CN107913802B - A method of from selecting flotation recovery fluorite in tin tailings - Google Patents
A method of from selecting flotation recovery fluorite in tin tailings Download PDFInfo
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- CN107913802B CN107913802B CN201710948847.6A CN201710948847A CN107913802B CN 107913802 B CN107913802 B CN 107913802B CN 201710948847 A CN201710948847 A CN 201710948847A CN 107913802 B CN107913802 B CN 107913802B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/02—Froth-flotation processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/002—Inorganic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/008—Organic compounds containing oxygen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/007—Modifying reagents for adjusting pH or conductivity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/06—Depressants
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- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention discloses a kind of from the method for selecting flotation recovery fluorite in tin tailings, and this method is will to select tin tailings after ore grinding, is sized mixing using sodium carbonate, and using waterglass as inhibitor, kerosene and oleic acid carry out roughing as collecting agent；It is selected to get fluorite concentrate by least 6 times using calgon as inhibitor after rougher concentration regrinding.This method simple process, it is easy to operate, it realizes and selects in tin tailings with the FLOTATION SEPARATION of quartz gangue and fluorite as main component, it is low to solve fluorite Beneficiation Feed Grade, impurity content is high, the problem of poor selectivity, this method are applicable not only to the low-grade fluorite FLOTATION SEPARATION using quartz as main gangue, are also applied for the low-grade fluorite FLOTATION SEPARATION with quartz for main gangue association multi-metal sulfide.
Description
Technical field
It is the present invention relates to a kind of beneficiation method of low-grade fluorite, in particular to a kind of that high-grade is recycled in tailing from selecting
The method of fluorite belongs to mineral resources reutilization technology field.
Background technique
Fluorite is strategic mineral, and for domestic every profession and trade to the demand of fluorite up to 5,200,000 tons, this is much higher than current China
4200000 tons of fluorite production capacity, practical Service Efficiency are only 80%, and wherein chemical grade fluorite fine powder Service Efficiency is less than 70%.By
In the reason of the technology and market, past to select factory by fluorite grade lower than 15%, even lower than 25% fluorite ore is considered as tailing
The accumulation of discharge, these tailings needs a large amount of Tailings Dam, not only occupies a large amount of soil, also causes the waste of available resources.
With Yunnan, Guizhou province, further include South Sichuan fluorite ore for, these fluorite ores largely belong to fluorite with
Cassiterite, lead zinc sulfide association type, fluorite grade is 7%~8%, and reserves are at 8,000,000 tons or so, the fluorite in these areas
Mine is stored mostly in the form of tailing.It is effectively comprehensively utilized to improve resource, protects mine environment, past tailing is opened
Hair is to significant the needs of meeting China's fluorite resource.
The beneficiation method of fluorite mainly has picking, gravity treatment, a flotation, and fluorite usually with some other mineral intergrowth, such as carbon
Hydrochlorate, silicate etc., the density difference between this kind of gangue mineral and fluorite is smaller, while with the dilution of fluorite and and gangue
Close relation is inlayed between mineral, only fine grinding can be only achieved monomer dissociation, and the separation of this kind of fluorite and gangue can only take flotation
Method.For different types of fluorite ore, existing floatation is divided into following three classes: quartz type fluorite flotation, calcite type firefly
Stone ore flotation, barite type fluorite flotation.
Domestic ore dressing worker has carried out a large amount of research to processing of fluorspar ores for many years, and achieve more research at
Fruit has been gained most valuable experience for processing of fluorspar ores, but still has no that recycling fluorite grade is special lower than 10% from tailing at present
Benefit or document, low product complicated difficult select the drop silicon of fluorite ore to drop calcium problem and are never well solved.
Tailing gangue mineral complicated component is selected, the type of essential mineral includes quartz, feldspar, calcite, muscovite, firefly
Stone, a small amount of cassiterite and other metalliferous minerals etc., cassiterite and other useful metal mineral 1% hereinafter, can not be subject to benefit again
With fluorite grade is lower than 10%, and there is presently no well from the method for selecting recycling fluorite in tailing.
Summary of the invention
For in the prior art to quartz be main gangue or with the tailing of quartzy gangue association multi-metal sulfide it is (low
Grade fluorite) beneficiation method existing for defect, the purpose of the invention is to provide one kind from association cassiterite, lead zinc sulfide
Select in tailing through the method for discontinuous flotation high efficiente callback high-grade fluorite concentrate.
The present invention provides a kind of from the method for selecting flotation recovery fluorite in tin tailings, method includes the following steps:
1) it selects tin tailings after ore grinding accounts for 55%~85% to -200 mesh grade mass percents, is sized mixing using sodium carbonate
To pH values of pulp to 7.5~9.5, using waterglass as inhibitor, kerosene and oleic acid carry out roughing as collecting agent；
2) after rougher concentration regrinding to -400 mesh grade mass percents account for 75%~95%, using calgon as suppression
Preparation, it is selected to get fluorite concentrate by least 6 times.
Preferred scheme, sodium carbonate amount is 2000~3500g/t in the rougher process, waterglass dosage is 800~
1400g/t, collector dosage are 800~1600g/t.
More preferably scheme, the mass ratio of kerosene and oleic acid is 1:1~2:1 in the collecting agent.
Preferred scheme, the dosage of calgon is 10~80g/t in the refining process.
Of the invention is a kind of from the method for selecting flotation recovery fluorite in tin tailings, comprising the following specific steps
(1) after selecting tin tailings is levigate to account for 55%~85% to -200 mesh grade mass percentage contents, add water to size mixing, obtain
The ore pulp for being 50%~75% to mass percent concentration；
(2) into ore pulp with 2000~3500g/t amount be added sodium carbonate, stir 2~4min, adjust pH values of pulp be 7.5~
9.0, then waterglass is added with 800~1400g/t amount, 1~3min is stirred, then oleic acid and coal are added with 800~1600g/t amount
Oil stirs 4~6min, carries out froth flotation under conditions of slurry temperature is 15~30 DEG C；
(3) after flotation froth product is placed 1~3 day in 10~20 DEG C of environment, add water to size mixing, it is dense to obtain mass percent
The ore pulp that degree is 20%~80%, and ore grinding to -400 mesh grade mass percentage contents account for 75%~95%；
(4) solid-to-liquid ratio of ore pulp is adjusted between 1g:5~20mL, and calgon is added with 10~80g/t amount, carries out 6
Secondary froth flotation is to get fluorite concentrate.
Ore grinding of the invention is realized in the ball mill.
Rougher process of the invention is realized in 1.5L flotation device.Flotation time is to scrape the bubble on froth bed without mine
Until measure.
Refining process of the invention is realized in 0.5L flotation device.
Compared with the prior art, technical solution of the present invention has the benefit that
Technical solution of the present invention first passage floatation process from using quartz as the tailing of main gangue or with quartzy gangue
High efficiente callback high-grade fluorite in association multi-metal sulfide tailing, fluorite concentrate is high-quality, and impurity content is low, and grade reaches
85% or more, the rate of recovery reaches 40% or more.
Using sodium carbonate as regulator in floatation process of the invention, not only adjustable slurry pH and to sludge
Dispersed, while can prevent the metal ions such as calcium and magnesium in hard water from having an adverse effect to fluorite with softening of water.It is floating
Select in technique roughing that can inhibit the silicate gangue minerals such as quartz, feldspar as inhibitor using waterglass, and in flotation
Sludge can be dispersed in the process, eliminate thin mud the cover.Using oleic acid and kerosene hybrid collector in floatation process, relatively often
Oleic collector has higher collecting ability and selectivity, and overcomes that simple oleic acid is low temperature resistant, bad dispersibility
The problems such as.
Regrinding process is used in floatation process of the invention.Be mainly based upon the particularity of tailings ore object phase, fluorite with
Quartz inlays relationship complexity, and disseminated grain size is subtle, can make fluorite and quartzy monomer dissociation by fine grinding；And regrinding can make
With quartz, the impurity De contamination weaker in conjunction with collecting agent such as sulfide, to further increase fluorite grade in flotation.
Present invention employs the floatation process of interruption operation, the suction-operated of fluorite and hybrid collector is better than impurity and mixes
The suction-operated of collecting agent is closed, interruption operation is conducive to quartz, the impurity such as lead zinc sulfide and collecting agent De contamination, and regrinding
Mechanism enhance the separation of impurity and collecting agent, thus be conducive to improve fluorite grade.
Detailed description of the invention
[Fig. 1] is process flow chart of the invention.
Specific embodiment
Content that following embodiment is further intended to that the present invention will be described in detail, the claims in the present invention protection scope but unrestricted
In embodiment.
The main mineral in CHARACTERISTICS OF TAILINGS SAND used in following embodiment and comparison is quartzy (accounting for 60% or more), feldspar
(accounting for 20% or so) and calcite, muscovite, a small amount of skarn mineral, metalliferous mineral and fluorite (accounting for 10% or so).
Embodiment 1
- 200 mesh are milled to mine and account for 70%, water is added to be made into the magma of pulp density 30%, are poured into 1.5L flotation device and are added
Sodium carbonate 3000g/t, pH values of pulp 8.5 stir 3min；Dispersing agent waterglass 1000g/t is added, stirs 2min；Kerosene is added
It with oleic acid mixture (2:1) 1200g/t, stirs 5 minutes, air flotation 7min obtains rough concentrate；Rough concentrate regrinding extremely -400 mesh
80% is accounted for, is added in 0.5L flotation device, adding water to adjust pulp density is 18%；It is selected for the first time, 1500g/t sodium carbonate is added,
3min is stirred, 30g/t calgon is added and stirs 2min, air flotation 5min；It is selected for the second time to be separately added into the 6th time
20g/t calgon, stirs 2min, and air flotation 3min obtains fluorite concentrate product
The fluorite concentrate yield that this example obtains is 4.0%, grade 85.0%, rate of recovery 42.5%.
Embodiment 2
- 200 mesh are milled to mine and account for 80%, water is added to be made into the magma of pulp density 30%, are poured into 1.5L flotation device and are added
Sodium carbonate 3500g/t, pH values of pulp 9 stir 3min；Dispersing agent waterglass 1000g/t is added, stirs 2min；Be added kerosene with
Oleic acid mixture (1:1) 1500g/t is stirred 5 minutes, and air flotation 7min obtains rough concentrate；Rough concentrate at normal temperature (15~25
DEG C) place 1 day；Rough concentrate regrinding to -400 mesh account for 90%, are added in 0.5L flotation device, and adding water to adjust pulp density is 20%；
It is selected for the first time, 2000g/t sodium carbonate is added, stirs 3min, 10g/t calgon is added and stirs 2min, air flotation
5min；Second is separately added into 10g/t calgon selected to the 6th time, stirs 2min, air flotation 3min obtains fluorite
Concentrate product
The fluorite concentrate yield that this example obtains is 4.2%, grade 93.84%, the rate of recovery 46.37%.
Embodiment 3
- 200 mesh are milled to mine and account for 85%, water is added to be made into the magma of pulp density 30%, are poured into 1.5L flotation device and are added
Sodium carbonate 2500g/t, pH values of pulp 8.0 stir 3min；Dispersing agent waterglass 1200g/t is added, stirs 2min；Kerosene is added
It with oleic acid mixture (1:1) 1200g/t, stirs 5 minutes, air flotation 7min obtains rough concentrate；Rough concentrate at normal temperature (15~
25 DEG C) it places 3 days；Rough concentrate regrinding to -400 mesh account for 95%, are added in 0.5L flotation device, add water to adjust pulp density and are
20%；It is selected for the first time, 2000g/t sodium carbonate is added, stirs 3min, 20g/t calgon is added and stirs 2min, Inflated floating
Select 5min；Second is separately added into 20g/t calgon selected to the 6th time, stirs 2min, air flotation 3min obtains firefly
Stone concentrate product
The fluorite concentrate yield that this example obtains is 3.9%, grade 96.10%, the rate of recovery 43.87%.
Embodiment 4
- 200 mesh are milled to mine and account for 80%, water is added to be made into the magma of pulp density 30%, are poured into 1.5L flotation device and are added
Sodium carbonate 3000g/t, pH values of pulp 8.5 stir 3min；Dispersing agent waterglass 1500g/t is added, stirs 2min；Kerosene is added
It with oleic acid mixture (1:1) 1500g/t, stirs 5 minutes, air flotation 7min obtains rough concentrate；Rough concentrate regrinding extremely -400 mesh
90% is accounted for, is added in 0.5L flotation device, adding water to adjust pulp density is 20%；It is selected for the first time, 2000g/t sodium carbonate is added,
3min is stirred, 20g/t calgon is added and stirs 2min, air flotation 5min；It is selected for the second time to be separately added into the 6th time
20g/t calgon stirs 2min, air flotation 3min；Selected four, selected five and selected six chats is mixed, mixing
It is closed circuit that middling recurrence enters a selected formation together with the rough concentrate after regrinding；Finally obtain fluorite concentrate product
The fluorite concentrate yield that this example obtains is 4.8%, grade 86.30%, the rate of recovery 53.65%.
Comparative example 1
- 200 mesh are milled to mine and account for 70%, water is added to be made into the magma of pulp density 30%, are poured into 1.5L flotation device and are added
Sodium carbonate 3000g/t, pH values of pulp 8.5 stir 3min；Dispersing agent waterglass 1000g/t is added, stirs 2min；Kerosene is added
It with oleic acid mixture (2:1) 1000g/t, stirs 5 minutes, air flotation 7min obtains rough concentrate；The grade of fluorite in rough concentrate
It is 38.98%, the rate of recovery 91.88%.
When oleic acid being only added in roughing as collecting agent 1000g/t, rough concentrate grade is 21.82%, and the rate of recovery is
72.69%.
When kerosene being only added in roughing as collecting agent 1000g/t, rough concentrate grade is 32.12%, and the rate of recovery is
69.34%.
Comparative example explanation, when kerosene and oleic acid are as combined capturing and collecting agent, the two generates apparent synergy and makees
With when relatively single kerosene and oleic acid are as collecting agent, the flotation effects such as fluorite grade and the rate of recovery are obviously improved.
Comparative example 2
- 200 mesh are milled to mine and account for 85%, water is added to be made into the magma of pulp density 30%, are poured into 1.5L flotation device and are added
Sodium carbonate 2500g/t, pH values of pulp 8.0 stir 3min；Dispersing agent waterglass 1200g/t is added, stirs 2min；Kerosene is added
It with oleic acid mixture (1:1) 1200g/t, stirs 5 minutes, air flotation 7min obtains rough concentrate；Rough concentrate at normal temperature (15~
25 DEG C) it places 3 days；It is added in 0.5L flotation device, adding water to adjust pulp density is 20%；It is selected for the first time, 2000g/t carbon is added
Sour sodium stirs 3min, and 20g/t calgon is added and stirs 2min, air flotation 5min；Second of selected to the 6th time difference
20g/t calgon is added, stirs 2min, air flotation 3min obtains fluorite concentrate product.The firefly that this comparison example obtains
Stone concentrate grade is 76.50%, the rate of recovery 36.38%.
Fluorite concentrate grade and the rate of recovery are substantially reduced after rough concentrate flotation of the explanation without regrinding in the comparative example.
Claims (3)
1. a kind of from the method for selecting flotation recovery fluorite in tin tailings, it is characterised in that: the following steps are included:
1) it selects tin tailings after ore grinding accounts for 55 %~85% to -200 mesh grade mass percentage contents, is sized mixing using sodium carbonate
It is 7.5~9.5 to pH values of pulp, using waterglass as inhibitor, kerosene and oleic acid carry out roughing as collecting agent；
2) after rougher concentration regrinding to -400 mesh grade mass percentage contents account for 75%~95%, using calgon as inhibition
Agent, it is selected to get fluorite concentrate by least 6 times；
Sodium carbonate amount is 2000~3500g/t in the rougher process, and waterglass dosage is 800~1400g/t, and collecting agent is used
Amount is 800~1600g/t；
The mass ratio of kerosene and oleic acid is 1:1 ~ 2:1 in the collecting agent.
2. according to claim 1 a kind of from the method for selecting flotation recovery fluorite in tin tailings, it is characterised in that: the essence
The dosage of calgon is 10 ~ 80g/t during choosing.
3. described in any item a kind of from the method for selecting flotation recovery fluorite in tin tailings according to claim 1 ~ 2, feature exists
In: the following steps are included:
(1) after selecting tin tailings is levigate to account for 55 %~85% to -200 mesh grade mass percentage contents, add water to size mixing, obtain matter
Measure the ore pulp that percent concentration is 50%~75%；
(2) sodium carbonate is added with 2000 ~ 3500g/t amount into ore pulp, stirs 2 ~ 4min, adjusting pH values of pulp is 7.5 ~ 9.0, then with
Waterglass is added in 800 ~ 1400g/t amount, stirs 1 ~ 3min, then oleic acid and kerosene is added with 800 ~ 1600g/t amount, stir 4 ~
6min carries out froth flotation under conditions of slurry temperature is 15 ~ 30 DEG C；
(3) after flotation froth product is placed 1 ~ 3 day in 10 ~ 20 DEG C of environment, water is added to size mixing, obtaining mass percent concentration is
20% ~ 80% ore pulp, and ore grinding to -400 mesh grade mass percentage contents account for 75%~95%；
(4) solid-to-liquid ratio of ore pulp is adjusted between 1g:5 ~ 20mL, and calgon is added with 10 ~ 80g/t amount, carries out 6 foams
Flotation is to get fluorite concentrate.
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| CN108624765B (en) * | 2018-06-14 | 2019-08-27 | 中南大学 | A kind of technique from the low-grade high efficiente callback of tailing containing rubidium rubidium |
| CN112264195B (en) * | 2020-11-18 | 2021-10-12 | 东北大学 | Cassiterite mineral flotation inhibitor and application thereof |
| CN114570531A (en) * | 2022-01-25 | 2022-06-03 | 贵州省新材料研究开发基地 | Flotation separation method for low-grade carbonate fluorite ore |
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