CN102515214A - Method for reducing magnesium oxide impurity in solid magnesium chloride - Google Patents
Method for reducing magnesium oxide impurity in solid magnesium chloride Download PDFInfo
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- CN102515214A CN102515214A CN2011104412492A CN201110441249A CN102515214A CN 102515214 A CN102515214 A CN 102515214A CN 2011104412492 A CN2011104412492 A CN 2011104412492A CN 201110441249 A CN201110441249 A CN 201110441249A CN 102515214 A CN102515214 A CN 102515214A
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- magnesium chloride
- solid magnesium
- manganese dioxide
- natural manganese
- fluorochemical
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Abstract
The invention relates to the field of magnesium chloride electrolysis, and specifically to a method for reducing a magnesium oxide impurity in solid magnesium chloride. The specific method for reducing the magnesium oxide impurity in the solid magnesium chloride comprises: heating the solid magnesium chloride to form a magnesium chloride solution, wherein the heating temperature is 800-820 DEG C; adding a fluoride to the magnesium chloride solution at the temperature of 800-820 DEG C; stirring and uniformly mixing, and standing; detecting the magnesium oxide content in the magnesium chloride solution, wherein the electrolytic production requirement is met if the magnesium oxide content is less than or equal to 1%, and the addition amount of the fluoride is 1-3% of the mass of the magnesium oxide in the solid magnesium chloride. With the method of the present invention, it is ensured that the molten body of the solid magnesium chloride can meet the production requirement of the magnesium electrolyte tank; compared to the impurity removal method in the prior art, the method of the present invention has the following advantages that: the harm to the human body and the equipment is reduced, the operation is simple, and the cost is low.
Description
Technical field
The present invention relates to electrolysis of magnesium chloride field, be specifically related to a kind of method that reduces Natural manganese dioxide impurity in the solid magnesium chloride.
Background technology
The process method of industrial production Titanium Sponge 40-60 mesh at present in enormous quantities is magnesium reduction-vacuum distillation method; Its production primary process is under the protection of argon gas; At first in reactor drum, add a certain amount of liquid magnesium; Add smart titanium tetrachloride by certain material speed then and make it and reactive magnesium, the Titanium Sponge 40-60 mesh of generation is deposited on reactor bottom, and reaction finishes that final vacuum distill, cools, takes out, broken, packing is put in storage; The sub product melt magnesium chloride that produces in the reaction process then is transported to closing down magnesium electrolysis bath through vacuum ladle and passes through dc electrolysis; The liquid magnesium of output is returned to again and is used for Titanium Sponge 40-60 mesh production in the reactor drum, the chlorine of electrolysis output then produces crude titanic chloride through pipe-line transportation to chloride process or direct liquefaction is to sell outside the liquid chlorine.So closed cycle utilization can reduce the Titanium Sponge 40-60 mesh production cost greatly, reduces the environmental pollution and the wasting of resources again.
In actual production process,, then need replenish a certain amount of chlorine and magnesium because the loss of the loss of chlorine and magnesium, magnesium chloride is stable for guaranteeing production smoothing.The chlorine quality of general caustic soda enterprise production can satisfy the titanium tetrachloride production requirement fully, but the magnesium ingot that silicothermic process is produced then exists trace impurities such as silicon, manganese higher than electrolytic magnesium, directly influence the quality of Titanium Sponge 40-60 mesh, and surplus appears in the electrowinning process ability.So satisfy Titanium Sponge 40-60 mesh production through replenishing the electrolysis of magnesium chloride; Because the bad remote storage of melt magnesium chloride, transportation; Can only adopt the solid magnesium chloride to be used for electrolysis production; But because of the solid magnesium chloride store and transportation in the moisture absorption very easily, the fusing under atmospheric pressure state of the magnesium chloride solids behind the deliquescence will generate certain Natural manganese dioxide and hydrogen chloride impurity, contain the work-ing life that will directly influence current efficiency and anode, negative electrode, cell body behind the melt magnesium chloride adding electrolyzer of these two kinds of impurity.
At present for reducing the foreign matter content after the solid magnesium chloride melts; The general employing feeds a certain amount of chlorine or hydrogen chloride gas in the airtight smelting furnace; And because chlorine and hydrogen chloride gas are big to human body and equipment injury, so equipment making requires than higher, the cost input is also higher relatively.
Summary of the invention
The present invention is directed to above-mentioned defective provide a kind of low for equipment requirements, cost is low and to the method for Natural manganese dioxide impurity in the less reduction solid magnesium chloride of human injury; Guarantee that the molten magnesium chloride that adds electrolyzer satisfies (the foreign matter content requirement of molten magnesium chloride: MgO＜1%, H of electrolysis production demand
2O≤0.5%).
Technical scheme of the present invention:
The invention provides a kind of method that reduces Natural manganese dioxide impurity in the solid magnesium chloride, concrete steps are:
A adds the thermosetting magnesium chloride solution with the solid magnesium chloride, and Heating temperature is 800-820 ℃;
B adds fluorochemical in above-mentioned magnesium chloride solution under 800 ℃-820 ℃, leave standstill behind the stirring and evenly mixing;
C detects content of magnesia in the magnesium chloride solution, and content of magnesia≤1% promptly meets the electrolysis production requirement;
Wherein, the add-on of fluorochemical is the 1-3% of Natural manganese dioxide quality in the solid magnesium chloride.
Preferably, the add-on of said fluorochemical is the 1-2% of Natural manganese dioxide quality in the solid magnesium chloride.
Preferred, the add-on of said fluorochemical be in the solid magnesium chloride Natural manganese dioxide quality 1.5%.
Preferably, said fluorochemical is selected from MgF
2, LiF, NaF, CaF
2In at least a
Preferred, said fluorochemical is a Calcium Fluoride (Fluorspan).
Preferably, the composition of Calcium Fluoride (Fluorspan) is: CaF
2>=94%, SO
4 2-＜0.01%, CaCO
3＜0.5%, SiO
2＜0.5%, H
2O≤0.5%.
Preferably, in the aforesaid method, leave standstill more than the 0.5h behind the stirring and evenly mixing in the B step.
Preferably, in the aforesaid method, adopt the limit to add the mode of fluorochemical limit in the B step with stirring of inert gas.
Preferably, said rare gas element is an argon gas, and the composition of argon gas is: Ar
2>=99%, H
2O≤0.01%.
Beneficial effect of the present invention:
Compared with prior art, utilize the present invention to reduce the method for MgO impurity in the solid magnesium chloride, equipment need not particular requirement, common crucible or smelting furnace add dust removal installation (with add airborne dust that the fluorochemical powder causes take away remove) get final product; In addition, the stirring amount of inert gas of using among the present invention is little, in open spaces human body and environment is not had injury and pollution basically, and cost of investment is low, and is easy and simple to handle, and environment is good, and can guarantee that the molten mass of solid magnesium chloride satisfies the production demand of closing down magnesium electrolysis bath.
Embodiment
The invention provides a kind of method that reduces Natural manganese dioxide impurity in the solid magnesium chloride, concrete steps are:
A adds the thermosetting magnesium chloride solution with the solid magnesium chloride, and Heating temperature is 800-820 ℃;
B adds fluorochemical in above-mentioned magnesium chloride solution under 800 ℃-820 ℃, leave standstill behind the stirring and evenly mixing;
C detects content of magnesia in the magnesium chloride solution, and content of magnesia≤1% promptly meets the electrolysis production requirement;
Wherein, the add-on of fluorochemical is the 1-3% of Natural manganese dioxide quality in the solid magnesium chloride; If the fluorochemical add-on is excessive, reduce gradually on the contrary with the increase electrolytic cell currents efficient of fluoride concn.
Preferably, the add-on of said fluorochemical is the 1-2% of Natural manganese dioxide quality in the solid magnesium chloride.
Preferred, the add-on of said fluorochemical be in the solid magnesium chloride Natural manganese dioxide quality 1.5%; When guaranteeing impurity-eliminating effect, for the add-on of practicing thrift cost preferred fluorinated thing be in the solid magnesium chloride Natural manganese dioxide quality 1.5%.
Preferably, said fluorochemical is selected from MgF
2, LiF, NaF, CaF
2In at least a; Calcium Fluoride (Fluorspan) more preferably.
Preferably, the composition of Calcium Fluoride (Fluorspan) is: CaF
2>=94%, SO
4 2-＜0.01%, CaCO
3＜0.5%, SiO
2＜0.5%, H
2O≤0.5%; If fluoride impurities is higher, then impurity will be with MgCl
2Melt is brought into electrolyzer, influences current efficiency and increases the groove quantity of slag.
Preferably, in the aforesaid method, leave standstill more than the 0.5h behind the stirring and evenly mixing in the B step.
Preferably, in the aforesaid method, adopt the limit to add the mode of fluorochemical limit in the B step with stirring of inert gas; Feed rare gas element to quicken stirring.Amount of inert gas is rolled up and down with solution and is as the criterion during stirring, and gas vol is excessive possibly to be caused solution to splash to hurt sb.'s feelings, and the too small stirring of tolerance is uneven, and impurity-eliminating effect is not good; In addition, churning time is unsuitable long, and churning time is controlled at 2～3min/t-
MgCl2, the consumption of overlong time waste rare gas element increases cost, too short fluorochemical and the MgCl of causing easily of time
2Contact insufficiently, impurity-eliminating effect is not good.
Preferably, said rare gas element is an argon gas, and the composition of argon gas is: Ar>=99%, H
2O≤0.01%.
Among the present invention,, can prolong time of repose again, or add a certain amount of fluorochemical again, repeat B, C step in the aforesaid method if handle content of magnesia＞1% in the post chlorization magnesium solution.
MgCl in the solid magnesium chloride
2>=95%, H
2O≤5% o'clock can adopt the inventive method to reduce content of magnesia wherein, makes it reach electrolyzer the foreign matter content of molten magnesium chloride is required: MgO＜1%, H
2O≤0.5%.Adopt the inventive method also can reduce MgCl
2＜95%, H
2The molten mass foreign matter content of the solid magnesium chloride of O＞5%, but because moisture is too high, and the impurity that produces after the fusion is too much, it is big to generate the quantity of slag, and cost is high, is unfavorable for electrolysis production, therefore, does not advise adopting this method to be used for the production of electrolytic magnesium.
Fluorochemical is removed the mechanism of MgO impurity among the present invention:
MgO+4F
-＝MgF
2- 4+O
2-；
MgO+F
-＝MgOF
--。
Prior art is in sealed furnace, to feed chlorine or hydrogen chloride gas reduces MgO impurity in the solid magnesium chloride; Adopt the method for Natural manganese dioxide impurity in chlorine or the hydrogen chloride gas chlorination melt magnesium chloride; Require gas transmission pipeline and smelting furnace that extremely strong erosion resistance is arranged; Therefore pipeline and equipment performance are required high, and because the chlorine or the hydrogenchloride that use belong to toxic gas, in case take place to leak will to manipulation fields in one's power periphery cause toxicity damage among environmental pollution or the personnel.Method of the present invention need not particular requirement to equipment, common crucible or smelting furnace add dust removal installation (with add airborne dust that the fluorochemical powder causes take away remove) get final product; In addition, the stirring argon gas amount of using among the present invention is little, in open spaces human body and environment is not had injury and pollution basically, and cost of investment is low, and is easy and simple to handle, and environment is good, and can guarantee that the molten mass of solid magnesium chloride satisfies the production demand of closing down magnesium electrolysis bath.
Through embodiment the present invention is specifically described below; It is important to point out that embodiment only is used for further specifying of the present invention; Can not be interpreted as the restriction to protection domain of the present invention, these those skilled in the art can make some nonessential improvement and adjustment according to the present invention.
Embodiment 1
3 tons of solid magnesium chlorides are added fusing under 800 ℃ in 3.5 tons of crucible furnaces, treat that the solid material melts the back sampling analysis fully, recording MgO content is 3.16%, adds 1kg CaF down at 800 ℃ then
2Powder (CaF
2CaF in the powder
2Content is 95.15%, CaF
2Additional proportion is by 1% of the MgO quality), stir with argon gas while adding, churning time is 8min, the argon gas amount is rolled up and down not splash with feed liquid and is advisable, after leave standstill 30min, sampling detects MgO content in the melt, MgO content is 1.47%; After leaving standstill 60min, sampling detects MgO content in the melt, and detecting the back value is 1.01%; After leaving standstill 90min, MgO content is 0.85% in the sampling detection melt, meets the requirements, and can directly add electrolytic tank electrolysis.
Embodiment 2
3 tons of solid magnesium chlorides are added fusing under 800 ℃ in 3.5 tons of crucible furnaces, treat that the solid material melts the back sampling analysis fully, recording MgO content is 3.58%, adds 1.7kg CaF down at 800 ℃ then
2Powder (CaF
2CaF in the powder
2Content is 95.15%, CaF
2Additional proportion is by 1.5% of the MgO quality), stir with argon gas while adding, churning time is 8min, the argon gas amount is rolled up and down not splash with feed liquid and is advisable, after leave standstill 30min, sampling detects MgO content in the melt, MgO content is 1.0%; After leaving standstill 60min, sampling detects MgO content in the melt, and detecting the back value is 0.68%; After leaving standstill 90min, MgO content is 0.55% in the sampling detection melt; Leave standstill 120min, MgO content is 0.54%.
Embodiment 3
3 tons of solid magnesium chlorides are added fusing under 800 ℃ in 3.5 tons of crucible furnaces, treat that the solid material melts the back sampling analysis fully, recording MgO content is 3.58%, adds 2.2kg CaF down at 800 ℃ then
2Powder (CaF
2CaF in the powder
2Content is 95.15%, CaF
2Additional proportion is by 2% of the MgO quality), stir with argon gas while adding, churning time is 8min, the argon gas amount is rolled up and down not splash with feed liquid and is advisable, after leave standstill 30min, sampling detects MgO content in the melt, MgO content is 0.98%; After leaving standstill 60min, sampling detects MgO content in the melt, and detecting the back value is 0.68%; After leaving standstill 90min, MgO content is 0.53% in the sampling detection melt; Leave standstill 120min, MgO content is 0.53%.
Embodiment 4
3 tons of solid magnesium chlorides are added fusing under 800 ℃ in 3.5 tons of crucible furnaces, treat that the solid material melts the back sampling analysis fully, recording MgO content is 3.63%, adds 2.5kg CaF down at 800 ℃ then
2Powder (CaF
2CaF in the powder
2Content is 95.15%, CaF
2Additional proportion is by 2.2% of the MgO quality), stir with argon gas while adding, churning time is 8min, the argon gas amount is rolled up and down not splash with feed liquid and is advisable, after leave standstill 30min, sampling detects MgO content in the melt, MgO content is 1.02%; After leaving standstill 60min, sampling detects MgO content in the melt, and detecting the back value is 0.71%; After leaving standstill 90min, MgO content is 0.56% in the sampling detection melt; Leave standstill 120min, MgO content is 0.55%.
Embodiment 5
3 tons of solid magnesium chlorides are added fusing under 800 ℃ in 3.5 tons of crucible furnaces, treat that the solid material melts the back sampling analysis fully, recording MgO content is 3.68%, adds 3.3kg CaF down at 800 ℃ then
2Powder (CaF
2CaF in the powder
2Content is 95.15%, CaF
2Additional proportion is by 3% of the MgO quality), stir with argon gas while adding, churning time is 8min, the argon gas amount is rolled up and down not splash with feed liquid and is advisable, after leave standstill 30min, sampling detects MgO content in the melt, MgO content is 1%; After leaving standstill 60min, sampling detects MgO content in the melt, and detecting the back value is 0.69%; After leaving standstill 90min, MgO content is 0.55% in the sampling detection melt; Leave standstill 120min, MgO content is 0.55%.
Embodiment 6
The melt material that " embodiment 1 " is handled extract 1.5t add the 1# electrolyzer (before reinforced in the sampling analysis ionogen each component and Calcium Fluoride (Fluorspan) concentration all within specialized range; Current efficiency is 81%), behind the 1h, recording this cell current efficient is 81%; Behind the 2h, recording this cell current efficient is 81%;
The melt material that " embodiment 2 " are handled extract 1.5t add the 3# electrolyzer (before reinforced in the sampling analysis ionogen each component and Calcium Fluoride (Fluorspan) concentration all within specialized range; Current efficiency is 82%); Behind the 1h; Recording this cell current efficient is 82.2%, and behind the 2h, recording this cell current efficient is 82.6%;
The melt material that " embodiment 3 " are handled extract 1.5t add the 5# electrolyzer (before reinforced in the sampling analysis ionogen each component and Calcium Fluoride (Fluorspan) concentration all within specialized range; Current efficiency is 80%); Behind the 1h; Recording this cell current efficient is 80.3%, and behind the 2h, recording this cell current efficient is 80.5%;
The melt material that " embodiment 4 " are handled extract 1.5t add the 7# electrolyzer (before reinforced in the sampling analysis ionogen each component and Calcium Fluoride (Fluorspan) concentration all within specialized range; Current efficiency is 82%), behind the 1h, record this cell current efficient and become 82%; Behind the 2h, recording this cell current efficient is 82%;
The melt material that " embodiment 5 " are handled extract 1.5t add the 8# electrolyzer (before reinforced in the sampling analysis ionogen each component and Calcium Fluoride (Fluorspan) concentration all within specialized range; Current efficiency is 82%); Behind the 1h, record this cell current efficient and become 81.2%, behind the 2h; Record this cell current efficient reduce to 80.9% (show when the fluorochemical addition be in the magnesium chloride content of magnesia 3% the time, its current efficiency descends on the contrary); Again add 1.5t titanium sponge reduction output sub product melt magnesium chloride (not fluorinated calcium) to this groove, behind the 1h, record this cell current efficient and become 81%, behind the 2h, record this cell current efficient and reduce to 81.4%.
Claims (10)
1. reduce the method for Natural manganese dioxide impurity in the solid magnesium chloride, concrete steps are:
A adds the thermosetting magnesium chloride solution with the solid magnesium chloride, and Heating temperature is 800-820 ℃;
B adds fluorochemical in above-mentioned magnesium chloride solution under 800 ℃-820 ℃, leave standstill behind the stirring and evenly mixing;
C detects content of magnesia in the magnesium chloride solution, and content of magnesia≤1% promptly meets the electrolysis production requirement;
Wherein, the add-on of fluorochemical is the 1-3% of Natural manganese dioxide quality in the solid magnesium chloride.
2. the method for Natural manganese dioxide impurity is characterized in that in the reduction solid magnesium chloride according to claim 1, and the add-on of said fluorochemical is the 1-2% of Natural manganese dioxide quality in the solid magnesium chloride.
3. the method for Natural manganese dioxide impurity is characterized in that in the reduction solid magnesium chloride according to claim 2, the add-on of said fluorochemical be in the solid magnesium chloride Natural manganese dioxide quality 1.5%.
4. according to the method for Natural manganese dioxide impurity in each described reduction solid magnesium chloride of claim 1-3, it is characterized in that said fluorochemical is that fluorochemical is selected from MgF
2, LiF, NaF, CaF
2In at least a.
5. the method for Natural manganese dioxide impurity is characterized in that in the reduction solid magnesium chloride according to claim 4, and said fluorochemical is CaF2.
6. the method for Natural manganese dioxide impurity is characterized in that the composition of Calcium Fluoride (Fluorspan) is: CaF in the reduction solid magnesium chloride according to claim 5
2>=94%, SO
4 2-＜0.01%, CaCO
3＜0.5%, SiO
2＜0.5%, H
2O≤0.5%.
7. according to the method for Natural manganese dioxide impurity in each described reduction solid magnesium chloride of claim 1-6, it is characterized in that, leave standstill more than the 0.5h behind the stirring and evenly mixing in the said B step.
8. according to the method for Natural manganese dioxide impurity in each described reduction solid magnesium chloride of claim 1-7, it is characterized in that, adopt the limit to add the mode of fluorochemical limit in the B step with stirring of inert gas.
9. the method for Natural manganese dioxide impurity is characterized in that in the reduction solid magnesium chloride according to claim 8, and said rare gas element is an argon gas.
10. the method for Natural manganese dioxide impurity is characterized in that the composition of said argon gas is: Ar>=99%, H in the reduction solid magnesium chloride according to claim 9
2O≤0.01%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104412492A CN102515214A (en) | 2011-12-26 | 2011-12-26 | Method for reducing magnesium oxide impurity in solid magnesium chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104412492A CN102515214A (en) | 2011-12-26 | 2011-12-26 | Method for reducing magnesium oxide impurity in solid magnesium chloride |
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|---|---|
| CN102515214A true CN102515214A (en) | 2012-06-27 |
Family
ID=46286366
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|---|---|---|---|
| CN2011104412492A Pending CN102515214A (en) | 2011-12-26 | 2011-12-26 | Method for reducing magnesium oxide impurity in solid magnesium chloride |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107217144A (en) * | 2017-06-20 | 2017-09-29 | 东方弗瑞德（北京）科技有限公司 | Magnesium and magnesium ingot purification technique are distilled during a kind of titanium sponge production |
| CN107557812A (en) * | 2017-08-28 | 2018-01-09 | 攀钢集团研究院有限公司 | A kind of method for extending closing down magnesium electrolysis bath service life |
| CN107587163A (en) * | 2017-09-21 | 2018-01-16 | 攀钢集团研究院有限公司 | A kind of method for reducing magnesium eletrolysis impurity content in melt magnesium chloride |
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|---|---|---|---|---|
| CN1736872A (en) * | 2005-07-29 | 2006-02-22 | 华东理工大学 | Bischofite dehydration-electrolysis method for refining magnesian |
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2011
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1736872A (en) * | 2005-07-29 | 2006-02-22 | 华东理工大学 | Bischofite dehydration-electrolysis method for refining magnesian |
Non-Patent Citations (1)
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|---|
| 张文成等: "镁的精炼方法", 《轻金属》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107217144A (en) * | 2017-06-20 | 2017-09-29 | 东方弗瑞德（北京）科技有限公司 | Magnesium and magnesium ingot purification technique are distilled during a kind of titanium sponge production |
| CN107557812A (en) * | 2017-08-28 | 2018-01-09 | 攀钢集团研究院有限公司 | A kind of method for extending closing down magnesium electrolysis bath service life |
| CN107557812B (en) * | 2017-08-28 | 2019-09-17 | 攀钢集团研究院有限公司 | A method of extending closing down magnesium electrolysis bath service life |
| CN107587163A (en) * | 2017-09-21 | 2018-01-16 | 攀钢集团研究院有限公司 | A kind of method for reducing magnesium eletrolysis impurity content in melt magnesium chloride |
| CN107587163B (en) * | 2017-09-21 | 2019-05-24 | 攀钢集团研究院有限公司 | A method of reducing magnesium eletrolysis impurity content in melt magnesium chloride |
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Application publication date: 20120627 |