | 18.8 | 121 | 28 | 0.41 | 1.17 | ＜0.17 | ＜0.2 | ＜4.01 |
As can be seen from Table 1, containing scandium in the ilmenite per ton in river course silt sand is 101g, and it is the highest that scandium contains scandium, is 121g/t, and they are the essential minerals that contain scandium in the river course silt sand, is the main object that reclaims, and also is the main component of carrying scandium in the river course silt sand; Contain the scandium amount higher relatively hornblend, titanomagnetite arranged; Its quartz, plagioclase, chlorite etc. contain the scandium amount that contains (6.6g/t) that the scandium amount all is lower than raw ore, can remove in the steps such as magnetic separation, electric separation in selected the sorting in the process through gravity treatment of scandium.
Since in the river course silt sand scandium to contain scandium higher, can from the river course becomes silted up sand, select the scandium concentrate again, therefore, first link of the present invention is exactly to extract the scandium concentrate from silt sand.
The present invention adopts extract technology to extract and contains the scandium immersion liquid after obtaining the scandium concentrate, leachate is handled obtaining stoste again, again stoste is extracted, and can get following extraction results:
Table 2
| Sequence number | Stock solution flow (ml/10s) | Grade (g/t) | Come together and flow quantity (ml/10s) | Collection fluid grade (g/t) | Abandon water grade (g/t) | Actual extraction rate (%) | Theoretical extraction yield (%) |
| 1234 is average | 51 50 52 51 51 | 17 17 17 17 17 | 5 6 5 5 5.25 | 155.74 128.04 159.44 157.28 150.12 | 1.24 1.14 1.17 1.20 1.19 | 89.82 90.38 90.18 90.70 90.27 | 93.45 94.13 93.80 93.66 93.76 |
Table 2 is 4 experimental result tables, and as known from Table 2: total actual extraction rate is 90.27%, and is lower by 3.49% than theoretical value, illustrates that it is feasible that stoste is extracted the technology of carrying scandium.
To obtaining feed liquid after the extract processing, adopt oxalate precipitation method to realize the phase inversion of scandium again, result of the test sees Table 3
Table 3
| Reduction of feed volume (g) | Grade (g/t) | Precipitation capacity (g) | Scandium grade (%) | The rate of recovery (%) |
| 830 | 149.9 | 128.98 | 87.27 | 90.47 |
Precipitation capacity is the thick product of scandium, has reached the purpose of carrying scandium, and rate of recovery height.
In order to obtain scandium product of high grade, can adopt repeating step to reach higher purity, final available SC
2O
3, grade is 99.85% final scandium product.
The invention has the beneficial effects as follows:
1, exploitation river course silt sand can be turned waste into wealth, and saves mineral resources, meets the national industrial policies of sustainable development.
2, to put forward the scandium resource abundant, unrestricted, widely distributed for river course silt sand, the cost cheapness, and scandium product price is low, can occupy tangible competitive advantage in market.
3, silt sand in river course is carried scandium and can not destroyed ecological environment, helps environmental protection, carry scandium after silt sand more clean, be used for building industry and help improving concrete quality, very favourable to engineering construction.
4, economic benefit is obvious, to produce the SC of 1Kg
2O
3Meter, purity is 99.99% SC
2O
3, state's tax-included price is 30,000 yuan/Kg, and American market is 2500 dollars/Kg, and the purity that the present invention produces is 99.85% SC
2O
3Price can 20,000 yuan //Kg, calculate the recyclable SC of silt sand per ton by technical indicator of the present invention
2O
3Amount be 4.06 the gram, the silt sand output value then per ton can reach 81 yuan.
Description of drawings
Fig. 1 is the present invention extracts the scandium concentrate from river course silt sand a process chart;
Fig. 2 is the process chart that extracts scandium from the scandium concentrate.
Specific embodiments
Adopt Chongqing, the Changjiang river section river course silt sand, sampling 60t has removed cobble, maximum particle size＜2mm;
1. from silt sand, select the scandium concentrate
Be 80 purpose vibratory sieve classifications with sieve aperture earlier, again with spiral concentrator and spiral chute gravity treatment+80 orders and-80 purpose silt sand respectively, wherein on the sieve+80 purpose silt sand enter spiral concentrator ,-80 purpose silt sand enter spiral chute under the sieve, 37.5% the mine tailing of skimming.To contain the scandium product in order improving, to guarantee monomer dissociation, gravity concentrate is merged into the closed cycle into ball milling and spiral classifier formation, and the control granularity is 200 orders, sends into the low intensity magnetic separation machine, and magnetic product is an iron ore concentrate.Nonmagnetic portion is through high-gradient magnetic separation, 50.81% the mine tailing of can skimming, and concentrate is through hydroclone classification, and the control granularity is 400 orders, and 400 orders enter table concentration.Gravity tailings discards, and the chats Returning process enters electric separation behind the concentrate drying.Electrostatic separation tailing is incorporated the shaking table chats into, and concentrate then is the scandium concentrate.The concentrate index is a productive rate 4.26%, grade 96.23g/t, the rate of recovery 61.33%.Used equipment and producer, optimal processing parameter such as table 4 in each step:
Table 4
Because the solubility of scandium salts, therefore, the present invention's second link is extracted scandium by hydrometallurgy exactly from the scandium concentrate.
| Job title | The specification of equipment model | Factory | Technological parameter |
| Classification for the first time | Self-fixed centre shale shaker 600 * 1200mm | Liuzhou mining machine factory | Feed preparation unit size＜2mm screen size 0.18mm |
| Gravity treatment | Spiral concentrator Φ 600mm | West Lu's fiberglass Development Co., Ltd | Mine-supplying quantity 1.1t/h, feed ore concentration 15%, flushing water 3 give birth to/minute |
| Spiral chute Φ 600mm | West Lu's fiberglass Development Co., Ltd | Mine-supplying quantity 1.1t/h, feed ore concentration 9%, flushing water 2 give birth to/minute | |
| Ore grinding | Ball mill Φ 400 * 500mm | Behaviour ore deposit, Hengyang machinery plant | Hold ball rate 45.5%, ball load 120Kg, sphere diameter proportioning: Φ 50 11.74%, Φ 35 30.69%, Φ 25 34.08%, Φ 15 23.49%, mine-supplying quantity 120Kg/h. ore milling concentration 60%, 75 rev/mins of mill speeds |
| Classification for the second time | Single-spiral classifier Φ 150 * 1200mm | Behaviour ore deposit, Hengyang machinery plant | Partition size 74 μ m, graded concentration 10% |
| Low intensity magnetic separation | Drum-type magnetic separator XCG5-74 type Φ 400 | Tianjin mining machinery plant | Magnetic field intensity 120KA/m, feed ore concentration 25% dispels, rinsing water yield 3000ml/ branch |
| High gradient magnetic separator | High gradient magnetic separator Φ 850mm | Self-control | Magnetic matrix cooperates exciting curent 400A, the rinsing water yield 5000～6000ml/ branch for the magnetic stainless steel expanded metals adopts the 1# coarse net with the 3# fine-structure mesh |
| Classification for the third time | Hydrocyclone Φ 250mm | Cloud tin machinery plant | Partition size 37 μ m, graded concentration 14% is given ore deposit pressure 70KPa |
| Shaking table | Ion waveform shaking table | Self-control | Stroke (mm) jig frequency (inferior)+37 μ m 12 420-37 μ m 10 460 |
| Dry | Drying box 101 types | Shanghai | |
| Electric separation | 120,000 volts of High Voltage Suspension electrostatic separators | Self-control | + 37 μ m-37 μ m voltages, (KV) 85 80 corona electrodes, (root) 34 arc earth electrodes are long, (mm) 700 800 flashboard positions 10 15 |
2. from the scandium concentrate, extract scandium
(1), the leaching of scandium
Get 30000g and be finely ground to-320 purpose scandium concentrate, add hydrochloric acid in the titanium reactor, concentration is 22.8%, and liquid-solid ratio is 2.5: 1, adds 7
#Cosolvent 45g/t, 90 ℃ of extraction temperatures stirred 9 hours, and what can get grade and be 13.5g/t contains the scandium immersion liquid, and its leaching rate is 80.28%, and leaching equipment titanium reactor is produced by Baoji Nonferrous Metal Processing Plant.
(2), extraction stoste produces
A large amount of ferric ions have influenced the grade of scandium in the immersion liquid, for deironing, get immersion liquid 200ml and are heated to 90 ℃, add Na
2SO
48g stirred 20 minutes, added NaClO again
33.5g continue to stir 20 minutes, use Na then
2CO
3Adjust PH=2.3, at this moment solution is salmon pink, constantly stirs about 3 hours, leaves standstill back filtration about 1 hour, and filtrate is stoste; It contains the scandium grade and rises to 17g/t by 13.5g/t; Filter residue is a siderotil, can be used as accessory substance.
(3), the extraction of scandium
Get stoste 1000ml, adjust PH=1.26, add 52ml tbp and 3.5ml kerosene, stirred 3 minutes, and left standstill and abandoned water in 20 minutes, wash 3 times, the each stirring 3 minutes, leave standstill and abandoned water in 20 minutes, then carry out secondary and strip, add 5% hydrochloric acid 46ml at every turn, vibrated 1～2 minute, left standstill 30 minutes, and told extract, this moment, total extraction yield was 90.27%; 4 groups of extraction equipments, the extraction tank self-control.
(4), the phase inversion of scandium
The oxalic acid that adds extraction liquid measure 12% stirs in extract, adjusts PH=4.5 with NaOH, leaves standstill filtration, and filter residue is the head product of scandium, and it is 87.27% that head product contains scandium, and the phase inversion rate of recovery is 90.47%, and phase inversion equipment titanium bucket is produced by Baoji titanium factory.
(5), the purification of scandium
Adopt above-mentioned steps (1), (2), (3) and (4) to handle head product once more, again filter residue is put into cabinet-type electric furnace and carried out the high temperature ashing, temperature is controlled at below 1000 ℃, when product is white powder, promptly get purity and be 99.85% scandium oxide, high temperature incineration equipment cabinet-type electric furnace is produced by Baoji titanium factory.
(6), metal scandium produces
Be 87.27% thick scandium with step (5) gained purity with the reduction of vacuum metallurgy equipment, can make purity is 97.38% metal scandium, the self-control of vacuum metallurgy equipment.
Handling 60t silt sand by the present invention, finally can to get purity be 99.85% SC
2O
3For:
60t×6.6g/t×61.33％×80.28％×90.27％×90.47％×1.53＝243.6g
In the formula: 60t is a silt sand amount;
6.6g/t for silt sand contains the scandium grade;
61.33% is the scandium concentrate rate of recovery;
80.28% is the leaching rate of scandium;
90.27% is total extraction yield of scandium;
90.47% is the rate of recovery of scandium phase inversion;
1.53 be SC
2O
3/ Sc
2Conversion coefficient.
Claims (1)
1, a kind of method for extracting scandium of river course silt sand is characterized in that the cut-off footpath is a raw material less than 2mm silt sand, carries out as follows:
(1). from silt sand, select the scandium concentrate
Be 80 purpose vibratory sieve classifications with sieve aperture earlier, with spiral concentrator and spiral chute difference gravity treatment+80 orders and-80 purpose silt sand, the gained gravity concentrate is merged into the closed cycle into ball milling and spiral classifier formation again, and the control granularity is 200 orders, send into the low intensity magnetic separation machine, magnetic product is an iron ore concentrate; Nonmagnetic portion is through high-gradient magnetic separation, and the gained concentrate is through hydroclone classification, and the control granularity is 400 orders, and 400 orders enter table concentration; Gravity tailings discards, and the chats Returning process enters electric separation behind the concentrate drying; Electrostatic separation tailing is incorporated the shaking table chats into, and concentrate then is the scandium concentrate;
(2), from the scandium concentrate, extract scandium
(A), the leaching of scandium
Be finely ground to-320 purpose scandium concentrate, add hydrochloric acid in the titanium reactor, concentration is 22.8%, and liquid-solid ratio is 2.5: 1, adds 7
#Cosolvent 30～50g/t, 88 ℃～95 ℃ of extraction temperatures stirred 8.5～10.5 hours;
(B), extraction stoste produces
Get immersion liquid 200ml and be heated to 90 ℃, add Na
2SO
49～12g stirred 20 minutes, added NaClO again
34～5.5g continues to stir 20 minutes, uses Na then
2CO
3Adjust PH=2.3, at this moment solution is salmon pink, constantly stirs about 2～3 hours, leaves standstill back filtration about 1 hour, and filtrate is the used stoste of extraction;
(C), the extraction of scandium
Get stoste 1000ml, adjust PH=1.26, add 48～50ml tbp and 3～5ml kerosene, stirred 3 minutes, leave standstill and abandoned water in 20 minutes, wash 2～4 times, stirred 3 minutes at every turn, leave standstill and abandoned water in 20 minutes, then carry out secondary and strip, add hydrochloric acid 42～56ml of 5% at every turn, vibrated 1～2 minute, left standstill 30 minutes, and told extract;
(D), the phase inversion of scandium
The oxalic acid that adds extraction liquid measure 10～18% stirs in extract, adjusts PH=4.5 with NaOH, leaves standstill filtration, and filter residue is the head product of scandium;
(E), the purification of scandium
Adopt above-mentioned steps (A), (B), (C) once more and (D) handle head product, filter residue is put into cabinet-type electric furnace again and carried out the high temperature ashing, temperature is controlled at below 1000 ℃, when product is white powder, promptly gets scandium oxide;
(F), metal scandium produces
With step (E) gained purity be 87.27% thick scandium with the reduction of vacuum metallurgy equipment, can make metal scandium.
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|---|---|---|---|
| CNB031353541A CN1181925C (en) | 2003-07-03 | 2003-07-03 | Scandium extraction method of river channel sedimentation |
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|---|---|---|---|
| CNB031353541A CN1181925C (en) | 2003-07-03 | 2003-07-03 | Scandium extraction method of river channel sedimentation |
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| CN1181925C true CN1181925C (en) | 2004-12-29 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100370040C (en) * | 2006-03-17 | 2008-02-20 | 汪友华 | Method for extracting scandium from red mud |
| CN101543803B (en) * | 2008-12-31 | 2013-07-17 | 赵金光 | Sand-washing method and sand-washing equipment |
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| CN101797531B (en) * | 2010-03-23 | 2012-11-14 | 云南锡业集团（控股）有限责任公司 | Method for recovering valuable metal mineral in zinc tailing |
| CN102021343A (en) * | 2010-10-13 | 2011-04-20 | 赣州鑫磊稀土新材料有限公司 | Method for separating and recovering scandium oxide from aluminum-scandium alloy smelting waste |
| CN102886310B (en) * | 2012-10-19 | 2013-08-14 | 内蒙古科技大学 | Method for separating scandium concentrate from bayan obo tailings |
| CN102886305B (en) * | 2012-10-19 | 2015-11-25 | 内蒙古科技大学 | A kind of Bayan Obo mine tailing selects scandium method |
| CN102925668B (en) * | 2012-11-20 | 2014-04-30 | 湖南稀土金属材料研究院 | Method for leaching out scandium from niobium tailing dressing |
| AU2016200868B2 (en) | 2015-02-10 | 2021-05-13 | Scandium International Mining Corporation | Systems and processes for recovering scandium values from laterite ores |
| CN105312148B (en) * | 2015-12-10 | 2018-05-25 | 中国地质科学院矿产综合利用研究所 | Beneficiation and enrichment method suitable for associated scheelite in molybdenite flotation tailings |
| CN113894034B (en) * | 2021-09-13 | 2022-09-13 | 长沙矿冶研究院有限责任公司 | Purification method of quartz sand raw material |
| CN113941441A (en) * | 2021-10-14 | 2022-01-18 | 中钢集团马鞍山矿山研究总院股份有限公司 | Wet-type strong magnetic preselection method for low-grade chromite |
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2003
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100370040C (en) * | 2006-03-17 | 2008-02-20 | 汪友华 | Method for extracting scandium from red mud |
| CN101543803B (en) * | 2008-12-31 | 2013-07-17 | 赵金光 | Sand-washing method and sand-washing equipment |
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|---|---|
| CN1478600A (en) | 2004-03-03 |
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Granted publication date: 20041229 Termination date: 20170703 |