CN103395792B - A kind of method preparing white carbon black - Google Patents
A kind of method preparing white carbon black Download PDFInfo
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- CN103395792B CN103395792B CN201310300541.1A CN201310300541A CN103395792B CN 103395792 B CN103395792 B CN 103395792B CN 201310300541 A CN201310300541 A CN 201310300541A CN 103395792 B CN103395792 B CN 103395792B
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- hydrochloric acid
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000006229 carbon black Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 39
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 126
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 105
- 238000002386 leaching Methods 0.000 claims abstract description 76
- 239000002253 acid Substances 0.000 claims abstract description 53
- 150000003839 salts Chemical class 0.000 claims abstract description 43
- 238000005406 washing Methods 0.000 claims abstract description 41
- 239000006210 lotion Substances 0.000 claims abstract description 28
- 239000002893 slag Substances 0.000 claims abstract description 17
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims abstract description 11
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 11
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 54
- 238000003756 stirring Methods 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 10
- 239000012716 precipitator Substances 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 238000012216 screening Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 230000003750 conditioning effect Effects 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 34
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 26
- 239000010703 silicon Substances 0.000 abstract description 26
- 229910052710 silicon Inorganic materials 0.000 abstract description 26
- 238000000605 extraction Methods 0.000 abstract description 22
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract description 17
- 238000011084 recovery Methods 0.000 abstract description 12
- 239000000126 substance Substances 0.000 abstract description 4
- 239000006227 byproduct Substances 0.000 abstract description 3
- 229910052783 alkali metal Inorganic materials 0.000 abstract 1
- 150000001340 alkali metals Chemical class 0.000 abstract 1
- 239000004411 aluminium Substances 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 abstract 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract 1
- 238000005660 chlorination reaction Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000012452 mother liquor Substances 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 18
- 239000011707 mineral Substances 0.000 description 18
- 238000000354 decomposition reaction Methods 0.000 description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 239000004115 Sodium Silicate Substances 0.000 description 8
- 239000003513 alkali Substances 0.000 description 8
- 238000010828 elution Methods 0.000 description 8
- 239000012065 filter cake Substances 0.000 description 8
- 239000002002 slurry Substances 0.000 description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 8
- 229910052911 sodium silicate Inorganic materials 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 3
- 244000043261 Hevea brasiliensis Species 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229920003052 natural elastomer Polymers 0.000 description 2
- 229920001194 natural rubber Polymers 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 229940034610 toothpaste Drugs 0.000 description 2
- 239000000606 toothpaste Substances 0.000 description 2
- 241001672018 Cercomela melanura Species 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of method preparing white carbon black, by baiyuneboite or its mine tailing sodium carbonate roasting, wash this roasted ore, water lotion is for reclaiming silicon, aluminium and alkali-metal oxyhydroxide, Leaching in Hydrochloric Acid is adopted to washing slag, leach liquor is for containing the thick solution of scandium, and as the raw material extracting scandium further, and the slag of acidleach is exactly raw material of the present invention.Again the ratio of acid leaching residue and the alkali metal hydroxide after drying grinding and chlorination system fused salt 1.0:1.0 ~ 2.0:1.0 is in mass ratio mixed, roasting is carried out at 600 DEG C ~ 750 DEG C, then neutrality is washed to the first water logging of the acid leaching residue after roasting, adopts preparing white carbon black by precipitation method using water lotion as mother liquor.The simple science of present invention process, the scandium enriched substance acid leaching residue that can prepare from baiyuneboite or its mine tailing efficiently leaches extraction silicon and prepares white carbon black, leaching yield >=90%, and other byproducts can be reclaimed from technique, be the method for silicon in a kind of synthetical recovery Bayan Obo mine tailing.
Description
Technical field
The present invention relates to a kind of method preparing white carbon black, belong to chemical field.
Background technology
During World War II, white carbon black starts extensive for industrial production, mainly precipitated silica, what it is found that white carbon black adds the performance greatly can improving some material, precipitated silica is mainly used as natural rubber and elastomeric strengthening agent, brightening of toothpaste abrasives and paper, white carbon black can be used as natural rubber and elastomeric reinforced filling, additive for synthetic resin, ink thickeners, the antisettling agent of pigment in coating, vehicle and soft metal rumbling compound, and the antisettling agent in emulsifying agent, the filler of all right used as pesticides carrier and light black newsprinting paper, abrasive etc. in toothpaste.This makes the performance study of white carbon black and practical application request amount greatly increase.
Baiyuneboite is typical intergrowth mineral, the resources such as rare earth, iron, niobium, fluorite and scandium are not only rich in ore deposit, also be rich in the silicon of certain content, and along with the exploitation of the resource such as rare earth, iron, and after elements scandium extracts, silicon obtains further enrichment, and have benefited from the leaching process of scandium, make the destroyed of the silicate sturcture part in mine tailing, make the extraction of silicon relatively easy, be mine tailing and extract silicon and prepare white carbon black and provide approach.About the extraction work of iron tailings silicon, forefathers also do excessive quantifier elimination, as patent (application number is 201110071373) have studied the method that iron tailings prepares Nano carbon white, but fail for actual production always, its major cause is that the angle of failing from comprehensive utilization of resources is considered, process costs is too high.And what progress the extraction of silicon never has in baiyuneboite iron tailings, so the present invention still has actual meaning very much.
Summary of the invention
The technical issues that need to address of the present invention are just the defect overcoming prior art, a kind of method preparing white carbon black is provided, the simple science of present invention process, the scandium enriched substance acid leaching residue that can prepare from baiyuneboite or its mine tailing efficiently leaches extraction silicon and prepares white carbon black, leaching yield >=90%, and other byproducts can be reclaimed from technique, be the method for silicon in a kind of synthetical recovery Bayan Obo mine tailing.
For solving the problem, the present invention adopts following technical scheme:
The invention provides a kind of method preparing white carbon black, described method is with Bayan Obo mine tailing acid leaching residue for raw material, and concrete steps are:
(1), by grinding after Bayan Obo mine tailing mix with alkali metal hydroxide, roasting;
(2), by the tailings water after roasting be washed till neutrality, filter, obtain water lotion and washing slag, washing slag adopts Leaching in Hydrochloric Acid, filtration again, obtains leach liquor and leached mud, and leach liquor is that leached mud is acid leaching residue containing scandium solution;
(3), acid leaching residue is mixed with alkali metal hydroxide and fused salt, roasting;
(4), by the acid leaching residue after roasting stir water logging in a water bath, after water logging, filtered water is washed till screening in neutral, obtains filtrate and washing slag;
(5), under water-bath, stirring, extremely neutral with hydrochloric acid conditioning solution pH to filtrate, utilize precipitator method production of silica white, washing, oven dry are filtered to obtained white carbon black.
The SiO of acid leaching residue prepared by Bayan Obo mine tailing of the present invention
2content is 500 ~ 700kg/t.
Alkali metal hydroxide of the present invention is the one in sodium hydroxide or potassium hydroxide, and the mass ratio of mine tailing and alkali metal hydroxide is 1:1.3:, maturing temperature is 350 DEG C, and the time is 2h, concentration of hydrochloric acid 2 ~ 3mol/L.
Fused salt of the present invention is NaCl/KCl fused salt, and the NaCl/KCl in fused salt is 1:1 proportioning in mass ratio, and 1:1 ~ 2:1 is baking mixed in mass ratio for acid leaching residue and alkali metal hydroxide and fused salt, maturing temperature 600 ~ 750 DEG C, roasting time 0.5 ~ 3h.
Acid leaching residue after roasting of the present invention stirs water logging, and water soaking temperature 50 ~ 95 DEG C, filters after water logging, by hot water wash screening to neutral.
Filtrate reaction water bath temperature of the present invention is 50 ~ 95 DEG C, time 0.15 ~ 0.5h, stir speed (S.S.) 500r/min.
The simple science of present invention process, the scandium enriched substance acid leaching residue that can prepare from baiyuneboite or its mine tailing efficiently leaches extraction silicon and prepares white carbon black, leaching yield >=90%, and other byproducts can be reclaimed from technique, be the method for silicon in a kind of synthetical recovery Bayan Obo mine tailing.
Advantage of the present invention is:
1, to have maturing temperature low for technique of the present invention, energy consumption is little, raw material dosage is little, and equipment requirements is low, the rate of recovery high of silicon, in the process extracting silicon, do not have poisonous, severe corrosive gas generation, can not leave over a large amount of industrial slags, major impurity element can effectively be recycled, become Industrial products, reduce the cost in white carbon black preparation process.
2, the raw material of employing of the present invention is the baiyuneboite mine tailing acid leaching residue obtained through low-temperature bake acid treatment, silicone content is high, impurity is few, it also avoid the waste of other resources when extracting silicon, cost is low, can scandium be reclaimed simultaneously, noble metal niobium enrichment of element can also be made, there is stronger industrial application value.
3, the present invention is not only suitable for the silicon resource in baiyuneboite mine tailing acid leaching residue, be also suitable for other area, mineral deposit containing silicon resource.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in detail, but content of the present invention is not only confined to the following examples.
Embodiment 1
(1) sodium carbonate roasting: get 100g Bayan Obo mine tailing, add 130g sodium hydroxide and mix, carry out roasting, the temperature of roasting 350 DEG C, the time is 2h;
(2) wash: adopt general industry water, washing filtering is carried out to the mineral after Roasting Decomposition, and repeatedly washing leaching cake is less than 9 to the pH of water lotion;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after being decomposed by sodium carbonate roasting adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 DEG C, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and with 400mL salt acid elution filter cake, obtains hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get 100g acid leaching residue, add 130g sodium hydroxide and 100g fused salt and mix, carry out roasting, the temperature of roasting 700 DEG C, the time is 2h;
(5) water logging: adopt general industry water, carry out water logging to the mineral after Roasting Decomposition, extraction temperature is 85 DEG C, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, filtered water is washed till pH is 7 ~ 9, obtain water lotion and washing slag, water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates about Ph to 7, under water-bath 95 DEG C, stirring 500r/min, utilizes the precipitator method to obtain white carbon black, and obtained white carbon black is filtered to washing, dries, and the rate of recovery of silicon is 78.25%.
Embodiment 2
(1) sodium carbonate roasting: get 100g Bayan Obo mine tailing, add 130g sodium hydroxide and mix, carry out roasting, the temperature of roasting 350 DEG C, the time is 2h;
(2) wash: adopt general industry water, washing filtering is carried out to the mineral after Roasting Decomposition, and repeatedly washing leaching cake is less than 9 to the pH of water lotion;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after being decomposed by sodium carbonate roasting adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 DEG C, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and with 400mL salt acid elution filter cake, obtains hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get 100g acid leaching residue, add 160g sodium hydroxide and 100g fused salt and mix, carry out roasting, the temperature of roasting 700 DEG C, the time is 2h;
(5) water logging: adopt general industry water, carry out water logging to the mineral after Roasting Decomposition, extraction temperature is 85 DEG C, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, filtered water is washed till pH is 7 ~ 9, obtain water lotion and washing slag, water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates about Ph to 7, under water-bath 95 DEG C, stirring 500r/min, utilizes the precipitator method to obtain white carbon black, and obtained white carbon black is filtered to washing, dries, and the rate of recovery of silicon is 93.33%.
Embodiment 3
(1) sodium carbonate roasting: get 100g Bayan Obo mine tailing, add 130g sodium hydroxide and mix, carry out roasting, the temperature of roasting 350 DEG C, the time is 2h;
(2) wash: adopt general industry water, washing filtering is carried out to the mineral after Roasting Decomposition, and repeatedly washing leaching cake is less than 9 to the pH of water lotion;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after being decomposed by sodium carbonate roasting adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 DEG C, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and with 400mL salt acid elution filter cake, obtains hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get 100g acid leaching residue, add 200g sodium hydroxide and 100g fused salt and mix, carry out roasting, the temperature of roasting 700 DEG C, the time is 2h;
(5) water logging: adopt general industry water, carry out water logging to the mineral after Roasting Decomposition, extraction temperature is 85 DEG C, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, filtered water is washed till pH is 7 ~ 9, obtain water lotion and washing slag, water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates about Ph to 7, under water-bath 95 DEG C, stirring 500r/min, utilizes the precipitator method to obtain white carbon black, and obtained white carbon black is filtered to washing, dries, and the rate of recovery of silicon is 94.26%.
Embodiment 4
(1) sodium carbonate roasting: get 100g Bayan Obo mine tailing, add 130g sodium hydroxide and mix, carry out roasting, the temperature of roasting 350 DEG C, the time is 2h;
(2) wash: adopt general industry water, washing filtering is carried out to the mineral after Roasting Decomposition, and repeatedly washing leaching cake is less than 9 to the pH of water lotion;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after being decomposed by sodium carbonate roasting adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 DEG C, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and with 400mL salt acid elution filter cake, obtains hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get 100g acid leaching residue, add 160g sodium hydroxide and 100g fused salt and mix, carry out roasting, the temperature of roasting 600 DEG C, the time is 2h;
(5) water logging: adopt general industry water, carry out water logging to the mineral after Roasting Decomposition, extraction temperature is 85 DEG C, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, filtered water is washed till pH is 7 ~ 9, obtain water lotion and washing slag, water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates about Ph to 7, under water-bath 95 DEG C, stirring 500r/min, utilizes the precipitator method to obtain white carbon black, and obtained white carbon black is filtered to washing, dries, and the rate of recovery of silicon is 78.35%.
Embodiment 5
(1) sodium carbonate roasting: get 100g Bayan Obo mine tailing, add 130g sodium hydroxide and mix, carry out roasting, the temperature of roasting 350 DEG C, the time is 2h;
(2) wash: adopt general industry water, washing filtering is carried out to the mineral after Roasting Decomposition, and repeatedly washing leaching cake is less than 9 to the pH of water lotion;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after being decomposed by sodium carbonate roasting adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 DEG C, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and with 400mL salt acid elution filter cake, obtains hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get 100g acid leaching residue, add 160g sodium hydroxide and 100g fused salt and mix, carry out roasting, the temperature of roasting 750 DEG C, the time is 2h;
(5) water logging: adopt general industry water, carry out water logging to the mineral after Roasting Decomposition, extraction temperature is 85 DEG C, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, filtered water is washed till pH is 7 ~ 9, obtain water lotion and washing slag, water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates about Ph to 7, under water-bath 95 DEG C, stirring 500r/min, utilizes the precipitator method to obtain white carbon black, and obtained white carbon black is filtered to washing, dries, and the rate of recovery of silicon is 93.85%.
Embodiment 6
(1) sodium carbonate roasting: get 100g Bayan Obo mine tailing, add 130g sodium hydroxide and mix, carry out roasting, the temperature of roasting 350 DEG C, the time is 2h;
(2) wash: adopt general industry water, washing filtering is carried out to the mineral after Roasting Decomposition, and repeatedly washing leaching cake is less than 9 to the pH of water lotion;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after being decomposed by sodium carbonate roasting adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 DEG C, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and with 400mL salt acid elution filter cake, obtains hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get 100g acid leaching residue, add 160g sodium hydroxide and 100g fused salt and mix, carry out roasting, the temperature of roasting 700 DEG C, the time is 0.5h;
(5) water logging: adopt general industry water, carry out water logging to the mineral after Roasting Decomposition, extraction temperature is 85 DEG C, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, filtered water is washed till pH is 7 ~ 9, obtain water lotion and washing slag, water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates about Ph to 7, under water-bath 95 DEG C, stirring 500r/min, utilizes the precipitator method to obtain white carbon black, and obtained white carbon black is filtered to washing, dries, and the rate of recovery of silicon is 73.24%.
Embodiment 7
(1) sodium carbonate roasting: get 100g Bayan Obo mine tailing, add 130g sodium hydroxide and mix, carry out roasting, the temperature of roasting 350 DEG C, the time is 2h;
(2) wash: adopt general industry water, washing filtering is carried out to the mineral after Roasting Decomposition, and repeatedly washing leaching cake is less than 9 to the pH of water lotion;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after being decomposed by sodium carbonate roasting adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 DEG C, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and with 400mL salt acid elution filter cake, obtains hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get 100g acid leaching residue, add 160g sodium hydroxide and 100g fused salt and mix, carry out roasting, the temperature of roasting 700 DEG C, the time is 1.5h;
(5) water logging: adopt general industry water, carry out water logging to the mineral after Roasting Decomposition, extraction temperature is 85 DEG C, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, filtered water is washed till pH is 7 ~ 9, obtain water lotion and washing slag, water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates about Ph to 7, under water-bath 95 DEG C, stirring 500r/min, utilizes the precipitator method to obtain white carbon black, and obtained white carbon black is filtered to washing, dries, and the rate of recovery of silicon is 89.65%.
Embodiment 8
(1) sodium carbonate roasting: get 100g Bayan Obo mine tailing, add 130g sodium hydroxide and mix, carry out roasting, the temperature of roasting 350 DEG C, the time is 2h;
(2) wash: adopt general industry water, washing filtering is carried out to the mineral after Roasting Decomposition, and repeatedly washing leaching cake is less than 9 to the pH of water lotion;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after being decomposed by sodium carbonate roasting adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 DEG C, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and with 400mL salt acid elution filter cake, obtains hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get 100g acid leaching residue, add 160g sodium hydroxide and 100g fused salt and mix, carry out roasting, the temperature of roasting 700 DEG C, the time is 3h;
(5) water logging: adopt general industry water, carry out water logging to the mineral after Roasting Decomposition, extraction temperature is 85 DEG C, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, filtered water is washed till pH is 7 ~ 9, obtain water lotion and washing slag, water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates about Ph to 7, under water-bath 95 DEG C, stirring 500r/min, utilizes the precipitator method to obtain white carbon black, and obtained white carbon black is filtered to washing, dries, and the rate of recovery of silicon is 94.39%.
Last it is noted that obviously, above-described embodiment is only for example of the present invention is clearly described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And thus the apparent change of amplifying out or variation be still among protection scope of the present invention.
Claims (6)
1. prepare a method for white carbon black, it is characterized in that, described method is with Bayan Obo mine tailing acid leaching residue for raw material, and concrete steps are:
(1), by grinding after Bayan Obo mine tailing mix with alkali metal hydroxide, roasting;
(2), by the tailings water after roasting be washed till neutrality, filter, obtain water lotion and washing slag, washing slag adopts Leaching in Hydrochloric Acid, filtration again, obtains leach liquor and leached mud, and leach liquor is that leached mud is acid leaching residue containing scandium solution;
(3), acid leaching residue is mixed with alkali metal hydroxide and fused salt, roasting;
(4), by the acid leaching residue after roasting stir water logging in a water bath, after water logging, filtered water is washed till screening in neutral, obtains filtrate and washing slag;
(5), under water-bath, stirring, extremely neutral with hydrochloric acid conditioning solution pH to filtrate, utilize precipitator method production of silica white, washing, oven dry are filtered to obtained white carbon black.
2. a kind of method preparing white carbon black as claimed in claim 1, is characterized in that: SiO in acid leaching residue prepared by described Bayan Obo mine tailing
2content is 500 ~ 700kg/t.
3. a kind of method preparing white carbon black as claimed in claim 1, it is characterized in that: the alkali metal hydroxide in step (1) and step (3) is the one in sodium hydroxide or potassium hydroxide, the mass ratio of mine tailing and alkali metal hydroxide is 1:1.3, maturing temperature is 350 DEG C, time is 2h, and the concentration of hydrochloric acid in step (2) and step (5) is 2 ~ 3mol/L.
4. a kind of method preparing white carbon black as claimed in claim 1, it is characterized in that: described fused salt is NaCl/KCl fused salt, NaCl/KCl in fused salt is 1:1 proportioning in mass ratio, 1:1 ~ 2:1 is baking mixed in mass ratio for acid leaching residue and alkali metal hydroxide and fused salt, maturing temperature 600 ~ 750 DEG C, roasting time 0.5 ~ 3h.
5. a kind of method preparing white carbon black as claimed in claim 1, is characterized in that: the acid leaching residue after described roasting stirs water logging, and water soaking temperature 50 ~ 95 DEG C, filters after water logging, by hot water wash screening to neutral.
6. a kind of method preparing white carbon black as claimed in claim 1, is characterized in that: described filtrate reaction water bath temperature is 50 ~ 95 DEG C, time 0.15 ~ 0.5h, stir speed (S.S.) 500r/min.
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| CN105621418B (en) * | 2015-12-31 | 2017-09-29 | 包头稀土研究院 | A kind of method for preparing Ludox |
| CN105752994A (en) * | 2016-04-29 | 2016-07-13 | 攀枝花学院 | Method for preparing white carbon black from graphite tailings |
| CN109231253A (en) * | 2018-11-09 | 2019-01-18 | 长沙万荣粉体设备科技有限公司 | A kind of native sulfate of barium method of purification and equipment |
| CN111534683A (en) * | 2020-04-13 | 2020-08-14 | 广东工业大学 | Method for enriching iron oxide in iron tailings by using alkali fusion method |
| CN114349013B (en) * | 2021-12-24 | 2023-06-20 | 江西双龙硅材料科技有限公司 | White carbon black used as toothpaste abrasive and preparation process thereof |
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| CN101942562A (en) * | 2010-04-26 | 2011-01-12 | 张夫道 | Harmless treatment technology of main metal tailings |
| CN102653820A (en) * | 2012-04-24 | 2012-09-05 | 包头稀土研究院 | Method for extracting scandium from baiyuneboite tailings |
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| CN101942562A (en) * | 2010-04-26 | 2011-01-12 | 张夫道 | Harmless treatment technology of main metal tailings |
| CN102653820A (en) * | 2012-04-24 | 2012-09-05 | 包头稀土研究院 | Method for extracting scandium from baiyuneboite tailings |
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| 熔盐法从铁尾矿中制取高纯白炭黑;于洪浩等;《化工学报》;20090831;第60卷(第8期);2125-2129 * |
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