CN105132936B - One kind prepares CaTiO with fused salt electrolysis process from ilmenite3The method of powder - Google Patents
One kind prepares CaTiO with fused salt electrolysis process from ilmenite3The method of powder Download PDFInfo
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- CN105132936B CN105132936B CN201510391422.0A CN201510391422A CN105132936B CN 105132936 B CN105132936 B CN 105132936B CN 201510391422 A CN201510391422 A CN 201510391422A CN 105132936 B CN105132936 B CN 105132936B
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- fused salt
- ilmenite
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- 150000003839 salts Chemical class 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 56
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 38
- 239000000843 powder Substances 0.000 title claims abstract description 26
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 claims abstract description 28
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 16
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 16
- 239000011733 molybdenum Substances 0.000 claims abstract description 16
- 239000012535 impurity Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000001110 calcium chloride Substances 0.000 claims abstract description 8
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 8
- 239000000292 calcium oxide Substances 0.000 claims abstract description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 8
- 239000010439 graphite Substances 0.000 claims abstract description 8
- 239000011780 sodium chloride Substances 0.000 claims abstract description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- 229910002971 CaTiO3 Inorganic materials 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 238000009856 non-ferrous metallurgy Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 230000005611 electricity Effects 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- WEUCVIBPSSMHJG-UHFFFAOYSA-N calcium titanate Chemical compound [O-2].[O-2].[O-2].[Ca+2].[Ti+4] WEUCVIBPSSMHJG-UHFFFAOYSA-N 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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- Electrolytic Production Of Metals (AREA)
Abstract
CaTiO is prepared from ilmenite with fused salt electrolysis process the present invention relates to one kind3The method of powder, belong to non-ferrous metallurgy technology field.Under an inert atmosphere, by CaO, NaCl and CaCl2The fused salt for obtaining and melting completely is well mixed and heated up, the ilmenite for accounting for fused salt mass fraction 1%~15.2% is added into fused salt and well mixed obtain is electrolysed fused salt;Electrolysis fused salt is placed in electrolytic cell, negative electrode is used as using molybdenum bar, control molybdenum bar does not contact the ilmenite of bottom of electrolytic tank, graphite rod is as 6~8h of anode electrolysis, take out bottom of electrolytic tank product, after impurity in product, deionized water rinsing and drying and other steps are filtered away through 1wt.%HCl solution, CaTiO is obtained3Powder.This method is solve CaTiO3Prior art into the problems such as reaction temperature during production is high, technological process is long, high energy consumption.
Description
Technical field
CaTiO is prepared from ilmenite with fused salt electrolysis process the present invention relates to one kind3The method of powder, belongs to non-ferrous metal
Metallurgical technology field.
Background technology
Calcium titanate(CaTiO3)As perovskite composite oxide ABO3One kind of novel inorganic nonmetallic materials, has
The crystal structure of stabilization, unique electromagnetic performance and very high redox, photocatalysis and electro-catalysis isoreactivity, are situated between in microwave
The fields such as matter ceramics, photo catalytic reduction are widely used.
CaTiO at present3Production method mainly have solid sintering technology, mechanochemistry synthesis method, soft chemical method etc..Its
In, solid sintering technology uses TiO2Be raw material with corresponding metal carbonate or oxide, by it is pre-sintered, re-sinter, cool down
Make its crystallization etc. step, obtain titanate micro mist, but the crystallite dimension of this method synthesis influenceed by sintering temperature it is big, to raw material
Requirement it is high, energy consumption is big, therefore is not suitable for extensive use.Mechanochemistry synthesis method is that raw material is passed through into the timing of high-energy ball milling one
Between after obtain presoma, then obtained after high temperature sintering.But this method influenceed by Ball-milling Time it is notable, using still not extensive.
Soft chemical method mainly has sol-gel(sol-gel)Method, fused salt(Cosolvent)Method etc., such method can prepare that ultra-fine, composition is equal
Even composite oxides powder, but grow reaction time, process conditions are difficult to control, and yield is less.
Fused salt electrolysis process prepares metal and the existing long history of alloy, wherein most typical represent is with ice crystal-oxygen
Change the Bayer method electrolytic production of aluminum that aluminium is raw material.Since 20th century, using FFC methods as the fused salt electrolysis process of new generation of representative and with
SOM methods are the appearance of the novel molten salt method of representative, new vitality are filled with for the research of molten-salt electrolysis, especially in refractory metal
Preparation process in substantially reduce production procedure, degraded cost, to reducing requirement in the preparation of raw material.
The A of China Patent Publication No. CN 102874866 report prepares flake micron with molten-salt growth method combination topochemistry method
Level calcium titanate crystal.This method adds reaction speed, contracted by two steps of chemical synthesis in the preparation and fused salt of presoma
Short manufacturing cycle, but reaction temperature is high, easily there is impurity generation.
The B of China Patent Publication No. CN 101792304 report to be prepared with satisfactory electrical conductivity and excellent with solid sintering technology
The complex perovskite structure ceramic material of different decay resistance, but this method length reaction time, composition are uncontrollable.
The A of China Patent Publication No. CN 103159473, which provide one kind, can prepare dielectric constant, high Q, frequency temperature system
The preparation method of the adjustable microwave dielectric ceramic materials of number.Mainly have that technological process is long, crystallite dimension is uneven the shortcomings that this method.
The content of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides one kind fused salt electrolysis process from ilmenite
Prepare CaTiO3The method of powder.The purpose of this method is solve CaTiO3Prior art into reaction temperature during production it is high,
The problems such as technological process is long, high energy consumption, the present invention is achieved through the following technical solutions.
One kind prepares CaTiO with fused salt electrolysis process from ilmenite3The method of powder, it is comprised the following steps that:
Step 1, under an inert atmosphere, by CaO, NaCl and CaCl2According to mol ratio(0.8~1):(8~12):(10~
20)It is well mixed and is warming up to 650~850 DEG C and obtain the fused salt melted completely, is added into fused salt and account for fused salt mass fraction 1%
~15.2% ilmenite and well mixed acquisition electrolysis fused salt;
Step 2, the electrolysis fused salt of step 1 is placed in electrolytic cell, using molybdenum bar as negative electrode, control molybdenum bar does not contact electrolysis
The ilmenite of trench bottom, graphite rod is as anode, then it in 2.8~3.2V, electrolysis temperature is 650~850 DEG C of bars to control tank voltage
6~8h is electrolysed under part, takes out bottom of electrolytic tank product, impurity in product, deionized water are filtered away through 1wt.%HCl solution
Rinse with after drying and other steps, obtain CaTiO3Powder.
The inert atmosphere is argon inert gas, wherein purity of argon>99.9%.
The ilmenite includes following mass percent component:Titanium 31.6%, iron 36.8%.
The beneficial effects of the invention are as follows:CaTiO is prepared from ilmenite with fused salt electrolysis process process provides one kind3Powder
The effective way at end, obtained CaTiO3Powder purity is high, compared with existing solid phase method, significantly reduces the temperature of reaction,
Shorten production cycle and technological process, and it is ilmenite abundance, cheap, prepare CaTiO in electrolysis ilmenite3Powder
Energy consumption is smaller during end, economic and environment-friendly.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
This prepares CaTiO with fused salt electrolysis process from ilmenite3The method of powder, it is comprised the following steps that:
Step 1, under an inert atmosphere, by CaO, NaCl and CaCl2According to mol ratio 0.8:8:20 are well mixed and heat up
The fused salt melted completely is obtained to 650 DEG C, the ilmenite of fused salt mass fraction 1% and well mixed acquisition electricity are added into fused salt
Solve fused salt;Inert atmosphere is argon gas, purity>99.9%;Ilmenite includes following mass percent component:Titanium 31.6%, iron
36.8%;
Step 2, the electrolysis fused salt of step 1 is placed in electrolytic cell, with molybdenum bar(Purity >=99.95%)As negative electrode, control
Molybdenum bar does not contact the ilmenite of bottom of electrolytic tank, and graphite rod is as anode, then controls tank voltage in 2.8V, electrolysis temperature 650
It is electrolysed 8h under the conditions of DEG C, takes out bottom of electrolytic tank product, impurity in product, deionized water is filtered away through 1wt.%HCl solution
Rinse with after drying and other steps, obtain CaTiO3Powder.
Embodiment 2
This prepares CaTiO with fused salt electrolysis process from ilmenite3The method of powder, it is comprised the following steps that:
Step 1, under an inert atmosphere, by CaO, NaCl and CaCl2According to mol ratio 1:12:10 are well mixed and are warming up to
850 DEG C obtain the fused salt melted completely, and the ilmenite of fused salt mass fraction 15.2% and well mixed acquisition electricity are added into fused salt
Solve fused salt;Inert atmosphere is argon gas, purity>99.9%;Ilmenite includes following mass percent component:Titanium 31.6%, iron 36.8%
Step 2, the electrolysis fused salt of step 1 is placed in electrolytic cell, with molybdenum bar(Purity >=99.95%)As negative electrode, control
Molybdenum bar does not contact the ilmenite of bottom of electrolytic tank, and graphite rod is as anode, then controls tank voltage in 3.2V, electrolysis temperature 850
It is electrolysed 6h under the conditions of DEG C, takes out bottom of electrolytic tank product, impurity in product, deionized water is filtered away through 1wt.%HCl solution
Rinse with after drying and other steps, obtain CaTiO3Powder.
Embodiment 3
This prepares CaTiO with fused salt electrolysis process from ilmenite3The method of powder, it is comprised the following steps that:
Step 1, under an inert atmosphere, by CaO, NaCl and CaCl2According to mol ratio 1:10:15 are well mixed and are warming up to
700 DEG C obtain the fused salt that melts completely, and the ilmenite of fused salt mass fraction 10% is added into fused salt and well mixed is electrolysed
Fused salt;Inert atmosphere is argon gas, purity>99.9%;Ilmenite includes following mass percent component:Titanium 31.6%, iron 36.8%
Step 2, the electrolysis fused salt of step 1 is placed in electrolytic cell, with molybdenum bar(Purity >=99.95%)As negative electrode, control
Molybdenum bar does not contact the ilmenite of bottom of electrolytic tank, and graphite rod is as anode, then controls tank voltage in 3.2V, electrolysis temperature 700
It is electrolysed 7h under the conditions of DEG C, takes out bottom of electrolytic tank product, impurity in product, deionized water is filtered away through 1wt.%HCl solution
Rinse with after drying and other steps, obtain CaTiO3Powder.
Embodiment 4
This prepares CaTiO with fused salt electrolysis process from ilmenite3The method of powder, it is comprised the following steps that:
Step 1, under an inert atmosphere, by CaO, NaCl and CaCl2According to mol ratio 1:8:20 are well mixed and are warming up to
700 DEG C obtain the fused salt melted completely, and the ilmenite of fused salt mass fraction 15.2% and well mixed acquisition electricity are added into fused salt
Solve fused salt;Inert atmosphere is argon gas, purity>99.9%;Ilmenite includes following mass percent component:Titanium 31.6%, iron
36.8%;
Step 2, the electrolysis fused salt of step 1 is placed in electrolytic cell, with molybdenum bar(Purity >=99.95%)As negative electrode, control
Molybdenum bar does not contact the ilmenite of bottom of electrolytic tank, and graphite rod is as anode, then controls tank voltage in 3.2V, electrolysis temperature 700
It is electrolysed 8h under the conditions of DEG C, takes out bottom of electrolytic tank product, impurity in product, deionized water is filtered away through 1wt.%HCl solution
Rinse with after drying and other steps, obtain CaTiO3Powder.
Embodiment 5
This prepares CaTiO with fused salt electrolysis process from ilmenite3The method of powder, it is comprised the following steps that:
Step 1, under an inert atmosphere, by CaO, NaCl and CaCl2According to mol ratio 0.8:12:20 are well mixed and heat up
The fused salt melted completely is obtained to 750 DEG C, the ilmenite of fused salt mass fraction 10% and well mixed acquisition electricity are added into fused salt
Solve fused salt;Inert atmosphere is argon gas, purity>99.9%;Ilmenite includes following mass percent component:Titanium 31.6%, iron
36.8%;
Step 2, the electrolysis fused salt of step 1 is placed in electrolytic cell, with molybdenum bar(Purity >=99.95%)As negative electrode, control
Molybdenum bar does not contact the ilmenite of bottom of electrolytic tank, and graphite rod is as anode, then controls tank voltage in 3.0V, electrolysis temperature 750
It is electrolysed 6h under the conditions of DEG C, takes out bottom of electrolytic tank product, impurity in product, deionized water is filtered away through 1wt.%HCl solution
Rinse with after drying and other steps, obtain CaTiO3Powder.
The embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula, in those of ordinary skill in the art's possessed knowledge, it can also make on the premise of present inventive concept is not departed from
Go out various change.
Claims (3)
1. one kind prepares CaTiO with fused salt electrolysis process from ilmenite3The method of powder, it is characterised in that comprise the following steps that:
Step 1, under an inert atmosphere, by CaO, NaCl and CaCl2According to mol ratio(0.8~1):(8~12):(10~20)It is mixed
Close uniformly and be warming up to 650~850 DEG C and obtain the fused salt that melts completely, added into fused salt account for fused salt mass fraction 1%~
15.2% ilmenite and well mixed acquisition electrolysis fused salt;
Step 2, the electrolysis fused salt of step 1 is placed in electrolytic cell, using molybdenum bar as negative electrode, control molybdenum bar does not contact cell bottom
The ilmenite in portion, graphite rod is as anode, then controls tank voltage under the conditions of 2.8~3.2V, electrolysis temperature are 650~850 DEG C
6~8h is electrolysed, bottom of electrolytic tank product is taken out, impurity, the deionized water rinsing in product is filtered away through 1wt.%HCl solution
After drying steps, CaTiO is obtained3Powder.
2. according to claim 1 prepare CaTiO with fused salt electrolysis process from ilmenite3The method of powder, its feature exist
In:The inert atmosphere is argon inert gas, wherein purity of argon>99.9%.
3. according to claim 1 prepare CaTiO with fused salt electrolysis process from ilmenite3The method of powder, its feature exist
In:The ilmenite includes following mass percent component:Titanium 31.6%, iron 36.8%.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101445942A (en) * | 2008-11-28 | 2009-06-03 | 清华大学 | Method for preparing solid oxide electrolytic cell anode material perovskite structure nano-powder |
EP2064369B1 (en) * | 2006-09-21 | 2011-03-30 | Qit-Fer Et Titane Inc. | Electrochemical process for the recovery of metallic iron and chlorine values from iron-rich metal chloride wastes |
CN103556167A (en) * | 2013-10-23 | 2014-02-05 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium carbide through molten salt electrolysis |
CN104451758A (en) * | 2014-11-13 | 2015-03-25 | 昆明理工大学 | Method for preparing titanium carbide by performing molten salt electrolysis on high titanium slags |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
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GB0913736D0 (en) * | 2009-08-06 | 2009-09-16 | Chinuka Ltd | Treatment of titanium ores |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2064369B1 (en) * | 2006-09-21 | 2011-03-30 | Qit-Fer Et Titane Inc. | Electrochemical process for the recovery of metallic iron and chlorine values from iron-rich metal chloride wastes |
CN101445942A (en) * | 2008-11-28 | 2009-06-03 | 清华大学 | Method for preparing solid oxide electrolytic cell anode material perovskite structure nano-powder |
CN103556167A (en) * | 2013-10-23 | 2014-02-05 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium carbide through molten salt electrolysis |
CN104451758A (en) * | 2014-11-13 | 2015-03-25 | 昆明理工大学 | Method for preparing titanium carbide by performing molten salt electrolysis on high titanium slags |
Non-Patent Citations (1)
Title |
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熔盐电解法制备高钛铁合金;李晴宇等;《稀有金属》;20111130;第35卷(第6期);第1.2及2.2节 * |
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