CN103072975A - Low-grade aphanitic graphite dressing and purifying method - Google Patents
Low-grade aphanitic graphite dressing and purifying method Download PDFInfo
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- CN103072975A CN103072975A CN2012105812020A CN201210581202A CN103072975A CN 103072975 A CN103072975 A CN 103072975A CN 2012105812020 A CN2012105812020 A CN 2012105812020A CN 201210581202 A CN201210581202 A CN 201210581202A CN 103072975 A CN103072975 A CN 103072975A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000010439 graphite Substances 0.000 title claims abstract description 34
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 34
- 238000005188 flotation Methods 0.000 claims abstract description 61
- 239000012141 concentrate Substances 0.000 claims abstract description 33
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 26
- 238000007885 magnetic separation Methods 0.000 claims abstract description 13
- 238000000746 purification Methods 0.000 claims abstract description 13
- 239000003112 inhibitor Substances 0.000 claims abstract description 9
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 8
- 239000011707 mineral Substances 0.000 claims abstract description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 21
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 239000003350 kerosene Substances 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 239000011148 porous material Substances 0.000 claims description 12
- WVYWICLMDOOCFB-UHFFFAOYSA-N 4-methyl-2-pentanol Chemical compound CC(C)CC(C)O WVYWICLMDOOCFB-UHFFFAOYSA-N 0.000 claims description 11
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 11
- 239000004115 Sodium Silicate Substances 0.000 claims description 11
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 235000019353 potassium silicate Nutrition 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 239000006148 magnetic separator Substances 0.000 claims description 4
- 230000010349 pulsation Effects 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- 239000001117 sulphuric acid Substances 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims description 2
- 238000000227 grinding Methods 0.000 abstract description 23
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 238000003801 milling Methods 0.000 description 10
- 229910052742 iron Inorganic materials 0.000 description 9
- 229910000831 Steel Inorganic materials 0.000 description 7
- 239000010959 steel Substances 0.000 description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000007670 refining Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000013081 microcrystal Substances 0.000 description 2
- 238000005065 mining Methods 0.000 description 2
- 229910021382 natural graphite Inorganic materials 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 229960000411 camphor oil Drugs 0.000 description 1
- 239000010624 camphor oil Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a low-grade aphanitic graphite dressing and purifying method, belonging to the technical field of graphite purification. The method comprises the following steps: firstly, crushing and grinding aphanitic graphite ores with fixed carbon content of 45-80%; adding a slime flocculant, an inhibitor, a collector and a foamer into the ore pulp, separating by flotation in a mechanical flotation machine, re-grinding and re-separating the flotation concentrate to remove most gangue mineral in the ores, thus obtaining final flotation concentrate; removing iron-contained gangue mineral in the final flotation concentrate by high-gradient magnetic separation, thus being capable of obtaining a product II satisfying the requirements of number WT88 or more. And a product II satisfying the requirements of number W80 can be obtained by re-grinding and re-separating the middling product and concentratedly re-separating the magnetically separated middling product. The total recovery is more than 80%. The low-grade aphanitic graphite dressing and purifying method is low in requirement on fixed carbon content of the ores, capable of effectively reducing iron-contained impurities, large in processing amount, low in production cost and environmental-friendly.
Description
Technical field
The present invention relates to a kind of low-grade aphanitic graphite ore dressing method of purification, belong to the graphite purification technical field.
Background technology
Aphanitic graphite is one of Dominant Mineral Resources of China, and wherein Chenzhou Lu Tang graphite mining area head grade is 50% ~ 90%, and the iron level of part raw ore is 1.0% ~ 1.5%; Panshi City, Jilin and aphanitic graphite mining area, Mei County, Shaanxi average grade 60%～65%, the iron level of raw ore is 2.0% ~ 3.0%.Present site technique: raw ore → coarse crushing → in broken → oven dry → ore grinding → classification → packing, there is following problem in this production technique: 1) part low-carbon (LC) raw ore is difficult to utilization; 2) preliminary working product fixed carbon content is low, and further deep processing is graphite material, and product is mainly used in the low side fields such as casting, steel-smelting and carburating agent, Graphite Electrodes, carbon rod of battery, and added value is not high.3) iron level exceeds standard in the raw ore, according to the technical requirements of GB3519-2008-T microcrystalline graphite product, for major part iron requirement product is arranged, and its iron level requires below 1.0% at least, and the requirement that has more is low to moderate 0.15%, and technique can't satisfy according to this.
In order to make the aphanitic graphite raw ore be able to high value added utilization, carried out a large amount of research both at home and abroad, obtain the higher product of purity by purification, the method for purification mainly contains flotation process, acid-base method, hydrofluoric acid method, chlorinating roasting, pyroprocess etc.Wherein hydrofluoric acid method and acid-base method exist the raw ore foreign matter content to change to cause purify rear graphite grade fluctuation greatly, concentrate grade can reach 99% preferably the time, and only on average gets off 94% ~ 96%, and the soda acid consumption is large, cost is high, and it is serious that a large amount of acidic and alkaline waste waters produce environmental pollution.Chlorinating roasting, Chinese invention patent ZL94105051.3 high-temp chlorination refining process for natural graphite and the Reaktionsofen that adopts, the product after this method is purified can reach more than 99%, and chlorine consumption is large, and environment and people's safety is caused a significant threat.Pyroprocess: utilize the resistant to elevated temperatures characteristics of graphite energy, under the condition of secluding air, high temperature (greater than 2700 ℃) makes the impurity vaporization and is evaporated, thereby reach the purification purpose, Chinese invention patent ZL200420035742.X continuous industrial natural graphite purifying device, this equipment can be produced high-purity micro crystal graphite of 99%, 99.9% and 99.99%, and cost is respectively 8000 yuan/tons, 15000 yuan/tons and 28000 yuan/tons, this method product purity is high, but production cost is higher simultaneously.
Flotation process is utilized the interfacial chemistry nature difference of the gangue minerals such as aphanitic graphite and aluminosilicate, realizes separating of graphite and impurity by adjusting close and distant water difference therebetween.Chinese invention patent ZL200910112366.7 discloses ore dressing purification and the new technology for purifying of a kind of micro crystal graphite (being hidden graphite).The technique first half is the flotation process hidden graphite of purifying, fixed carbon content is greater than 80% raw ore, take water glass as inhibitor, kerosene is collecting agent, and pine camphor oil is pore forming material, through primary grinding, one roughing, once purging selection, twice is selected, obtain the concentrate of the fixed carbon content about 90% of productive rate about 50%, concentrate is purified through acid-base method and is obtained the product of fixed carbon about 98%.Its floatation process is high to raw ore fixed carbon content requirement, and be lower than 80% raw ore adaptability for a large amount of fixed carbon content not strong; The efficiency of separation is not high, and flotation concentrate fixed carbon content is only brought up to about 90% from about 85% of raw ore.
Thereby, develop the raw ore that can effectively utilize low fixed carbon content, the efficiency of separation is high, effectively reduces the concentrate iron level, and processing cost is low, and the hidden graphite purification method of environmental protection seems particularly important.
Summary of the invention
Purpose of the present invention is exactly in order to overcome exist in the existing hidden graphite purification high to raw ore fixed carbon content requirement, processing cost is high, the problem that environmental pollution is large, the method that provides a kind of aphanitic graphite ore dressing to purify, make a large amount of fixed carbon content low, the hidden graphite resource that iron level exceeds standard is able to efficient utilization.
A kind of low-grade aphanitic graphite ore dressing method of purification may further comprise the steps:
1) with the aphanitic graphite crushing raw ore of fixed carbon content 45-80%, then through at least two stage grinding-flotation, every section flotation is by one roughing and selectedly at least one times consist of, roughly select front adding slime flocculant, inhibitor water glass, collecting agent kerosene, pore forming material MIBC in ore pulp at every turn, stir, and flotation in subaeration flotation machine, the concentrate that every section ore grinding-flotation obtains enters lower primary grinding-flotation, is fixed at last carbon content and is not less than 88% flotation final concentrate and regrinding and reconcentration chats; Described slime flocculant is a kind of in polyethylene oxide and the acidified sodium silicate, or both are according to the mixture of mass ratio 1:1 ~ 15; Polyethylene oxide molecular weight 500,000-1,000 ten thousand wherein, acidified sodium silicate be mass concentration be 5% modulus be 2 ~ 3.6 water glass solution and mass concentration be 5% sulphuric acid soln in mass ratio 1:1 ~ 1.5 mixed preparing form; During alone polyethylene oxide, its consumption is 10 ~ 400g/t, and during alone acidified sodium silicate, its consumption is at 500g/t ~ 4000g/t, and when adopting both mixtures, its consumption is 100g/t ~ 2000g/t;
2) the flotation final concentrate is deviate from rider mineral wherein through magnetic separation, is met above product I and the magnetic middling ore that requires of trade mark WT88 or WT88;
3) magnetic middling ore that the regrinding and reconcentration chats and the step 2 that obtain of step 1)) obtains is concentrated, and adds collecting agent kerosene, and pore forming material MIBC and stirs in ore pulp, and is selected through roughly selecting 2 times for 1 time, obtains to satisfy the product II that trade mark W80 requires.
The described degree of crushing of step 1) is to be crushed to below the 0.5mm;
As when being three sections and above grinding flotation, the first paragraph grinding fineness accounts for 40-60% to-0.074mm, and ore milling concentration is 30-50%; The second segment grinding fineness accounts for 60-85% to-0.074mm, and ore milling concentration is 30-50%; Final grinding fineness accounts for 85-98% to-0.074mm, and ore milling concentration is 20-40%;
As when being two stage grinding-flotation, the first paragraph grinding fineness accounts for 40-60% to-0.074mm, and ore milling concentration is 30-50%; The second segment grinding fineness accounts for 85-98% to-0.074mm, and ore milling concentration is 20-40%.
Step 2) vertical ring pulsating high gradient magnetic separator is adopted in magnetic separation in, and its processing condition are, background magnetic field intensity 0.6T ~ 1.0T, magnetic separation concentration is 5% ~ 30%, pulsion stroke is 10mm ~ 40mm, the pulsation jig frequency be 100-300 time/divide 3 rev/mins of change revolutions.
In every section ore grinding-floatation process of step 1), roughly select front adding medicine, adding medicine no longer in the refining process;
Regrinding and reconcentration chats described in the step 1) is the concentrate of first paragraph ore grinding-flotation, continues ore grinding-flotation and is called regrinding and reconcentration, and the mine tailing that obtains in the regrinding and reconcentration process is referred to as the regrinding and reconcentration chats because fixed carbon content is relatively high;
Step 2) mine tailing that the magnetic separation of flotation final concentrate obtains in is because of the relatively high magnetic middling ore that is called of fixed carbon content;
The step 3) chats is concentrated and selected also is the rougher process adding medicine, and refining process no longer adds medicament.
The present invention compared with prior art has following innovative characteristics and effect:
1) the present invention is through stage grinding-flotation, and added the slime flocculant of effect excellence, improved hidden graphite flotation pulp environment, improve flotation efficiency, can be that about 50% raw ore is purified with fixed carbon content, be fixed carbon content 88% or 88% above product and the product of fixed carbon content 80%;
2) the further high-gradient magnetic separation deironing of the flotation concentrate of fixed carbon content 88% is met the above product of trade mark WT88 or WT88.
Description of drawings
Fig. 1: low-grade aphanitic graphite ore dressing purification techniques principle process;
Fig. 2: the schema of the embodiment of the invention 1;
Fig. 3: the schema of the embodiment of the invention 2.
Embodiment
Be intended to further specify the present invention below in conjunction with embodiment, and unrestricted the present invention.
Embodiment 1
With reference to Fig. 2, describe embodiments of the invention 1 in detail.
1) first paragraph ore grinding-flotation
With fixed carbon content 49.26%, the aphanitic graphite crushing raw ore of iron level 2.307% below 0.5mm, the first paragraph ore grinding, fineness accounts for 40% to-0.074mm, ore milling concentration is 50%; Add slime flocculant (for polyethylene oxide and the acidified sodium silicate mixture that mixes of 1:10 in mass ratio) 500g/t, inhibitor water glass 1000g/t in the first paragraph ore grinding ore pulp, collecting agent kerosene 1000g/t, pore forming material MIBC are 200g/t, and stir in steel basin; Pass into to roughly select in the subaeration flotation machine with ore pulp behind the pharmacy effect and separate, it is selected through 1 time to roughly select concentrate, obtain first paragraph ore grinding-flotation concentrate, this concentrate enters second segment ore grinding-flotation, roughly selects and the mine tailing I of selected generation abandons as true tailings;
2) second segment ore grinding-flotation
First paragraph ore grinding-flotation concentrate is through the second segment ore grinding, and grinding fineness accounts for 80% for-0.074mm; Ore milling concentration is 40%, add slime flocculant (for polyethylene oxide and the acidified sodium silicate mixture that mixes of 1:10 in mass ratio) 400g/t, inhibitor water glass 800g/t, collecting agent kerosene 800g/t, pore forming material MIBC are 100g/t, and stir in steel basin; And selected through roughly selecting 2 times for 1 time; Can obtain accordingly second segment ore grinding-flotation concentrate and second segment ore grinding-flotation chats;
3) the 3rd section ore grinding-flotation
Second segment ore grinding-flotation concentrate is through the 3rd section ore grinding, and grinding fineness accounts for 92% for-0.074mm; Ore milling concentration is 30%, add slime flocculant (for polyethylene oxide and the acidified sodium silicate mixture that mixes of 1:10 in mass ratio) 300g/t, inhibitor water glass 600g/t, collecting agent kerosene 300g/t, pore forming material MIBC are 100g/t, and stir in steel basin; And selected through roughly selecting 2 times for 1 time; Can obtain accordingly the 3rd section ore grinding-flotation concentrate and the 3rd section ore grinding-flotation chats;
4) the 3rd section ore grinding-flotation concentrate process pulsating high gradient magnetic separator with vertical ring magnetic separation, background magnetic field intensity 1.0T, magnetic separation concentration is 20%, and pulsion stroke is 25mm, and the pulsation jig frequency is 250 times/minutes, 3 rev/mins of change revolutions.Deviate from rider mineral wherein, can obtain to satisfy product I and the magnetic middling ore that trade mark WT88 requires;
5) second segment ore grinding-flotation chats and the 3rd section ore grinding-flotation chats and magnetic middling ore are concentrated again choosing, add collecting agent kerosene 400g/t, pore forming material MIBC and are 40g/t, and stir in steel basin; And through roughly select for 1 time 2 times selected, can obtain to satisfy the product II that trade mark W80 requires, chats selects the mine tailing II of generation to abandon as true tailings again;
6) concentrate is shown in Table 1 through concentrating, filter, dry, be packaged to be the finished product specific targets.
Three sections ore grinding ━ of table 1 flotation flowsheet index
Embodiment 2
With reference to Fig. 3, describe embodiments of the invention 2 in detail.
1) first paragraph ore grinding-flotation
With fixed carbon content 63.52%, the aphanitic graphite crushing raw ore of iron level 2.12% below 0.5mm, the first paragraph ore grinding, fineness accounts for 60% to-0.074mm, ore milling concentration is 50%; Add slime flocculant (for polyethylene oxide and the acidified sodium silicate mixture that mixes of 1:10 in mass ratio) 450g/t, inhibitor water glass 1000g/t in the first paragraph ore grinding ore pulp, collecting agent kerosene 1200g/t, pore forming material MIBC are 240g/t, and stir in steel basin; Pass into to roughly select in the subaeration flotation machine with ore pulp behind the pharmacy effect and separate, it is selected through 1 time to roughly select concentrate, obtain first paragraph ore grinding-flotation concentrate, this concentrate enters second segment ore grinding-flotation, roughly selects and the mine tailing I of selected generation abandons as true tailings.
2) second segment ore grinding-flotation
First paragraph ore grinding-flotation concentrate is through the second segment ore grinding, and grinding fineness accounts for 94% for-0.074mm; Ore milling concentration is 30%, add slime flocculant (for polyethylene oxide and the acidified sodium silicate mixture that mixes of 1:10 in mass ratio) 260g/t, inhibitor water glass 600g/t, collecting agent kerosene 600g/t, pore forming material MIBC are 150g/t, and stir in steel basin; And selected through roughly selecting 2 times for 1 time; Can obtain accordingly second segment ore grinding-flotation concentrate and second segment ore grinding-flotation chats.
3) second segment ore grinding-flotation concentrate process pulsating high gradient magnetic separator with vertical ring magnetic separation, background magnetic field intensity 1.0T, magnetic separation concentration is 20%, and pulsion stroke is 25mm, and the pulsation jig frequency is 250 times/minutes, 3 rev/mins of change revolutions.Deviate from rider mineral wherein, can obtain to satisfy product I and the magnetic middling ore that trade mark WT90 requires.
4) second segment ore grinding-flotation chats and magnetic middling ore are concentrated again choosing, add collecting agent kerosene 440g/t, pore forming material MIBC and are 50g/t, and stir in steel basin; And through roughly select for 1 time 2 times selected, can obtain to satisfy the product II that trade mark W80 requires, chats selects the mine tailing II of generation to abandon as true tailings again.
5) concentrate is shown in Table 2 through concentrating, filter, dry, be packaged to be the finished product specific targets.
Table 2 secondary grinding ━ flotation flowsheet index
Claims (2)
1. a low-grade aphanitic graphite ore dressing method of purification is characterized in that, may further comprise the steps:
1) with the aphanitic graphite crushing raw ore of fixed carbon content 45-80%, then through at least two stage grinding-flotation, every section flotation is by one roughing and selectedly at least one times consist of, roughly select front adding slime flocculant, inhibitor water glass, collecting agent kerosene, pore forming material MIBC in ore pulp at every turn, stir, and flotation in subaeration flotation machine; The concentrate that every section ore grinding-flotation obtains enters lower primary grinding-flotation, is fixed at last carbon content and is not less than 88% flotation final concentrate and regrinding and reconcentration chats; Described slime flocculant is a kind of in polyethylene oxide and the acidified sodium silicate, or both are according to the mixture of mass ratio 1:1 ~ 15; Polyethylene oxide molecular weight 500,000-1,000 ten thousand wherein, acidified sodium silicate be mass concentration be 5% modulus be 2 ~ 3.6 water glass solution and mass concentration be 5% sulphuric acid soln in mass ratio 1:1 ~ 1.5 mixed preparing form; During alone polyethylene oxide, its consumption is 10 ~ 400g/t, and during alone acidified sodium silicate, its consumption is at 500g/t ~ 4000g/t, and when adopting both mixtures, its consumption is 100g/t ~ 2000g/t;
2) the flotation final concentrate is deviate from rider mineral wherein through magnetic separation, is met above product I and the magnetic middling ore that requires of trade mark WT88 or WT88;
3) magnetic middling ore that the regrinding and reconcentration chats and the step 2 that obtain of step 1)) obtains is concentrated, and adds collecting agent kerosene, and pore forming material MIBC and stirs in ore pulp, and is selected through roughly selecting 2 times for 1 time, obtains to satisfy the product II that trade mark W80 requires.
2. the method described in according to claim 1, it is characterized in that, step 2) magnetic separation in, adopt vertical ring pulsating high gradient magnetic separator, its processing condition are background magnetic field intensity 0.6T ~ 1.0T, magnetic separation concentration is 5% ~ 30%, pulsion stroke is 10mm ~ 40mm, and the pulsation jig frequency is 100-300 time/minute, 3 rev/mins of change revolutions.
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