CN104649328B - Method of preparing ferric vanadate from residue of aluminum powder vanadium removal of crude titanium tetrachloride - Google Patents
Method of preparing ferric vanadate from residue of aluminum powder vanadium removal of crude titanium tetrachloride Download PDFInfo
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- CN104649328B CN104649328B CN201310589820.4A CN201310589820A CN104649328B CN 104649328 B CN104649328 B CN 104649328B CN 201310589820 A CN201310589820 A CN 201310589820A CN 104649328 B CN104649328 B CN 104649328B
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Abstract
The invention relates to a method of recycling vanadium and preparing ferric vanadate from a residue of aluminum powder vanadium removal of crude titanium tetrachloride. The method includes following main steps: (1) performing oxidizing leaching to the residue of the aluminum powder vanadium removal of the crude titanium tetrachloride in hydrochloric acid, and performing liquid-solid separation to the leached substance to respectively obtain titanium residue and a leaching solution; (2) regulating the pH value of the leaching solution to precipitate-out ferric vanadate, and separating and drying the ferric vanadate to obtain the ferric vanadate product, in which the content of vanadium is higher than 20%; (3) further regulating the pH value of a mother liquid after the precipitation of the ferric vanadate to form hydroxide precipitations from iron, aluminum, calcium, magnesium in the mother liquid; (4) evaporating a waste water to recycle chlorides while a secondary steam condensate water is circulated and utilized. In the invention, the valuable ferric vanadate is prepared by recycling the vanadium and meanwhile innocent treatment of the residue of the aluminum powder vanadium removal of the crude titanium tetrachloride is achieved. The titanium residue and the hydroxide precipitations are in conformity with a requirement of permanent stack of common industrial solid wastes.
Description
Technical field
The present invention relates to a kind of hydrometallurgy or solid waste substance treating method, more particularly, to remove from crude titanic chloride aluminium powder
Vanadium the method preparing alkali metal ferric vandate is reclaimed in vanadium slag.
Background technology
Crude titanic chloride aluminium powder removes vanadium slag and uses aluminium powder to remove slag produced by vanadium for the crude titanic chloride that chloridising produces, and is
TiCl4One of production process typical solid discarded object.V in chloride processes, in titanium slag2O5It is chlorinated generation VOCl3.When
After adding aluminium powder in crude titanic chloride, titanium tetrachloride can be reacted with aluminium powder and produce TiCl3, produce after wherein aluminium is oxidized
Alchlor can play be catalyzed this reaction effect.TiCl3Get final product and VOCl3React generation precipitation VOCl2, thus real
The removing of existing vanadium, fundamental reaction formula is as follows：
Aluminum reduction TiCl4：
TiCl3Except vanadium：VOCl3(l)+TiCl3(l)→VOCl2(s)+TiCl4(l)
The VOCl generating2The impurity being produced with other distillations, rectifying is separated in the form of the residue of bottom, due to residual
Most TiCl is also contained in slag4, TiCl need to be evaporated using evaporating concentrating method recycling4Remaining residue is afterwards
VOCl2And other solid impurity, this slag i.e. referred to as crude titanic chloride aluminium powder is except vanadium slag.
Crude titanic chloride aluminium powder removes simple substance content of vanadium in vanadium slag and is about 3%～6%, has higher recovery value.Meanwhile,
Crude titanic chloride aluminium powder removes in vanadium slag and contains substantial amounts of chlorion, easily discharges harmful gas such as hydrogen chloride during storing up
Body, environmental pollution is serious.
Remove the comprehensive utilization of vanadium slag currently for crude titanic chloride aluminium powder both at home and abroad there is not yet laboratory research, industrialization
The documentation ＆ info report of test or industrial applications.
Content of the invention
It is an object of the invention to provide a kind of remove, from crude titanic chloride aluminium powder, the method preparing ferric vandate in vanadium slag.This
Bright reclaim vanadium be obtained use value ferric vandate while achieve crude titanic chloride aluminium powder remove vanadium slag harmless treatment,
Titanium slag therein and hydroxide precipitation meet the permanent requirement stacked of general industry solid waste.
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that：
A kind of removing in vanadium slag from crude titanic chloride aluminium powder prepares the method for ferric vandate, comprises the following steps：
(1) crude titanic chloride aluminium powder is removed vanadium slag and mixed in hydrochloric acid, and add oxidant to carry out Oxidation Leaching, after leaching
Slurry obtains filter cake and acid leaching solution after filtering；
(2) add alkaline matter regulation pH value to acidity to carry out ferric vandate in the acid leaching solution obtaining to step (1) to sink
Form sediment and react, after filtration, obtain ferric vandate and deposition vanadium mother liquid.The program has been obtained valuable ferric vandate using solid waste, is one
Plant the effective processing method of waste resource.
As optimal technical scheme, method of the present invention comprises the following steps：
(1) crude titanic chloride aluminium powder is removed vanadium slag and mixed in hydrochloric acid, and add oxidant to carry out Oxidation Leaching, after leaching
Slurry obtains filter cake and acid leaching solution after filtering；
(2) add alkaline matter regulation pH value to acidity to carry out ferric vandate in the acid leaching solution obtaining to step (1) to sink
Form sediment and react, after filtration, respectively obtain ferric vandate and deposition vanadium mother liquid；
(3) add and step (2) identical alkaline matter in the deposition vanadium mother liquid obtaining to step (2), regulation pH value to 5～
8 make metal cation, and such as iron, aluminium, calcium, magnesium etc. form hydroxide precipitation, are precipitated thing and vanadium wastewater after filtration；Obtain
Hydroxide precipitation meet the permanent requirement stacked of general industry solid waste；
(4) vanadium wastewater that step (3) obtains is evaporated, and separates out villaumite, after separating, obtain villaumite and evaporation concentrated solution,
Evaporation concentrated solution is in this step inner loop.The program both can be obtained valuable ferric vandate, so that emission is conformed to again
Ask, decrease the pollution of environment.
As optimal technical scheme, the method for the invention comprises the following steps：
(1) by crude titanic chloride aluminium powder except the cleaning solution that vanadium slag is obtained with hydrochloric acid and step (3) mixes, and add oxidant
Carry out Oxidation Leaching, the slurry after leaching obtains filter cake and acid leaching solution after filtering；
(2) add alkaline matter regulation pH value to acidity to carry out ferric vandate in the acid leaching solution obtaining to step (1) to sink
Form sediment and react, after filtration, obtain ferric vandate and deposition vanadium mother liquid；
(3) filter cake that step (1) is obtained carries out multi-stage countercurrent washing, obtains cleaning solution and titanium slag, and wherein cleaning solution returns
Return step (1) to use；The titanium slag obtaining meets the permanent requirement stacked of general industry solid waste；
(4) add and step (2) identical alkaline matter in the deposition vanadium mother liquid obtaining to step (2), regulation pH value to 5～
8 make metal cation, and such as iron, aluminium, calcium, magnesium etc. form hydroxide precipitation, are precipitated thing and vanadium wastewater after filtration；Obtain
Hydroxide precipitation meet the permanent requirement stacked of general industry solid waste；
(5) vanadium wastewater that step (4) obtains is evaporated, and separates out villaumite, after separating, obtain villaumite and evaporation concentrated solution,
Wherein indirect steam condensed water return to step (3) is used for multi-stage countercurrent washing process, and evaporation concentrated solution is in this step inner loop.
The program both can be obtained valuable ferric vandate, so that emission is met the requirements again, and raw material can also be made can to recycle,
Improve the utilization rate of resource, be a kind of processing method of environmental protection and energy saving..
As optimal technical scheme, method of the present invention, HCl and crude titanic chloride in hydrochloric acid described in step (1)
The mass ratio that aluminium powder removes vanadium slag is 0.3:1～1:1, for example, 0.5:1、0.7:1、0.9:1 etc., preferably 0.3:1～0.8:1, enter
One step preferably 0.4:1～0.5:1.
Preferably, the oxidant described in step (1) is a kind or 2 in perchloric acid, sodium hypochlorite, ozone or hydrogen peroxide
Plant above mixture；The addition of described oxidant is 1-5 times of theoretical amount, for example, 1.2 times, 1.5 times, 2.2 times, 2.6
Times, 3 times, 3.5 times, 4.1 times, 4.6 times, 4.9 times etc., preferably 2 times.
Preferably, described in step (1) leach temperature be 20～90 DEG C, for example, 25 DEG C, 30 DEG C, 45 DEG C, 55 DEG C, 66
DEG C, 80 DEG C, 85 DEG C etc., preferably normal temperature～90 DEG C, further preferred normal temperature～60 DEG C；The time of described leaching be 30～
180min, preferably 30～120min, more excellent 30～90min.
As optimal technical scheme, method of the present invention, the alkaline solution described in step (2) be NaOH,
One kind or two or more mixture in sodium carbonate, calcium oxide, calcium hydroxide or ammoniacal liquor.
Preferably, the pH value described in step (2) be 1.0～4.5, for example, 1.2,1.6,1.9,2.3,2.6,2.9,
3.3rd, 3.8,4.0,4.4 etc., preferably 1.5～2.5.
As optimal technical scheme, method of the present invention, the series of countercurrent washing described in step (3) is 2～4
Level, preferably 3 grades；
Preferably, the liquid solid of described washing amasss mass ratio is 1.5:1～4:1L/kg, for example, 1.7:1L/kg、2.2:
1L/kg、2.6:1L/kg、3.0:1L/kg、3.5:1L/kg etc., preferably 1.5:1～3:1L/kg, more preferably 2:1～2.5:1L/
kg.
As optimal technical scheme, method of the present invention, described is separated into centrifugation.
Present invention achieves the recovery of valuable metal and high-valued, and so that dangerous solid waste is detoxified, have
Preferable economic benefit and the removing toxic substances of environmental benefit hazardous solid waste.Meanwhile, method of the present invention flow process is simple, operating condition
Gently, there is industrial operability.
Brief description
Fig. 1 is to remove, from crude titanic chloride aluminium powder, the technological process reclaimed vanadium in vanadium slag and prepare ferric vandate.
Specific embodiment
To further illustrate technical scheme below by specific embodiment.
Embodiment 1
Crude titanic chloride aluminium powder used removes vanadium slag composition and mass fraction is as shown in table 1.
Table 1
| V | Al | Cl | Fe | Ti | Ca | Mg |
| 1.9% | 20.3% | 31% | 8.6% | 1.8% | 0.26% | 0.28% |
The crude titanic chloride aluminium powder of above-mentioned composition is carried out Oxidation Leaching except vanadium slag is mixed with hydrochloric acid and titanium slag cleaning solution, its
The mass ratio that in middle hydrochloric acid, HCl and crude titanic chloride aluminium powder remove vanadium slag is 0.3:1, extraction temperature is 20 DEG C, and oxidant is dioxygen
Water, oxidant addition is 1 times of theoretical amount, and extraction time is 180min, and after the completion of leaching, the leaching rate of V is 97%.To leach
Slurries filtration afterwards, obtains acid leaching solution and filter cake.NaOH is added to adjust pH value to 1.5 in oxytropism leachate, molten
There is ferric vandate precipitation to produce in liquid, after filtration, respectively obtain ferric vandate and deposition vanadium mother liquid, recording V content in ferric vandate is 21.5%,
Precipitation rate is 99%.Above-mentioned filter cake is carried out 2 stage countercurrents with the indirect steam condensed water that vanadium wastewater is concentrated by evaporation generation wash,
It is 4 that the liquid solid of washing process amasss mass ratio:1, obtain cleaning solution and titanium slag after filtration, in titanium slag, Ti content is 55%, V content
For 0.5%.Add NaOH in step deposition vanadium mother liquid, adjusting pH value makes the metal cations such as iron, aluminium precipitate to 8, after filtration
Respectively obtain iron aluminum slag and vanadium wastewater.Vanadium wastewater is evaporated, and precipitated sodium chloride, respectively obtain after centrifugation villaumite with
Evaporation concentrated solution, evaporation concentrated solution is in evaporation system circulation.
Embodiment 2
Crude titanic chloride aluminium powder used removes vanadium slag composition and mass fraction is as shown in table 2.
Table 2
| V | Al | Cl | Fe | Ti | Ca | Mg |
| 1.9% | 20.3% | 31% | 8.6% | 1.8% | 0.26% | 0.28% |
The crude titanic chloride aluminium powder of above-mentioned composition is carried out Oxidation Leaching except vanadium slag is mixed with hydrochloric acid and titanium slag cleaning solution, its
The mass ratio that in middle hydrochloric acid, HCl and crude titanic chloride aluminium powder remove vanadium slag is 0.5:1, extraction temperature is normal temperature, and oxidant is ozone,
Oxidant addition is 5 times of theoretical amount, and extraction time is 120min, and after the completion of leaching, the leaching rate of V is 98%.After leaching
Slurries filtration, obtain acid leaching solution and filter cake.Sodium carbonate is added to adjust pH value to 1.8, in solution in oxytropism leachate
There is ferric vandate precipitation to produce, after filtration, respectively obtain ferric vandate and deposition vanadium mother liquid, recording V content in ferric vandate is 20.5%, precipitation
Rate is 99%.Above-mentioned filter cake is carried out 3 stage countercurrents with the indirect steam condensed water that vanadium wastewater is concentrated by evaporation generation wash, washing
It is 3 that the liquid solid of process amasss mass ratio:1, obtain cleaning solution and titanium slag after filtration, in titanium slag, Ti content is 55%, V content is
0.3%.Add sodium carbonate in step deposition vanadium mother liquid, adjusting pH value makes the metal cations such as iron, aluminium precipitate to 7, after filtration respectively
Obtain iron aluminum slag and vanadium wastewater.Vanadium wastewater is evaporated, and precipitated sodium chloride, respectively obtain villaumite and evaporation after centrifugation
Concentrate, evaporation concentrated solution is in evaporation system circulation.
Embodiment 3
Crude titanic chloride aluminium powder used removes vanadium slag composition and mass fraction is as shown in table 3.
Table 3
| V | Al | Cl | Fe | Ti | Ca | Mg |
| 1.9% | 20.3% | 31% | 8.6% | 1.8% | 0.26% | 0.28% |
The crude titanic chloride aluminium powder of above-mentioned composition is carried out Oxidation Leaching except vanadium slag is mixed with hydrochloric acid and titanium slag cleaning solution, its
The mass ratio that in middle hydrochloric acid, HCl and crude titanic chloride aluminium powder remove vanadium slag is 0.8:1, extraction temperature is 60 DEG C, and oxidant is time chlorine
Sour sodium, oxidant addition is 2 times of theoretical amount, and extraction time is 90min, and after the completion of leaching, the leaching rate of V is 98.5%.Will
Slurries filtration after leaching, obtains acid leaching solution and filter cake.Calcium oxide is added to adjust pH value to 2 in oxytropism leachate, molten
There is ferric vandate precipitation to produce in liquid, after filtration, respectively obtain ferric vandate and deposition vanadium mother liquid, recording V content in ferric vandate is 20.3%,
Precipitation rate is 99%.Above-mentioned filter cake is carried out 4 stage countercurrents with the indirect steam condensed water that vanadium wastewater is concentrated by evaporation generation wash,
It is 1.5 that the liquid solid of washing process amasss mass ratio:1, obtain cleaning solution and titanium slag after filtration, in titanium slag, Ti content contains for 53%, V
Measure as 0.3%.Add calcium oxide in step deposition vanadium mother liquid, adjusting pH value makes the metal cations such as iron, aluminium precipitate to 5, after filtration
Respectively obtain iron aluminum slag and vanadium wastewater.Vanadium wastewater is evaporated, and separates out calcium chloride, respectively obtain after centrifugation villaumite with
Evaporation concentrated solution, evaporation concentrated solution is in evaporation system circulation.
Embodiment 4
Crude titanic chloride aluminium powder used removes vanadium slag composition and mass fraction is as shown in table 4.
Table 4
| V | Al | Cl | Fe | Ti | Ca | Mg |
| 1.9% | 20.3% | 31% | 8.6% | 1.8% | 0.26% | 0.28% |
The crude titanic chloride aluminium powder of above-mentioned composition is carried out Oxidation Leaching except vanadium slag is mixed with hydrochloric acid and titanium slag cleaning solution, its
The mass ratio that in middle hydrochloric acid, HCl and crude titanic chloride aluminium powder remove vanadium slag is 1:1, extraction temperature is 90 DEG C, and oxidant is perchloric acid
Sodium, oxidant addition is 2 times of theoretical amount, and extraction time is 30min, and after the completion of leaching, the leaching rate of V is 99.5%.To soak
Slurries filtration after going out, obtains acid leaching solution and filter cake.Calcium hydroxide is added to adjust pH value to 2.5 in oxytropism leachate,
There is ferric vandate precipitation to produce in solution, respectively obtain ferric vandate and deposition vanadium mother liquid after filtration, recording V content in ferric vandate is
23.0%, precipitation rate is 99%.Above-mentioned filter cake is concentrated by evaporation, with vanadium wastewater, the indirect steam condensed water producing and carries out 3 stage countercurrents
Washing, it is 2.5 that the liquid solid of washing process amasss mass ratio:1, obtain cleaning solution and titanium slag after filtration, in titanium slag, Ti content is
53%, V content is 0.5%.Add calcium hydroxide in step deposition vanadium mother liquid, adjusting pH value makes the metal cations such as iron, aluminium sink to 5
Form sediment, after filtration, respectively obtain iron aluminum slag and vanadium wastewater.Vanadium wastewater is evaporated, and separates out calcium chloride, after centrifugation respectively
Obtain villaumite and evaporation concentrated solution, evaporation concentrated solution is in evaporation system circulation.
Embodiment 5
Crude titanic chloride aluminium powder used removes vanadium slag composition and mass fraction is as shown in table 5.
Table 5
| V | Al | Cl | Fe | Ti | Ca | Mg |
| 1.9% | 20.3% | 31% | 8.6% | 1.8% | 0.26% | 0.28% |
The crude titanic chloride aluminium powder of above-mentioned composition is carried out Oxidation Leaching except vanadium slag is mixed with hydrochloric acid and titanium slag cleaning solution, its
The mass ratio that in middle hydrochloric acid, HCl and crude titanic chloride aluminium powder remove vanadium slag is 1:1, extraction temperature is 90 DEG C, and oxidant is perchloric acid
Sodium, oxidant addition is 2 times of theoretical amount, and extraction time is 30min, and after the completion of leaching, the leaching rate of V is 99.5%.To soak
Slurries filtration after going out, obtains acid leaching solution and filter cake.Ammoniacal liquor is added to adjust pH value to 2.5 in oxytropism leachate, solution
In have ferric vandate precipitation to produce, respectively obtain ferric vandate and deposition vanadium mother liquid after filtration, recording in ferric vandate V content is 23.0%, sinks
Vanadium rate is 99%.Above-mentioned filter cake is carried out 3 stage countercurrents with the indirect steam condensed water that vanadium wastewater is concentrated by evaporation generation wash, wash
The liquid solid washing process amasss mass ratio for 2.5:1, obtain cleaning solution and titanium slag after filtration, in titanium slag, Ti content is 53%, V content
For 0.5%.Add ammoniacal liquor in step deposition vanadium mother liquid, adjusting pH value makes the metal cations such as iron, aluminium precipitate to 8, after filtration respectively
Obtain iron aluminum slag and vanadium wastewater.Vanadium wastewater is evaporated, and separates out ammonium chloride, after centrifugation, respectively obtain villaumite and evaporation
Concentrate, evaporation concentrated solution is in evaporation system circulation.
Applicant states, the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, that is, do not mean that the present invention has to rely on above-mentioned detailed
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The interpolation of the equivalence replacement to each raw material of product of the present invention and auxiliary element, selection of concrete mode etc., all fall within the present invention's
Within the scope of protection domain and disclosure.
Claims (17)
1. a kind of removing in vanadium slag from crude titanic chloride aluminium powder prepares the method for ferric vandate, comprises the following steps：
(1) crude titanic chloride aluminium powder is removed vanadium slag and mixed in hydrochloric acid, and add oxidant to carry out Oxidation Leaching, the slurry after leaching
Obtain filter cake and acid leaching solution after filtering；
(2) add alkaline matter to adjust pH value to acidity in the acid leaching solution obtaining to step (1) and carry out ferric vandate precipitation instead
Should, obtain ferric vandate and deposition vanadium mother liquid after filtration；
The mass ratio that in hydrochloric acid described in step (1), HCl and crude titanic chloride aluminium powder remove vanadium slag is 0.3:1～1:1；
The temperature leaching described in step (1) is 20～90 DEG C, and the time of described leaching is 30～180min；
Alkaline matter described in step (2) is a kind or 2 in NaOH, sodium carbonate, calcium oxide, calcium hydroxide or ammoniacal liquor
Plant above mixture.
2. method according to claim 1 is it is characterised in that the method comprising the steps of：
(1) crude titanic chloride aluminium powder is removed vanadium slag and mixed in hydrochloric acid, and add oxidant to carry out Oxidation Leaching, the slurry after leaching
Obtain filter cake and acid leaching solution after filtering；
(2) add alkaline matter to adjust pH value to acidity in the acid leaching solution obtaining to step (1) and carry out ferric vandate precipitation instead
Should, respectively obtain ferric vandate and deposition vanadium mother liquid after filtration；
(3) add and step (2) identical alkaline matter in the deposition vanadium mother liquid obtaining to step (2), adjusting pH value makes to 5～8
Metal cation precipitates, and is precipitated thing and vanadium wastewater after filtration；
(4) vanadium wastewater that step (3) obtains is evaporated, and separate out villaumite, after separating, obtain villaumite and evaporation concentrated solution, evaporation
Concentrate is in this step inner loop.
3. method according to claim 1 is it is characterised in that the method comprising the steps of：
(1) by crude titanic chloride aluminium powder except the cleaning solution that vanadium slag is obtained with hydrochloric acid and step (3) mixes, and oxidant is added to carry out
Oxidation Leaching, the slurry after leaching obtains filter cake and acid leaching solution after filtering；
(2) add alkaline matter to adjust pH value to acidity in the acid leaching solution obtaining to step (1) and carry out ferric vandate precipitation instead
Should, obtain ferric vandate and deposition vanadium mother liquid after filtration；
(3) filter cake that step (1) is obtained carries out multi-stage countercurrent washing, obtains cleaning solution and titanium slag, and wherein cleaning solution returns step
Suddenly (1) uses；
(4) add and step (2) identical alkaline matter in the deposition vanadium mother liquid obtaining to step (2), adjusting pH value makes to 5～8
Metal cation precipitates, and is precipitated thing and vanadium wastewater after filtration；
(5) vanadium wastewater that step (4) obtains is evaporated, and separate out villaumite, after separating, obtain villaumite and evaporation concentrated solution, wherein
Indirect steam condensed water return to step (3) is used for multi-stage countercurrent washing process, and evaporation concentrated solution is in this step inner loop.
4. method according to claim 1 is it is characterised in that HCl and crude titanic chloride aluminium in hydrochloric acid described in step (1)
The mass ratio that powder removes vanadium slag is 0.3:1～0.8:1.
5. method according to claim 4 is it is characterised in that HCl and crude titanic chloride aluminium in hydrochloric acid described in step (1)
The mass ratio that powder removes vanadium slag is 0.4:1～0.5:1.
6. method according to claim 1 is it is characterised in that the oxidant described in step (1) is perchloric acid, hypochlorous acid
One kind or two or more mixture in sodium, ozone or hydrogen peroxide；The addition of described oxidant is 1-5 times of theoretical amount.
7. method according to claim 6 is it is characterised in that the addition of oxidant described in step (1) is theoretical amount
2 times.
8. method according to claim 1 it is characterised in that described in step (1) leach temperature be normal temperature～90 DEG C,
The time of described leaching is 30～120min.
9. method according to claim 8 is it is characterised in that the temperature leaching described in step (1) is normal temperature～60 DEG C；
The time of described leaching is 30～90min.
10. method according to claim 1 is it is characterised in that the pH value described in step (2) is 1.0～4.5.
11. methods according to claim 10 are it is characterised in that the pH value described in step (2) is 1.5～2.5.
12. methods according to claim 3 are it is characterised in that the series of countercurrent washing described in step (3) is 2～4
Level.
13. methods according to claim 12 are it is characterised in that the series of countercurrent washing described in step (3) is 3 grades.
14. methods according to claim 3 are it is characterised in that the long-pending mass ratio of the liquid solid of washing described in step (3) is
1.5:1～4:1L/kg.
15. methods according to claim 14 are it is characterised in that the liquid solid of washing described in step (3) amasss mass ratio
For 1.5:1～3:1L/kg.
16. methods according to claim 15 are it is characterised in that the liquid solid of washing described in step (3) amasss mass ratio
For 2:1～2.5:1L/kg.
17. methods according to claim 1 and 2 are it is characterised in that described is separated into centrifugation.
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|---|---|
| CN104649328A (en) | 2015-05-27 |
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