CN103706465B - Method for selecting preconcentration vanadium from high-calcium type stone coal in flotation mode - Google Patents
Method for selecting preconcentration vanadium from high-calcium type stone coal in flotation mode Download PDFInfo
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Abstract
The invention relates to a method for selecting preconcentration vanadium from high-calcium type stone coal in a flotation mode. According to the technical scheme, high-calcium type stone coal raw ore is smashed till the grain size is smaller than 25mm, the smashed high-calcium type stone coal raw ore is decarbonized and roasted for 1 hour to 2 hours at the temperature ranging from 600 DEG C to 750 DEG C, the decarbonized and roasted high-calcium type stone coal raw ore is ground till the part, with the grain size smaller than 0.074mm, of the high-calcium type stone coal raw ore accounts for 60-80wt% of the high-calcium type stone coal raw ore, and the ground high-calcium type stone coal raw ore is classified through a hydrocyclone. Calcium roughing is conducted on the classified coarse-fraction product, calcium scavenging is then conducted on the gangue after calcium roughing, vanadium roughing is conducted on the gangue after calcium scavenging, vanadium scavenging is conducted on the gangue after vanadium roughing, and flotation is adopted for all the mineral separation processes through floatation cells. The concentrate generated after calcium roughing, the concentrate generated after calcium scavenging and the gangue generated after vanadium scavenging are combined to form the final gangue, and classified fine-fraction product, the concentrate generated after calcium roughing, the concentrate generated after calcium scavenging and the concentrate generated after vanadium scavenging are combined to form the final concentrate. The method has the advantages of being reasonable in process, good in scavenging effect, small in amount of consumed collecting agents, high in concentrate grade, small in amount of consumed acid pH regulators, and capable of remarkably reducing follow-up chemical vanadium extraction cost.
Description
Technical field
The invention belongs to flotation preenrichment vanadium technical field.Be specifically related to a kind of method of flotation preenrichment vanadium from high-calcium type bone coal.
Background technology
Bone coal is the distinctive a kind of navajoite resource of China, wherein V
2o
5reserves are 1.18 × 10
8t is V in vanadium titano-magnetite
2o
56.7 times of reserves, account for 87% of China's vanadium resource total amount, extract an important directions of Fan Shi China vanadium resource exploitation from bone coal.Because the vanadium in China's bone coal mainly replaces the Al(III of alumina octahedral in mica mineral with isomorphous form) and exist, vanadium extraction difficulty is comparatively large, and the technique of current extracting vanadium from stone coal generally comprises the operations such as decarburization preroast, roasting, water logging/acidleach, ion cleaning, precipitation and calcining.Due to the V in bone coal
2o
5grade is low, and the overwhelming majority is between 0.13 ~ 1.2%, and in vanadium extracting process, pan feeding grade is low, treating capacity is large; In bone coal, the consumption such as calcite amount of acidic substances is high in addition, causes acid consumption cost to increase; The problem that in extracting vanadium from stone coal process, production cost is high highlights.Therefore, before chemical vanadium extraction, carry out ore dressing preenrichment, to improve the V in bone coal
2o
5grade is very necessary.
" research of high-carbon bone coal preferred coal separation Vanadium Concentrationin new technology " (Wu Huiling, Zhao Wei, Deng. China rare earth journal, 2008,26:530 ~ 533.) result show, due to the existence of fine-grained carbon mud, cover cap, at other mineral surfaces, affects the selective absorption of collecting agent at each mineral surfaces, causes flotation conditions to worsen, flotation effect can not be embodied, and is difficult to the floatation process of routine the separation realizing carbon, vanadium and other gangue mineral." a kind of beneficiation method from high-calcium type navajoite enrichment vanadic anhydride " (CN102274795A) carrys out the method for flotation calcium by thick two single-minded techniques of sweeping, indirect enrichment vanadium, the method only relies on jettisoning calcium mineral that vanadium grade in concentrate is increased, and the flotation directly do not carried out containing vanadium mineral, flotation concentrate vanadium grade is not high.The vanadium mineral that contains in bone coal is generally mica mineral, and gangue mineral is quartz, calcite and feldspar etc. mainly.Carry out mica with amine collector and quartz, feldspar FLOTATION SEPARATION need carry out under pH value is the acid condition of 2 ~ 3 (Wei Yunfeng. five the sericite ore dressing amine in Shanxi Province research [J]. North China land resources, 2007, (2): 37-38.), under this condition, pH adjusting agent can be reacted with the calcium mineral calcite in bone coal, causes consuming a large amount of pH adjusting agents.In addition, in the bone coal ore pulp high to calcic, add a large amount of acid mediums, can produce a large amount of bubble, easily cause " race groove " phenomenon, it is large that operation controls difficulty.
Summary of the invention
The present invention is intended to overcome prior art defect, object be to provide a kind of process structure rationally, good separation effect, collector dosage are few, concentrate grade is high, acid pH adjusting agent consumption is little and significantly can reduce the method for flotation preenrichment vanadium from high-calcium type bone coal of subsequent chemistry vanadium extraction cost.
For achieving the above object, the concrete steps of the technical solution used in the present invention are:
1) broken: high-calcium type bone coal crushing raw ore is less than 25mm to particle diameter.
2) decarburization roasting: the high-calcium type bone coal after fragmentation is placed in roaster, decarburization roasting 1 ~ 2h under 600 ~ 750 DEG C of conditions.
3) ore grinding: what the high-calcium type bone coal after decarburization roasting is milled to particle diameter is less than 0.074mm accounts for 60 ~ 80wt%.
4) classification: carry out classification to the high-calcium type bone coal after ore grinding with hydrocyclone, obtain particle diameter and be greater than the fine fraction product that the coarse fraction product of 0.020mm and particle diameter be less than 0.020mm, the fine fraction product that particle diameter is less than 0.020mm is final concentrate.
5) calcium is roughly selected and is scanned with calcium: coarse fraction product particle diameter being greater than 0.020mm adopts flotation cell to carry out calcium and roughly select, calcium roughly select after mine tailing adopt flotation grain to carry out calcium again to scan; The fatty acid collecting agent consumption that calcium roughly selects middle employing is 500 ~ 1000g/t, and the fatty acid collecting agent consumption that calcium scans middle employing is 200 ~ 500g/t; Calcium adds waterglass as inhibitor in roughly selecting, and waterglass consumption is 100 ~ 200g/t.
6) vanadium is roughly selected and is scanned with vanadium: mine tailing after being scanned by calcium adopts flotation cell to carry out vanadium and roughly selects, vanadium roughly select after mine tailing adopt flotation cell to carry out vanadium again to scan; The amine collector consumption that vanadium roughly selects middle employing is 50 ~ 200g/t, and the amine collector consumption that vanadium scans middle employing is 30 ~ 100g/t; Vanadium is roughly selected the pH value of scanning middle ore pulp with vanadium and is all controlled to be 2 ~ 3; Vanadium adds prodan as inhibitor in roughly selecting, and prodan consumption is 50 ~ 150g/t.
As true tailings together with the concentrate that concentrate, calcium that calcium is roughly selected are scanned merges with the mine tailing that vanadium is scanned; As final concentrate together with the concentrate that vanadium is roughly selected merges with the concentrate that vanadium is scanned; Vanadium is roughly selected to scan in process with vanadium and is all adopted amine collector.
V in described high-calcium type bone coal
2o
5grade is 0.5 ~ 1.0%, CaO content is 4 ~ 15wt%.
The carbon-drop rate of described decarburization roasting is 75 ~ 95%.
Described fatty acid collecting agent is the one in oleic acid, enuatrol, tall oil, oxidized paraffin wax soap.
Described amine collector is the one in lauryl amine, lauryl amine acetate, dodecylamine hydrochloride, ether amine.
Owing to adopting technique scheme, the present invention compared with prior art has following good effect:
1) significantly can reduce the Preferential adsorption of carbonaceous to flotation collector by decarburization roasting, reduce collector dosage.
2) solve the problem of carbonaceous cover cap at each mineral surfaces, collecting agent can be shown due selective to different minerals, separating effect is enhanced.
3) decarburization roasting process can realize the oxidation of vanadium in bone coal and turn valency, and the concentrate after preenrichment can directly leach, and process structure is reasonable; In addition, the heat that in decarburization roasting process, carbon burning produces can be used for the leaching operation of chemical vanadium extraction, and the scaling loss of carbon also can Vanadium Concentrationin to a certain extent simultaneously.
4) the fine fraction part high containing vanadium can be separated by classification operation on the one hand, on the other hand follow-up flotation circuit is also played to the effect of desliming; Calcium is roughly selected and is scanned by the calcic calcite jettisoning in high-calcium type bone coal, not only can improve the grade that vanadium roughly selects vanadium in pan feeding, and vanadium can be avoided to roughly select the reaction of acid pH adjusting agent and calcite with calcium, significantly reduces the consumption of acid pH adjusting agent.Zero point due to muscovite is less than the zero point of quartz and feldspar, be under the acid condition of 2 ~ 3 in pH value, muscovite particle surface bear point, quartz and feldspar particle surface lotus are on schedule, amine cation-collecting agent is adopted to carry out under this condition containing vanadium muscovite good with the separation selectivity of quartz, feldspar, simultaneously using prodan as inhibitor that is quartzy and feldspar, separating effect can be strengthened further;
5) concentrate obtained by flotation preenrichment, as the pan feeding of chemical vanadium extraction, obviously can reduce the treating capacity of chemical vanadium extraction, and reduces the content of the sour mineral of consumption such as calcite in pan feeding, reduces the acid consumption leached, significantly can reduce subsequent chemistry vanadium extraction cost.
Therefore, the present invention has rational technology, good separation effect, collector dosage is few, concentrate grade is high, acid pH adjusting agent consumption is little, significantly can reduce the feature of subsequent chemistry vanadium extraction cost.
Accompanying drawing explanation
Fig. 1 is a kind of process chart of the present invention.
Detailed description of the invention
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with the drawings and specific embodiments, but content of the present invention is not only confined to the following examples.
Now by the fatty acid collecting agent described in detailed description of the invention and amine collector Unify legislation as follows, repeat no more in embodiment:
Fatty acid collecting agent is the one in oleic acid, enuatrol, tall oil, oxidized paraffin wax soap.
Amine collector is the one in lauryl amine, lauryl amine acetate, dodecylamine hydrochloride, ether amine.
Embodiment 1
A kind of method of flotation preenrichment vanadium from high-calcium type bone coal.With the high-calcium type bone coal in somewhere, the method process Hubei, V in described high-calcium type bone coal
2o
5grade is 0.5 ~ 0.75%, CaO content is 7 ~ 15wt%.
The concrete steps of the present embodiment are as shown in Figure 1:
1) broken: high-calcium type bone coal crushing raw ore is less than 25mm to particle diameter.
2) decarburization roasting: the high-calcium type bone coal after fragmentation is placed in roaster, decarburization roasting 1 ~ 1.5h under 600 ~ 700 DEG C of conditions, carbon-drop rate is 75 ~ 80%.
3) ore grinding: what the high-calcium type bone coal after decarburization roasting is milled to particle diameter is less than 0.074mm accounts for 60 ~ 70wt%.
4) classification: carry out classification to the high-calcium type bone coal after ore grinding with hydrocyclone, obtain particle diameter and be greater than the fine fraction product that the coarse fraction product of 0.020mm and particle diameter be less than 0.020mm, the fine fraction product that particle diameter is less than 0.020mm is final concentrate.
5) calcium is roughly selected and is scanned with calcium: coarse fraction product particle diameter being greater than 0.020mm adopts flotation cell to carry out calcium and roughly select, calcium roughly select after mine tailing adopt flotation grain to carry out calcium again to scan; The fatty acid collecting agent consumption that calcium roughly selects middle employing is 500 ~ 750g/t, and the fatty acid collecting agent consumption that calcium scans middle employing is 200 ~ 350g/t; Calcium adds waterglass as inhibitor in roughly selecting, and waterglass consumption is 100 ~ 150g/t.
6) vanadium is roughly selected and is scanned with vanadium: mine tailing after being scanned by calcium adopts flotation cell to carry out vanadium and roughly selects, vanadium roughly select after mine tailing adopt flotation cell to carry out vanadium again to scan; The amine collector consumption that vanadium roughly selects middle employing is 50 ~ 120g/t, and the amine collector consumption that vanadium scans middle employing is 30 ~ 70g/t; Vanadium is roughly selected the pH value of scanning middle ore pulp with vanadium and is all controlled to be 2 ~ 2.5; Vanadium adds prodan as inhibitor in roughly selecting, and prodan consumption is 50 ~ 100g/t.
As true tailings together with the concentrate that concentrate, calcium that calcium is roughly selected are scanned merges with the mine tailing that vanadium is scanned; As final concentrate together with the concentrate that vanadium is roughly selected merges with the concentrate that vanadium is scanned; Vanadium is roughly selected to scan in process with vanadium and is all adopted amine collector.The index of concrete flotation preenrichment vanadium is in table 1.
Somewhere, table 1 Hubei high-calcium type bone coal flotation preenrichment vanadium index
Embodiment 2
A kind of method of flotation preenrichment vanadium from high-calcium type bone coal.With the high-calcium type bone coal vanadium of the method process Certain District, Hunan, described high-calcium type bone coal V
2o
5grade is 0.75 ~ 1.0%, CaO content is 4 ~ 7wt%.
The concrete steps of the present embodiment are as shown in Figure 1:
1) broken: high-calcium type bone coal crushing raw ore is less than 25mm to particle diameter;
2) decarburization roasting: the high-calcium type bone coal after fragmentation is placed in roaster, decarburization roasting 1.5 ~ 2h under 700 ~ 750 DEG C of conditions, carbon-drop rate is 80 ~ 95%.
3) ore grinding: what the high-calcium type bone coal after decarburization roasting is milled to particle diameter is less than 0.074mm accounts for 70 ~ 80wt%.
4) classification: carry out classification to the high-calcium type bone coal after ore grinding with hydrocyclone, obtain particle diameter and be greater than the fine fraction product that the coarse fraction product of 0.020mm and particle diameter be less than 0.020mm, the fine fraction product that particle diameter is less than 0.020mm is final concentrate.
5) calcium is roughly selected and is scanned with calcium: coarse fraction product particle diameter being greater than 0.020mm adopts flotation cell to carry out calcium and roughly select, calcium roughly select after mine tailing adopt flotation grain to carry out calcium again to scan; The fatty acid collecting agent consumption that calcium roughly selects middle employing is 750 ~ 1000g/t, and the fatty acid collecting agent consumption that calcium scans middle employing is 350 ~ 500g/t; Calcium adds waterglass as inhibitor in roughly selecting, and waterglass consumption is 150 ~ 200g/t.
6) vanadium is roughly selected and is scanned with vanadium: mine tailing after being scanned by calcium adopts flotation cell to carry out vanadium and roughly selects, vanadium roughly select after mine tailing adopt flotation cell to carry out vanadium again to scan; The amine collector consumption that vanadium roughly selects middle employing is 120 ~ 200g/t, and the amine collector consumption that vanadium scans middle employing is 70 ~ 100g/t; Vanadium is roughly selected the pH value of scanning middle ore pulp with vanadium and is all controlled to be 2.5 ~ 3; Vanadium adds prodan as inhibitor in roughly selecting, and prodan consumption is 100 ~ 150g/t.
As true tailings together with the concentrate that concentrate, calcium that calcium is roughly selected are scanned merges with the mine tailing that vanadium is scanned; As final concentrate together with the concentrate that vanadium is roughly selected merges with the concentrate that vanadium is scanned; Vanadium is roughly selected to scan in process with vanadium and is all adopted amine collector.The index of concrete flotation preenrichment vanadium is in table 2.
Table 2 Certain District, Hunan high-calcium type bone coal flotation preenrichment vanadium index
This detailed description of the invention describes technical scheme of the present invention and essential implementation in detail; not that protection scope of the present invention is limited; all any simple modification of doing according to Spirit Essence of the present invention and equivalent structure transformation or modification, all should be encompassed within protection scope of the present invention.
This detailed description of the invention arranged the benefit that decarburization calcining process has following several respects before ore grinding:
1) significantly can reduce the Preferential adsorption of carbonaceous to flotation collector by decarburization roasting, reduce collector dosage.
2) solve the problem of carbonaceous cover cap at each mineral surfaces, collecting agent can be shown due selective to different minerals, separating effect is enhanced.
3) decarburization roasting process can realize the oxidation of vanadium in bone coal and turn valency, and the concentrate after preenrichment can directly leach, and process structure is reasonable; In addition, the heat that in decarburization roasting process, carbon burning produces can be used for the leaching operation of chemical vanadium extraction, and the scaling loss of carbon also can Vanadium Concentrationin to a certain extent simultaneously.
4) the fine fraction part high containing vanadium can be separated by classification operation on the one hand, on the other hand follow-up flotation circuit is also played to the effect of desliming; Calcium roughly selects that scan with calcium can by the calcic calcite jettisoning in high-calcium type bone coal, not only can roughly select the grade of vanadium in pan feeding by vanadium, and vanadium can be avoided to roughly select the reaction of acid pH adjusting agent and calcite, can greatly reduce the consumption of acid pH adjusting agent; Zero point due to muscovite is less than the zero point of quartz and feldspar, be under the acid condition of 2 ~ 3 in pH value, muscovite particle surface bear point, quartz and feldspar particle surface lotus are on schedule, amine cation-collecting agent is adopted to carry out under this condition containing vanadium muscovite good with the separation selectivity of quartz, feldspar, simultaneously using prodan as inhibitor that is quartzy and feldspar, separating effect can be strengthened further.
5) concentrate obtained by flotation preenrichment, as the pan feeding of chemical vanadium extraction, can greatly reduce the treating capacity of chemical vanadium extraction, and reduces the content of the sour mineral of consumption such as calcite in pan feeding, reduces the acid consumption leached, significantly can reduce subsequent chemistry vanadium extraction cost.
Therefore this detailed description of the invention compared with the prior art, there is rational technology, good separation effect, collector dosage is few, concentrate grade is high, acid pH adjusting agent consumption is little and significantly can reduces the feature of subsequent chemistry vanadium extraction cost.
Claims (5)
1. the method for flotation preenrichment vanadium from high-calcium type bone coal, is characterized in that the concrete steps of the method are:
1) broken: high-calcium type bone coal crushing raw ore is less than 25mm to particle diameter;
2) decarburization roasting: the high-calcium type bone coal after fragmentation is placed in roaster, decarburization roasting 1 ~ 2h under 600 ~ 750 DEG C of conditions;
3) ore grinding: what the high-calcium type bone coal after decarburization roasting is milled to particle diameter is less than 0.074mm accounts for 60 ~ 80wt%;
4) classification: classification is carried out to the high-calcium type bone coal after ore grinding with hydrocyclone, obtain particle diameter and be greater than the fine fraction product that the coarse fraction product of 0.020mm and particle diameter be less than 0.020mm, the fine fraction product that particle diameter is less than 0.020mm is final concentrate;
5) calcium is roughly selected and is scanned with calcium: coarse fraction product particle diameter being greater than 0.020mm adopts flotation cell to carry out calcium and roughly select, calcium roughly select after mine tailing adopt flotation grain to carry out calcium again to scan; The fatty acid collecting agent consumption that calcium roughly selects middle employing is 500 ~ 1000g/t, and the fatty acid collecting agent consumption that calcium scans middle employing is 200 ~ 500g/t; Calcium adds waterglass as inhibitor in roughly selecting, and waterglass consumption is 100 ~ 200g/t;
6) vanadium is roughly selected and is scanned with vanadium: mine tailing after being scanned by calcium adopts flotation cell to carry out vanadium and roughly selects, vanadium roughly select after mine tailing adopt flotation cell to carry out vanadium again to scan; The amine collector consumption that vanadium roughly selects middle employing is 50 ~ 200g/t, and the amine collector consumption that vanadium scans middle employing is 30 ~ 100g/t; Vanadium is roughly selected the pH value of scanning middle ore pulp with vanadium and is all controlled to be 2 ~ 3; Vanadium adds prodan as inhibitor in roughly selecting, and prodan consumption is 50 ~ 150g/t;
As true tailings together with the concentrate that concentrate, calcium that calcium is roughly selected are scanned merges with the mine tailing that vanadium is scanned; As final concentrate together with the concentrate that vanadium is roughly selected merges with the concentrate that vanadium is scanned; Vanadium is roughly selected to scan in process with vanadium and is all adopted amine collector.
2. the method for flotation preenrichment vanadium from high-calcium type bone coal according to claim 1, is characterized in that V in described high-calcium type bone coal
2o
5grade is 0.5 ~ 1.0%, CaO content is 4 ~ 15wt%.
3. the method for flotation preenrichment vanadium from high-calcium type bone coal according to claim 1, is characterized in that the carbon-drop rate of described decarburization roasting is 75 ~ 95%.
4. the method for flotation preenrichment vanadium from high-calcium type bone coal according to claim 1, is characterized in that described fatty acid collecting agent is the one in oleic acid, enuatrol, tall oil, oxidized paraffin wax soap.
5. the method for flotation preenrichment vanadium from high-calcium type bone coal according to claim 1, is characterized in that described amine collector is the one in lauryl amine, lauryl amine acetate, dodecylamine hydrochloride, ether amine.
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| CN104060108B (en) * | 2014-06-10 | 2016-10-05 | 中南大学 | A kind of method extracting vanadium from high calcium siliceous shale containing vanadium |
| CN104437833B (en) * | 2014-11-07 | 2017-11-24 | 贵州省贵金属矿产资源综合利用工程技术研究中心有限公司 | A kind of method of physical upgrading enrichment carbonaceous shale type navajoite |
| CN105032598A (en) * | 2015-05-29 | 2015-11-11 | 武汉理工大学 | Method for floatation of preconcentration vanadium from high-calcium mica type vanadium-bearing stone coal |
| CN104907163A (en) * | 2015-07-07 | 2015-09-16 | 湖南有色金属研究院 | Mineral separation method of finely disseminated vanadium contained carbonaceous shale |
| CN106944243B (en) * | 2016-12-27 | 2020-02-18 | 核工业北京化工冶金研究院 | Pretreatment method of argillaceous uranium ore |
| WO2021146797A1 (en) * | 2020-01-20 | 2021-07-29 | First Vanadium Corp. | Vanadium extraction from disparate shale ores |
| CN115178363B (en) * | 2022-07-08 | 2024-03-01 | 中南大学 | Ultra-high purity quartz powder prepared from mudstone-containing quartz rock and comprehensive utilization process |
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