CN103395792A - White carbon black preparation method - Google Patents
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Abstract
The invention discloses a white carbon black preparation method which comprises the following steps: adding alkali into baiyuneboite or tailings thereof, calcining, and washing the calcined ores, wherein the water washing solution is used for recovery of silicon, aluminum and alkali metal hydroxide; leaching the water washing slag with hydrochloric acid, wherein the leaching solution is a scandium-containing crude solution used as a raw material for further scandium extraction, and the acid leaching slag is a raw material in the invention; mixing the dried and ground acid leaching slag, alkali metal hydroxide and chlorination system molten salt according to a ratio of 1.0:(1.0-2.0):1.0, and calcining at 600-750 DEG C; and performing water immersion on the calcined acid leaching slag, then washing with water to neutral, and preparing white carbon black through a precipitation method by taking the water washing solution as a mother solution. According to the invention, the process is simple and scientific, white carbon black can be efficiently prepared from silicon leached and extracted from scandium-enriched acid leaching slag prepared from baiyuneboite or tailings thereof, the leaching rate is at least 90%, and other byproducts can be recovered in the process. Thus, the method disclosed by the invention is a method for comprehensively recovering silicon in baiyuneboite tailings.
Description
Technical field
The present invention relates to a kind of method for preparing white carbon black, belong to chemical field.
Background technology
during World War II, white carbon black starts on a large scale for industrial production, it is mainly precipitated silica, it is found that the performance that can greatly improve some material that adds of white carbon black, precipitated silica is mainly 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, the printing ink thickening material, 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 in toothpaste etc.This makes the performance study of white carbon black and practical application request amount greatly increase.
Baiyuneboite is typical intergrowth mineral, in ore deposit, not only be rich in the resources such as rare earth, iron, niobium, fluorite and scandium, also be rich in the silicon of certain content, and along with the exploitation of the resources such as rare earth, iron, and after elements scandium extracted, silicon had obtained further enrichment, and have benefited from the leaching process of scandium, make the destroyed of silicate sturcture part in mine tailing, make the extraction of silicon relatively easy, be mine tailing and extract silicon and prepare white carbon black approach is provided.The extraction work of relevant iron tailings silicon, forefathers also did a large amount of research, as patent (application number is 201110071373), studied the method that iron tailings prepares Nano carbon white, but fail for actual production always, its major cause is to fail to consider from the angle of comprehensive utilization of resources, and process costs is too high.And in the baiyuneboite iron tailings, the extraction of silicon never has any progress, 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 just are to overcome the defect of prior art, a kind of method for preparing white carbon black is provided, the simple science of technique of the present invention, the scandium enriched substance acid leaching residue that can be efficiently prepares from baiyuneboite or its mine tailing leaches and extracts silicon and prepare white carbon black, leaching yield >=90%, and can, from technique, reclaiming other byproducts, be the method for silicon in a kind of comprehensive recovery Bayan Obo mine tailing.
For addressing the above problem, the present invention adopts following technical scheme:
The invention provides a kind of method for preparing white carbon black, described method is take Bayan Obo mine tailing acid leaching residue as raw material, and concrete steps are:
(1), the Bayan Obo mine tailing after grinding with alkali metal hydroxide, mix, roasting;
(2), the tailings water after roasting is washed till to neutrality, filter, obtain water lotion and washing slag, the washing slag adopts Leaching in Hydrochloric Acid, filtration again, obtains leach liquor and leached mud, and leach liquor is for containing scandium solution, and leached mud is acid leaching residue;
(3), acid leaching residue is mixed with alkali metal hydroxide and fused salt, roasting;
(4), by the acid leaching residue after roasting in the stirred in water bath water logging, after water logging, filtered water is washed till screening and is neutral, obtains filtrate and washing slag;
(5), under water-bath, stirring, to filtrate with hydrochloric acid conditioning solution pH to neutral, utilize precipitator method production of silica white, the white carbon black that makes is filtered to washing, oven dry.
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 a kind of 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 ℃, the time is 2h, concentration of hydrochloric acid 2～3mol/L.
Fused salt of the present invention is the NaCl/KCl fused salt, and the NaCl/KCl in fused salt is the 1:1 proportioning in mass ratio, and acid leaching residue and alkali metal hydroxide and fused salt 1:1～2:1 in mass ratio are baking mixed, 600～750 ℃ of maturing temperatures, roasting time 0.5～3h.
Acid leaching residue after roasting of the present invention stirs water logging, and 50～95 ℃ of water soaking temperatures, filter after water logging, and is extremely neutral with the hot water wash screening.
Filtrate reaction water bath temperature of the present invention is 50～95 ℃, time 0.15～0.5h, stir speed (S.S.) 500r/min.
The simple science of technique of the present invention, the scandium enriched substance acid leaching residue that can be efficiently prepares from baiyuneboite or its mine tailing leaches and extracts silicon and prepare white carbon black, leaching yield >=90%, and can, from technique, reclaiming other byproducts, be the method for silicon in a kind of comprehensive recovery Bayan Obo mine tailing.
Advantage of the present invention is:
1, to have a maturing temperature low for technique of the present invention, energy consumption is little, the raw material consumption is little, and equipment requirements is low, the rate of recovery high of silicon, in the process of extracting silicon, there is no poisonous, severe corrosive γ-ray emission, can not leave over a large amount of industrial slags, the major impurity element can effectively be recycled, become Industrial products, reduce the cost in the white carbon black preparation process.
2, the baiyuneboite mine tailing acid leaching residue of the raw material of employing of the present invention for obtaining through the low-temperature bake acid treatment, silicone content is high, impurity is few, also avoided the waste of other resources when extracting silicon, cost is low, simultaneously can reclaim scandium, can also make noble metal niobium enrichment of element, have stronger industrial application value.
3, the present invention not only be suitable for baiyuneboite mine tailing acid leaching residue in silicon resource, also be suitable for the silicon resource that contains in other area, mineral deposit.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in detail, but content of the present invention not only is 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, 350 ℃ of the temperature of roasting, the time is 2h;
(2) washing: adopt the general industry water, the mineral after Roasting Decomposition carried out to washing filtering, and repeatedly washing leaching cake to the pH of water lotion less than 9;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after sodium carbonate roasting is decomposed adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 ℃, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and, with filter cake of 400mL salt acid elution, obtain hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get the 100g acid leaching residue, add 130g sodium hydroxide and 100g fused salt and mix, carry out roasting, 700 ℃ of the temperature of roasting, the time is 2h;
(5) water logging: adopt the general industry water, the mineral after Roasting Decomposition are carried out to water logging, extraction temperature is 85 ℃, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, to be washed till pH be 7～9 to filtered water, obtains water lotion and washing slag, and water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates Ph to 7 left and right, under 95 ℃ of water-baths, stirring 500r/min, utilizes the precipitator method to make white carbon black, and the white carbon black that makes is filtered to washing, oven dry, 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, 350 ℃ of the temperature of roasting, the time is 2h;
(2) washing: adopt the general industry water, the mineral after Roasting Decomposition carried out to washing filtering, and repeatedly washing leaching cake to the pH of water lotion less than 9;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after sodium carbonate roasting is decomposed adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 ℃, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and, with filter cake of 400mL salt acid elution, obtain hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get the 100g acid leaching residue, add 160g sodium hydroxide and 100g fused salt and mix, carry out roasting, 700 ℃ of the temperature of roasting, the time is 2h;
(5) water logging: adopt the general industry water, the mineral after Roasting Decomposition are carried out to water logging, extraction temperature is 85 ℃, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, to be washed till pH be 7～9 to filtered water, obtains water lotion and washing slag, and water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates Ph to 7 left and right, under 95 ℃ of water-baths, stirring 500r/min, utilizes the precipitator method to make white carbon black, and the white carbon black that makes is filtered to washing, oven dry, 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, 350 ℃ of the temperature of roasting, the time is 2h;
(2) washing: adopt the general industry water, the mineral after Roasting Decomposition carried out to washing filtering, and repeatedly washing leaching cake to the pH of water lotion less than 9;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after sodium carbonate roasting is decomposed adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 ℃, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and, with filter cake of 400mL salt acid elution, obtain hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get the 100g acid leaching residue, add 200g sodium hydroxide and 100g fused salt and mix, carry out roasting, 700 ℃ of the temperature of roasting, the time is 2h;
(5) water logging: adopt the general industry water, the mineral after Roasting Decomposition are carried out to water logging, extraction temperature is 85 ℃, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, to be washed till pH be 7～9 to filtered water, obtains water lotion and washing slag, and water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates Ph to 7 left and right, under 95 ℃ of water-baths, stirring 500r/min, utilizes the precipitator method to make white carbon black, and the white carbon black that makes is filtered to washing, oven dry, 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, 350 ℃ of the temperature of roasting, the time is 2h;
(2) washing: adopt the general industry water, the mineral after Roasting Decomposition carried out to washing filtering, and repeatedly washing leaching cake to the pH of water lotion less than 9;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after sodium carbonate roasting is decomposed adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 ℃, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and, with filter cake of 400mL salt acid elution, obtain hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get the 100g acid leaching residue, add 160g sodium hydroxide and 100g fused salt and mix, carry out roasting, 600 ℃ of the temperature of roasting, the time is 2h;
(5) water logging: adopt the general industry water, the mineral after Roasting Decomposition are carried out to water logging, extraction temperature is 85 ℃, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, to be washed till pH be 7～9 to filtered water, obtains water lotion and washing slag, and water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates Ph to 7 left and right, under 95 ℃ of water-baths, stirring 500r/min, utilizes the precipitator method to make white carbon black, and the white carbon black that makes is filtered to washing, oven dry, 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, 350 ℃ of the temperature of roasting, the time is 2h;
(2) washing: adopt the general industry water, the mineral after Roasting Decomposition carried out to washing filtering, and repeatedly washing leaching cake to the pH of water lotion less than 9;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after sodium carbonate roasting is decomposed adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 ℃, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and, with filter cake of 400mL salt acid elution, obtain hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get the 100g acid leaching residue, add 160g sodium hydroxide and 100g fused salt and mix, carry out roasting, 750 ℃ of the temperature of roasting, the time is 2h;
(5) water logging: adopt the general industry water, the mineral after Roasting Decomposition are carried out to water logging, extraction temperature is 85 ℃, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, to be washed till pH be 7～9 to filtered water, obtains water lotion and washing slag, and water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates Ph to 7 left and right, under 95 ℃ of water-baths, stirring 500r/min, utilizes the precipitator method to make white carbon black, and the white carbon black that makes is filtered to washing, oven dry, 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, 350 ℃ of the temperature of roasting, the time is 2h;
(2) washing: adopt the general industry water, the mineral after Roasting Decomposition carried out to washing filtering, and repeatedly washing leaching cake to the pH of water lotion less than 9;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after sodium carbonate roasting is decomposed adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 ℃, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and, with filter cake of 400mL salt acid elution, obtain hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get the 100g acid leaching residue, add 160g sodium hydroxide and 100g fused salt and mix, carry out roasting, 700 ℃ of the temperature of roasting, the time is 0.5h;
(5) water logging: adopt the general industry water, the mineral after Roasting Decomposition are carried out to water logging, extraction temperature is 85 ℃, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, to be washed till pH be 7～9 to filtered water, obtains water lotion and washing slag, and water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates Ph to 7 left and right, under 95 ℃ of water-baths, stirring 500r/min, utilizes the precipitator method to make white carbon black, and the white carbon black that makes is filtered to washing, oven dry, 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, 350 ℃ of the temperature of roasting, the time is 2h;
(2) washing: adopt the general industry water, the mineral after Roasting Decomposition carried out to washing filtering, and repeatedly washing leaching cake to the pH of water lotion less than 9;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after sodium carbonate roasting is decomposed adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 ℃, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and, with filter cake of 400mL salt acid elution, obtain hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get the 100g acid leaching residue, add 160g sodium hydroxide and 100g fused salt and mix, carry out roasting, 700 ℃ of the temperature of roasting, the time is 1.5h;
(5) water logging: adopt the general industry water, the mineral after Roasting Decomposition are carried out to water logging, extraction temperature is 85 ℃, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, to be washed till pH be 7～9 to filtered water, obtains water lotion and washing slag, and water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates Ph to 7 left and right, under 95 ℃ of water-baths, stirring 500r/min, utilizes the precipitator method to make white carbon black, and the white carbon black that makes is filtered to washing, oven dry, 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, 350 ℃ of the temperature of roasting, the time is 2h;
(2) washing: adopt the general industry water, the mineral after Roasting Decomposition carried out to washing filtering, and repeatedly washing leaching cake to the pH of water lotion less than 9;
(3) Leaching in Hydrochloric Acid: the baiyuneboite after sodium carbonate roasting is decomposed adopts Leaching in Hydrochloric Acid, concentration of hydrochloric acid is 3mol/L, the consumption of hydrochloric acid is 800mL, extraction temperature is 85 ℃, time 2h, slurries after Leaching in Hydrochloric Acid are filtered, and, with filter cake of 400mL salt acid elution, obtain hydrochloric acid leachate and acid leaching residue.
(4) add alkali and fused salt roasting: get the 100g acid leaching residue, add 160g sodium hydroxide and 100g fused salt and mix, carry out roasting, 700 ℃ of the temperature of roasting, the time is 3h;
(5) water logging: adopt the general industry water, the mineral after Roasting Decomposition are carried out to water logging, extraction temperature is 85 ℃, water logging time 0.25h, stir speed (S.S.) 450r/min;
(6) filter: after water logging, to be washed till pH be 7～9 to filtered water, obtains water lotion and washing slag, and water lotion is for containing sodium silicate solution;
(7) salt adding acid for adjusting pH: concentration of hydrochloric acid is 2.4mol/L, regulates Ph to 7 left and right, under 95 ℃ of water-baths, stirring 500r/min, utilizes the precipitator method to make white carbon black, and the white carbon black that makes is filtered to washing, oven dry, and the rate of recovery of silicon is 94.39%.
Finally it should be noted that: obviously, above-described embodiment is only for example of the present invention clearly is described, and is not the restriction 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 also giving all embodiments.And the apparent variation of being amplified out thus or change still are among protection scope of the present invention.
Claims (6)
1. a method for preparing white carbon black, is characterized in that, described method is take Bayan Obo mine tailing acid leaching residue as raw material, and concrete steps are:
(1), the Bayan Obo mine tailing after grinding with alkali metal hydroxide, mix, roasting;
(2), the tailings water after roasting is washed till to neutrality, filter, obtain water lotion and washing slag, the washing slag adopts Leaching in Hydrochloric Acid, filtration again, obtains leach liquor and leached mud, and leach liquor is for containing scandium solution, and leached mud is acid leaching residue;
(3), acid leaching residue is mixed with alkali metal hydroxide and fused salt, roasting;
(4), by the acid leaching residue after roasting in the stirred in water bath water logging, after water logging, filtered water is washed till screening and is neutral, obtains filtrate and washing slag;
(5), under water-bath, stirring, to filtrate with hydrochloric acid conditioning solution pH to neutral, utilize precipitator method production of silica white, the white carbon black that makes is filtered to washing, oven dry.
2. a kind of method for 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 for preparing white carbon black as claimed in claim 1, it is characterized in that: described alkali metal hydroxide is a kind of in sodium hydroxide or potassium hydroxide, the mass ratio of mine tailing and alkali metal hydroxide is 1:1.3, maturing temperature is 350 ℃, time is 2h, concentration of hydrochloric acid 2～3mol/L.
4. a kind of method for preparing white carbon black as claimed in claim 1, it is characterized in that: described fused salt is the NaCl/KCl fused salt, NaCl/KCl in fused salt is the 1:1 proportioning in mass ratio, acid leaching residue and alkali metal hydroxide and fused salt 1:1～2:1 in mass ratio are baking mixed, 600～750 ℃ of maturing temperatures, roasting time 0.5～3h.
5. as claimed in claim 1 is a kind of method for preparing white carbon black, it is characterized in that: the acid leaching residue after described roasting stirs water logging, and 50～95 ℃ of water soaking temperatures, filter after water logging, and is extremely neutral with the hot water wash screening.
6. a kind of method for preparing white carbon black as claimed in claim 1, it is characterized in that: described filtrate reaction water bath temperature is 50～95 ℃, time 0.15～0.5h, stir speed (S.S.) 500r/min.
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Cited By (5)
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| CN105621418A (en) * | 2015-12-31 | 2016-06-01 | 包头稀土研究院 | Method for preparing silica sol |
| 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 |
| CN114349013A (en) * | 2021-12-24 | 2022-04-15 | 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 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621418A (en) * | 2015-12-31 | 2016-06-01 | 包头稀土研究院 | Method for preparing silica sol |
| 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 |
| CN114349013A (en) * | 2021-12-24 | 2022-04-15 | 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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| CN103395792B (en) | 2016-03-23 |
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