CN114525404B - Method for extracting metal from lunar soil by calcium reduction method - Google Patents
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Abstract
The invention belongs to the technical field of metallurgy, and relates to a method for extracting metals from lunar soil by a calcium reduction method, which comprises the following steps: s1, uniformly mixing lunar soil and calcium metal; s2, placing the mixture in a closed reactor, heating to a reduction temperature under an argon atmosphere, preserving heat, and reacting to obtain a mixture of calcium-based alloy and calcium oxide; s3, placing the mixture of the calcium-based alloy and the calcium oxide into a reactor filled with calcium chloride molten salt, wherein the calcium-based alloy is gradually enriched at the bottom of the reactor, and the calcium oxide is dissolved in the calcium chloride molten salt; s4, taking out the calcium-based alloy from the bottom of the reactor in the step S3, and performing vacuum distillation and separation to obtain metal calcium and an aluminum-silicon-iron alloy; s5, taking copper as a cathode and graphite as an anode, and treating the residual CaCl in the reactor S3 2 And (4) electrolyzing CaO molten salt to obtain metallic calcium at a cathode. The method adopts a calcium reduction method, can extract metals such as aluminum, silicon, iron and the like in the lunar soil, and realizes the recycling of the reducing agent calcium.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and relates to a method for extracting metals from lunar soil by a calcium reduction method.
Background
The construction of a lunar base and the development of lunar resources are the main trends of the lunar exploration in the 21 st century. A permanent base for human life and work is created on the moon, so that not only can mineral resources stored in the moon be developed, and a space power station is built to utilize moon nuclear fusion raw materials and solar energy for the earth to use, but also the moon can be used as a transfer station to provide building materials and rocket propellants for the human exploration to a farther universe. People need to normally live on the moon without water and air, and it is indispensable to mine and smelt in situ soil on the surface of the moon, so that the self-sufficiency of metal, water and oxygen is realized.
The method for preparing metal by utilizing lunar soil resources in situ comprises a hydrogen reduction method, a carbothermic reduction method, a vacuum thermal decomposition method, an electrolysis method, an aluminothermic reduction-molten salt electrolysis method and the like, and the adopted raw materials mainly comprise ilmenite and lunar soil simulation samples. However, the hydrogen reduction method and the carbothermic reduction method can only extract iron in minerals, and are difficult to utilize metals such as aluminum, silicon and the like contained in lunar soil; the vacuum thermal decomposition method can only decompose the oxides contained in the lunar soil into low oxides, a very small amount of metals and oxygen, and has high energy consumption; the electrolytic method can extract metals such as aluminum, silicon, iron and the like in lunar soil, but the temperature is as high as 1600 ℃, the energy consumption is high, and the problem of anode materials is difficult to solve; the aluminothermic reduction-molten salt electrolysis method can extract metals such as aluminum, silicon, iron and the like from the lunar soil, but the lunar soil contains 10-16% of CaO, which causes the change of the components of the electrolyte, i.e. the large enrichment of calcium salt in the electrolyte, and causes the reduction of the primary crystal temperature and the current efficiency. In addition, the hydrogen reduction method, the carbothermic method and the aluminothermic reduction-molten salt electrolysis method need to convey the reducing agent from the earth, and the reducing agent is lost in the reaction process, cannot be recycled and needs to be continuously supplemented.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for extracting metals from lunar soil by a calcium reduction method, the method can efficiently utilize mixed oxides contained in the lunar soil to prepare the metals, and a reducing agent can be recycled without additional supplement.
In order to achieve the above object, the method of the present invention comprises the steps of:
s1, uniformly mixing the lunar soil and the calcium metal.
And S2, placing the mixture in a closed reactor, heating to a reduction temperature in an argon atmosphere, preserving heat, and reacting to obtain a mixture of the calcium-based alloy and the calcium oxide.
And S3, placing the mixture of the calcium-based alloy and the calcium oxide into a reactor filled with calcium chloride molten salt, gradually enriching the calcium-based alloy at the bottom of the reactor, and dissolving the calcium oxide in the calcium chloride molten salt.
And S4, taking out the calcium-based alloy from the bottom of the reactor in the step S3, and performing vacuum distillation and separation to obtain metal calcium and the aluminum-silicon-iron alloy, wherein the metal calcium is returned to the step S1 for recycling.
And S5, electrolyzing the residual fused salt containing the calcium oxide and the calcium chloride in the reactor in the step S3 by adopting an inert electrode to obtain metal calcium at a cathode, and returning the metal calcium to the step S1 for recycling.
The calcium chloride fused salt is lost due to volatilization and electrolysis, the volatilized calcium chloride can be collected, meanwhile, a part of metal calcium obtained by the cathode and chlorine generated by the anode can be made into the calcium chloride fused salt again, and the calcium chloride fused salt is returned to the step S3 for recycling.
The mass ratio of the lunar soil to the metal calcium in the step S1 is preferably 1 (1-5).
In step S2, the reduction temperature is 800-1200 ℃, and the heat preservation time is 1-5 h.
In step S3, the temperature of the calcium chloride molten salt is 825-900 ℃.
In step S4, the vacuum degree of the vacuum distillation process is 1-100 Pa, the temperature is 1000-1200 ℃, and the time is 30-50 min.
In step S5, constant-cell-pressure electrolysis is adopted for electrolysis, the voltage of the electrolytic cell is controlled to be 3.5-4.3V, the electrolysis temperature is 850-1200 ℃, and the electrolysis time is 2-4 h.
The electrolysis of step S5 uses an inert electrode, preferably copper as the cathode and graphite as the anode. Thus, after electrolysis, the copper at the copper cathode is converted into copper-calcium alloy, so that calcium generated by electrolysis is easier to separate from the molten salt. Specifically, the copper in the copper-calcium alloy can be separated from the calcium by adopting a vacuum distillation mode similar to the step S4, the copper is recycled for the cathode, and the calcium is recycled for the reduction process of the lunar soil.
The beneficial effects of the invention are:
the invention provides a method for extracting metals from lunar soil by a calcium reduction method, which can extract the metals such as aluminum, silicon, iron and the like contained in the lunar soil, and has lower reduction temperature and lower energy consumption.
The method provided by the invention can be used for treating lunar soil without mineral separation, the lunar soil and metal calcium are directly and uniformly mixed, and then the calcium reduction method is adopted to reduce Al contained in the lunar soil 2 O 3 、SiO 2 And reducing oxides such as FeO and the like to prepare the calcium-based alloy and calcium oxide, wherein the calcium oxide can be dissolved in the calcium chloride molten salt, and the calcium-based alloy can not be dissolved in the calcium chloride molten salt, so that the separation of the calcium-based alloy and the calcium oxide is realized.
The method can prepare the metal calcium by electrolyzing the calcium chloride fused salt containing the calcium oxide through the fused salt. In addition, the calcium-based alloy obtained by calcium reduction and the copper-calcium alloy obtained by molten salt electrolysis can be subjected to vacuum distillation to obtain metal calcium, aluminum-silicon-iron alloy and copper, so that the recycling of the reducing agent calcium is realized. The method system can realize long-term circulating operation of the system basically without additionally supplementing new substances, and has wide application prospects in the processes of establishing a lunar base and developing lunar resources.
Drawings
Fig. 1 is an XRD spectrum of a product of extracting metals from lunar soil by calcium reduction in example 1 of the present invention.
Detailed Description
For a better understanding of the present invention, reference will now be made in detail to the present embodiments of the invention, which are illustrated in the accompanying drawings. In the embodiment of the invention, lunar soil is simulated by adopting a lunar soil simulation sample, and the lunar soil simulation sample comprises the following chemical components in percentage by mass: 42.5% -52.47% of SiO 2 ，12.36％～25.48％Al 2 O 3 ，5.2％～15.7％FeO，10.54％～16.9％CaO，3.54％～8.35％MgO，0.54％～7.31％TiO 2 ，0.09％～0.41％K 2 O and the balance of impurities.
Example 1
S1, chemical components 42.5% by mass of SiO 2 ，23.81％Al 2 O 3 ，7.61％FeO，13.59％CaO，4.82％MgO，7.31％TiO 2 ，0.35％K 2 O, the lunar soil simulation sample and metallic calcium are mixed according to the mass ratio of 1:1, uniformly mixing;
s2, placing the mixture in a closed reactor, heating to the reduction temperature of 800 ℃ in an argon atmosphere, and keeping the temperature for 3 hours to react to obtain a mixture of calcium-based alloy and calcium oxide;
s3, placing the mixture of the calcium-based alloy and the calcium oxide into a reactor filled with calcium chloride molten salt at 840 ℃, wherein the calcium-based alloy is gradually enriched at the bottom of the reactor, and the calcium oxide is dissolved in the calcium chloride molten salt;
s4, taking the calcium-based alloy out of the bottom of the reactor in the step S3, and carrying out vacuum distillation separation for 40min at the vacuum degree of 60Pa and the temperature of 1050 ℃ to obtain metal calcium and the aluminum-silicon-iron alloy, wherein the metal calcium returns to the step S1 for recycling;
s5, taking copper as a cathode and graphite as an anode, controlling the cell voltage to be 3.6V, and treating the residual CaCl in the reactor S3 2 The CaO fused salt is electrolyzed at 1200 ℃ for 2.5h, and metal calcium is obtained at the cathode, wherein the metal calcium is returned to the step S1 for recycling;
in step S3, as shown in FIG. 1, the phase composition of the obtained calcium-based alloy is Al 86 Fe 14 ，Ca 2 The extraction rates of Si and metal elements such as aluminum, silicon, iron and the like in the lunar soil simulation sample are respectively 75.41%, 81.26% and 84.34%.
Example 2
S1, chemical components 45.66% by mass of SiO 2 ，23.21％Al 2 O 3 ，5.2％FeO，16.73％CaO，5.26％MgO，3.52％TiO 2 ，0.41％K 2 O, the lunar soil simulation sample and metallic calcium are mixed according to the mass ratio of 1:2, mixing uniformly;
s2, placing the mixture in a closed reactor, heating to the reduction temperature of 1200 ℃ in an argon atmosphere, and keeping the temperature for 1.5 hours to react to obtain a mixture of calcium-based alloy and calcium oxide;
s3, placing the mixture of the calcium-based alloy and the calcium oxide into a reactor filled with 825 ℃ calcium chloride molten salt, wherein the calcium-based alloy is gradually enriched at the bottom of the reactor, and the calcium oxide is dissolved in the calcium chloride molten salt;
s4, taking the calcium-based alloy out of the bottom of the reactor in the step S3, and carrying out vacuum distillation separation for 35min at the vacuum degree of 15Pa and the temperature of 1100 ℃ to obtain metal calcium and the aluminum-silicon-iron alloy, wherein the metal calcium is returned to the step S1 for recycling;
s5, taking copper as a cathode and graphite as an anode, controlling the voltage of the tank to be 4.3V, and treating the residual CaCl in the reactor in S3 2 The CaO fused salt is electrolyzed at the temperature of 1125 ℃ for 3.5h, and metal calcium is obtained at the cathode, wherein the metal calcium is returned to the step S1 for recycling;
in step S2, the phase composition of the obtained calcium-based alloy is Al 86 Fe 14 ，Ca 2 The extraction rates of metal elements such as aluminum, silicon, iron and the like in the lunar soil simulation sample are respectively 79.53%, 84.46% and 86.59%.
Example 3
S1, 50.24% of chemical components by mass of SiO 2 ，15.86％Al 2 O 3 ，14.72％FeO，10.54％CaO，7.94％MgO，0.54％TiO 2 ，0.15％K 2 O, lunar soil simulation sample and metallic calcium are mixed according to the mass ratio of 1:3, uniformly mixing;
s2, placing the mixture in a closed reactor, heating to a reduction temperature of 950 ℃ in an argon atmosphere, and keeping the temperature for 4 hours to react to obtain a mixture of calcium-based alloy and calcium oxide;
s3, placing the mixture of the calcium-based alloy and the calcium oxide into a reactor filled with 900 ℃ calcium chloride molten salt, wherein the calcium-based alloy is gradually enriched at the bottom of the reactor, and the calcium oxide is dissolved in the calcium chloride molten salt;
s4, taking the calcium-based alloy out of the bottom of the reactor in the step S3, and carrying out vacuum distillation separation for 30min at the temperature of 1175 ℃ under the vacuum degree of 25Pa to obtain metal calcium and the aluminum-silicon-iron alloy, wherein the metal calcium is returned to the step S1 for recycling;
s5, taking copper as a cathode, graphite as an anode, controlling the voltage of a tank to be 4V, and treating the residual CaCl in the reactor S3 2 The CaO fused salt is electrolyzed at the temperature of 975 ℃ for 2h, and metallic calcium is obtained at the cathode, wherein the metallic calcium is returned to the step S1 for recycling;
in step S2, the phase composition of the obtained calcium-based alloy is Al 86 Fe 14 ，Ca 2 The extraction rates of metal elements such as aluminum, silicon, iron and the like in the lunar soil simulation sample are 82.96%, 85.58% and 90.24% respectively.
Example 4
S1, chemical components 51.44% SiO by mass fraction 2 ，13.46％Al 2 O 3 ，12.48％FeO，12.58％CaO，8.35％MgO，1.41％TiO 2 ，0.26％K 2 O, the lunar soil simulation sample and metallic calcium are mixed according to the mass ratio of 1:2.5, mixing uniformly;
s2, placing the mixture in a closed reactor, heating to the reduction temperature of 900 ℃ in an argon atmosphere, and keeping the temperature for 5 hours to react to obtain a mixture of calcium-based alloy and calcium oxide;
s3, placing the mixture of the calcium-based alloy and the calcium oxide into a reactor filled with 870 ℃ calcium chloride molten salt, wherein the calcium-based alloy is gradually enriched at the bottom of the reactor, and the calcium oxide is dissolved in the calcium chloride molten salt;
s4, taking out the calcium-based alloy from the bottom of the reactor in the step S3, and performing vacuum distillation separation for 45min at the vacuum degree of 30Pa and the temperature of 1150 ℃ to obtain metal calcium and an aluminum-silicon-iron alloy, wherein the metal calcium returns to the step S1 for recycling;
s5, taking copper as a cathode and graphite as an anode, controlling the cell voltage to be 3.5V, and treating the residual CaCl in the reactor S3 2 The CaO fused salt is electrolyzed at 850 ℃ for 4h, and metal calcium is obtained at a cathode, wherein the metal calcium returns to the step S1 for recycling;
in step S2, the phase composition of the obtained calcium-based alloy is Al 86 Fe 14 ，Ca 2 Si, extraction of metal elements such as aluminum, silicon, iron and the like in lunar soil simulation sampleThe extraction rates were 81.19%, 91.72%, and 93.75%, respectively.
Example 5
S1, chemical components are 48.59 percent of SiO by mass fraction 2 ，12.36％Al 2 O 3 ，12.43％FeO，16.9％CaO，4.21％MgO，5.28％TiO 2 ，0.22％K 2 O, lunar soil simulation sample and metallic calcium are mixed according to the mass ratio of 1:5, uniformly mixing;
s2, placing the mixture in a closed reactor, heating to a reduction temperature of 1100 ℃ in an argon atmosphere, and keeping the temperature for 2 hours to react to obtain a mixture of calcium-based alloy and calcium oxide;
s3, placing the mixture of the calcium-based alloy and the calcium oxide into a reactor filled with 850 ℃ calcium chloride molten salt, wherein the calcium-based alloy is gradually enriched at the bottom of the reactor, and the calcium oxide is dissolved in the calcium chloride molten salt;
s4, taking the calcium-based alloy out of the bottom of the reactor in the step S3, and carrying out vacuum distillation separation for 50min at the vacuum degree of 75Pa and the temperature of 1000 ℃ to obtain metal calcium and the aluminum-silicon-iron alloy, wherein the metal calcium is returned to the step S1 for recycling;
s5, taking copper as a cathode and graphite as an anode, controlling the voltage of the tank to be 3.9V, and treating the residual CaCl in the reactor in S3 2 The CaO fused salt is electrolyzed at 1050 ℃ for 3h to obtain metallic calcium at the cathode, wherein the metallic calcium is returned to the step S1 for recycling;
in step S2, the phase composition of the obtained calcium-based alloy is Al 86 Fe 14 ，Ca 2 The extraction rates of metal elements such as aluminum, silicon, iron and the like in the Si and lunar soil simulation sample are respectively 84.13%, 91.94% and 92.45%.
Example 6
S1, chemical composition 43.27% SiO by mass fraction 2 ，25.48％Al 2 O 3 ，9.05％FeO，14.93％CaO，3.54％MgO，3.56％TiO 2 ，0.16％K 2 O, the lunar soil simulation sample and metallic calcium are mixed according to the mass ratio of 1:3.5, mixing uniformly;
s2, placing the mixture in a closed reactor, heating to the reduction temperature of 1000 ℃ in an argon atmosphere, and keeping the temperature for 4.5 hours to react to obtain a mixture of calcium-based alloy and calcium oxide;
s3, placing the mixture of the calcium-based alloy and the calcium oxide into a reactor filled with 880 ℃ calcium chloride molten salt, wherein the calcium-based alloy is gradually enriched at the bottom of the reactor, and the calcium oxide is dissolved in the calcium chloride molten salt;
s4, taking the calcium-based alloy out of the bottom of the reactor in the step S3, and carrying out vacuum distillation and separation for 33min at the vacuum degree of 1Pa and the temperature of 1125 ℃ to obtain metal calcium and the ferro-silicon-aluminum alloy, wherein the metal calcium is returned to the step S1 for recycling;
s5, taking copper as a cathode and graphite as an anode, controlling the cell voltage to be 4.2V, and treating the residual CaCl in the reactor S3 2 The CaO fused salt is electrolyzed at 1100 ℃ for 2.25h, and metallic calcium is obtained at the cathode, wherein the metallic calcium is returned to the step S1 for recycling;
in step S2, the phase composition of the obtained calcium-based alloy is Al 86 Fe 14 ，Ca 2 The extraction rates of metal elements such as aluminum, silicon, iron and the like in the lunar soil simulation sample are 83.79%, 90.28% and 93.46% respectively.
Example 7
S1, chemical components 46.82% by mass of SiO 2 ，17.05％Al 2 O 3 ，15.7％FeO，12.43％CaO，6.18％MgO，1.71％TiO 2 ，0.09％K 2 O, the lunar soil simulation sample and metallic calcium are mixed according to the mass ratio of 1:4, mixing uniformly;
s2, placing the mixture in a closed reactor, heating to a reduction temperature of 850 ℃ in an argon atmosphere, and keeping the temperature for 1h to react to obtain a mixture of calcium-based alloy and calcium oxide;
s3, placing the mixture of the calcium-based alloy and the calcium oxide into a reactor filled with calcium chloride molten salt at 860 ℃, wherein the calcium-based alloy is gradually enriched at the bottom of the reactor, and the calcium oxide is dissolved in the calcium chloride molten salt;
s4, taking the calcium-based alloy out of the bottom of the reactor in the step S3, and carrying out vacuum distillation separation for 47min at the vacuum degree of 45Pa and the temperature of 1200 ℃ to obtain metal calcium and the aluminum-silicon-iron alloy, wherein the metal calcium is returned to the step S1 for recycling;
s5, taking copper as a cathode and using stoneInk as anode, cell voltage 4.1V, remaining CaCl of the reactor for S3 2 Electrolyzing CaO molten salt at 1175 ℃ for 3.25h to obtain metallic calcium at a cathode, wherein the metallic calcium is returned to the step S1 for recycling;
in step S2, the phase composition of the obtained calcium-based alloy is Al 86 Fe 14 ，Ca 2 The extraction rates of Si and metal elements such as aluminum, silicon, iron and the like in the lunar soil simulation sample are 81.42%, 91.02% and 91.32% respectively.
Example 8
S1, 52.47% SiO of chemical components by mass fraction 2 ，14.53％Al 2 O 3 ，10.62％FeO，11.97％CaO，5.83％MgO，4.32％TiO 2 ，0.24％K 2 O, the lunar soil simulation sample and metallic calcium are mixed according to the mass ratio of 1:1.5, mixing uniformly;
s2, placing the mixture in a closed reactor, heating to a reduction temperature of 1050 ℃ in an argon atmosphere, and keeping the temperature for 2.5 hours to react to obtain a mixture of calcium-based alloy and calcium oxide;
s3, placing the mixture of the calcium-based alloy and calcium oxide into a reactor filled with 890 ℃ calcium chloride molten salt, wherein the calcium-based alloy is gradually enriched at the bottom of the reactor, and the calcium oxide is dissolved in the calcium chloride molten salt;
s4, taking the calcium-based alloy out of the bottom of the reactor in the step S3, and carrying out vacuum distillation separation for 43min at the vacuum degree of 100Pa and the temperature of 1075 ℃ to obtain metal calcium and the ferro-silicon-aluminum alloy, wherein the metal calcium is returned to the step S1 for recycling;
s5, taking copper as a cathode and graphite as an anode, controlling the voltage of the tank to be 3.8V, and treating the residual CaCl in the reactor in S3 2 The CaO fused salt is electrolyzed at 900 ℃ for 3.75h, and metal calcium is obtained at the cathode, wherein the metal calcium is returned to the step S1 for recycling;
in step S2, the phase composition of the obtained calcium-based alloy is Al 86 Fe 14 ，Ca 2 The extraction rates of metal elements such as aluminum, silicon, iron and the like in the lunar soil simulation sample are respectively 80.74%, 88.52% and 89.13%.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art can change or modify the technical content disclosed above into an equivalent embodiment with equivalent changes. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (9)
1. A method for extracting metals from lunar soil by a calcium reduction method is characterized by comprising the following steps:
s1, uniformly mixing lunar soil and calcium metal;
s2, placing the mixture in a closed reactor, heating to a reduction temperature in an argon atmosphere, preserving heat, and reacting to obtain a mixture of calcium-based alloy and calcium oxide;
s3, placing the mixture of the calcium-based alloy and the calcium oxide into a reactor filled with calcium chloride molten salt, gradually enriching the calcium-based alloy at the bottom of the reactor, and dissolving the calcium oxide in the calcium chloride molten salt;
s4, taking out the calcium-based alloy from the bottom of the reactor in the step S3, and carrying out vacuum distillation and separation to obtain metal calcium and the aluminum-silicon-iron alloy, wherein the metal calcium is returned to the step S1 for recycling;
and S5, electrolyzing the residual fused salt containing calcium oxide and calcium chloride in the reactor in the step S3 by adopting an inert electrode to obtain metal calcium at a cathode, and returning the metal calcium to the step S1 for recycling.
2. The method for extracting metals from lunar soil by calcium reduction according to claim 1, wherein the mass ratio of lunar soil to metallic calcium in step S1 is 1 (1-5).
3. The method for extracting metals from lunar soil by calcium reduction according to claim 1, wherein in the step S2, the reduction temperature is 800-1200 ℃, and the heat preservation time is 1-5 h.
4. The method for extracting metals from lunar soil by calcium reduction according to claim 1, wherein the temperature of the calcium chloride molten salt in the step S3 is 825-900 ℃.
5. The method for extracting metals from lunar soil by calcium reduction according to claim 1, wherein in the step S4, the vacuum degree of the vacuum distillation process is 1-100 Pa, the temperature is 1000-1200 ℃, and the time is 30-50 min.
6. The method for extracting metal from lunar soil by calcium reduction according to claim 1, wherein in the step S5, the voltage of an electrolytic bath in the electrolysis process is 3.5-4.3V, the electrolysis temperature is 850-1200 ℃, and the electrolysis time is 2-4 h.
7. The method for extracting metals from lunar soil by calcium reduction according to claim 1, wherein the cathode used in electrolysis is copper in the step S5.
8. The calcium reduction method for extracting metals from lunar soil according to claim 7, wherein the electrolysis obtains copper calcium alloy at the cathode, and the copper calcium alloy is separated by vacuum distillation to obtain metal calcium.
9. The method for extracting metals from lunar soil by calcium reduction according to claim 1, wherein the anode used for electrolysis is graphite in the step S5.
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