CN109650893A - A kind of method of low temperature preparation titaniferous composite anode - Google Patents
A kind of method of low temperature preparation titaniferous composite anode Download PDFInfo
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- CN109650893A CN109650893A CN201910030250.2A CN201910030250A CN109650893A CN 109650893 A CN109650893 A CN 109650893A CN 201910030250 A CN201910030250 A CN 201910030250A CN 109650893 A CN109650893 A CN 109650893A
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- composite anode
- titaniferous
- titanium
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- titaniferous composite
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- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 60
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000010936 titanium Substances 0.000 claims abstract description 54
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 53
- 238000000465 moulding Methods 0.000 claims abstract description 37
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 30
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000003245 coal Substances 0.000 claims abstract description 19
- 230000003647 oxidation Effects 0.000 claims abstract description 19
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 19
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 17
- CYKMNKXPYXUVPR-UHFFFAOYSA-N [C].[Ti] Chemical compound [C].[Ti] CYKMNKXPYXUVPR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 12
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 12
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 20
- 238000000748 compression moulding Methods 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 2
- 239000003546 flue gas Substances 0.000 claims description 2
- 238000003754 machining Methods 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims 1
- 238000005868 electrolysis reaction Methods 0.000 abstract description 16
- 150000003839 salts Chemical class 0.000 abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 10
- 238000005363 electrowinning Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 13
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 11
- 229910052799 carbon Inorganic materials 0.000 description 10
- 239000000203 mixture Substances 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000008187 granular material Substances 0.000 description 8
- 239000000084 colloidal system Substances 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 3
- 239000005011 phenolic resin Substances 0.000 description 3
- 229920001568 phenolic resin Polymers 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000009766 low-temperature sintering Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- CSJDCSCTVDEHRN-UHFFFAOYSA-N methane;molecular oxygen Chemical compound C.O=O CSJDCSCTVDEHRN-UHFFFAOYSA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910010068 TiCl2 Inorganic materials 0.000 description 1
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- UKKGMDDPINLFIY-UHFFFAOYSA-N [C+4].[O-2].[Ti+4].[O-2].[O-2].[O-2] Chemical compound [C+4].[O-2].[Ti+4].[O-2].[O-2].[O-2] UKKGMDDPINLFIY-UHFFFAOYSA-N 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- LCDFWRDNEPDQBV-UHFFFAOYSA-N formaldehyde;phenol;urea Chemical compound O=C.NC(N)=O.OC1=CC=CC=C1 LCDFWRDNEPDQBV-UHFFFAOYSA-N 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- KHYBPSFKEHXSLX-UHFFFAOYSA-N iminotitanium Chemical compound [Ti]=N KHYBPSFKEHXSLX-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910001000 nickel titanium Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
- C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/58007—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides
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- C04B35/58021—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on refractory metal nitrides based on titanium nitrides, e.g. TiAlON based on titanium carbonitrides
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention discloses a kind of methods of low temperature preparation titaniferous composite anode.The combined inorganic bond of one or more of the combined titaniferous powder of one or more of the oxidation of coal titanium of 80~97%wt or carbon titanium oxynitride, the silicon dioxide gel of 3~20%wt, Aluminum sol, sodium silicate aqueous solution, TiO 2 sol is uniformly mixed and prepares slurry by the method for the present invention; slurry is pressed and molded; blank is dried again, then under vacuum, nitrogen or inert gas shielding at a temperature of 850-1250 DEG C sinter molding.Finally, forming to obtain titaniferous composite anode by surfacing.The titaniferous composite anode of preparation is used for electroextraction by molten salt electrolysis titanium.The present invention can use the oxidation of coal titanium of cheap titanium-containing materials preparation or carbon titanium oxynitride powder is raw material, and greatly reduce sintering temperature, energy saving.
Description
Technical field
The invention belongs to smelting field of nonferrous metal, and in particular to a kind of compound sun for electroextraction by molten salt electrolysis titanium
The low-temperature sintering forming method of pole.
Background technique
Existing Titanium industrialized preparing process is Kroll technique.The technique includes chlorination TiO in the presence of carbon2Mine
Stone, and the TiCl made4It is reacted with magnesium to produce titanium sponge.Kroll complex process, the TiCl in the technique4Purification,
TiCl4The separating at high temperature MgCl of reduction and Titanium2Purification is time-consuming, high energy consumption technology.
Generation nineteen fifty, patent US2722509 are described the anode molten-salt electrolysis of TiO and carbon preparation in cathode precipitating metal
Titanium.The MER company in the U.S. is reacted under the conditions of 1100 DEG C~1300 DEG C with the mixture of titanium oxide and carbon obtains TiO and TiC
Compound, and as electrolytic anode extract Titanium (CN104831318B).Patent CN100415940C using TiO and
The composite feedstock of TiC prepares Titanium as anode electrolysis.CN103451682B is with titaniferous material and carbon under nitrogen containing atmosphere
Reaction prepares carbon titanium oxynitride (TiCxOyNz, 0 < x≤y≤1,0 < z < 1, x+y+z=1) and it is used as molten-salt electrolysis anode.
The anode for the compound that CN102925930B is electrolysed titaniferous material and carbon by two-step method prepares Titanium.
Described in summary, the method for this kind of electroextraction by molten salt electrolysis titanium all use titaniferous composite anode as dissolution anode,
The titanium of low price of the composite anode of sinter molding in fused salt Inner electrolysis, anode is dissolved in fused salt and forms Ti2+、Ti3+Titanium from
Son, titanium ion are precipitated to obtain Titanium in cathode.Such method cannot be directly electrolysed using titaniferous powder body material, and need to pass through
It is reused after high temperature sintering molding.
CN1867702B is by directly mixing TiO2Un-sintered electrode is formed with carbon, and is heated under no air conditions
1000~2200 DEG C, continue 0.1-100 hours, to form titanium suboxide/carbon composite anode.Although prepared by one step of this method
Composite anode, but require high-purity TiO2As raw material, otherwise impurity can pollute fused salt and metal titanium products.
Patent CN106315584A is using titaniferous ore or clinker as raw material, and hydrogen, methane are as reducing agent and carburization agent, system
Standby oxidation of coal titanium obtains oxidation of coal titanium valve body after broken, fine grinding and except iron.Similarly, patent CN106744960A carbon
Powder is that oxidation of coal titanium valve body is prepared in carburization agent.
And oxidation of coal titanium valve body cannot be directly used to molten-salt electrolysis, need to prepare molding block anode by high temperature sintering
After can be only used for electroextraction by molten salt electrolysis titanium.Present invention applicant is the study found that if direct high temperature sintering oxidation of coal titanium
Or if carbon titanium oxynitride powder, temperature needs 1600~1800 DEG C or so, and temperature requirement is high, causes energy consumption very high.
Other anode sintering forming methods include following methods: patent CN105220180B by simultaneously be added carbon dust with
Pitch binder low-temperature sintering anode；Patent CN101949038B directly prepares oxidation of coal titanium (TiC in cathode with electrolysis methodxOy,
Wherein 0 < x≤1,1≤y < 2), electrolytic carbon titanium oxide obtains Titanium again later.Patent CN104831318B passes through addition phenol
Urea formaldehyde adhesive bonds raw material.The inventors of the present invention discovered through researches that organic bond pitch, phenolic resin etc. are organic viscous
The carbon that mixture is brought into can pollute the Titanium of molten salt electrolyte and extraction, reduce Titanium product quality.
The shortcoming of existing method:
The inventors of the present invention discovered through researches that there are two types of the titaniferous composite anodes of process route preparation sinter molding at present.
The existing composite anode forming and sintering method for electroextraction by molten salt electrolysis titanium has the disadvantage that
Method 1 and its shortcoming.Use the TiO of high-purity2, TiO, TiC powder be raw material single step reaction, sinter molding
The titaniferous composite anode of oxidation of coal titanium or carbon titanium oxynitride.But the TiO for needing high-purity of this method2, TiO, TiC powder system
Standby oxidation of coal titanium or carbon titanium oxynitride powder, the TiO of high-purity2, TiO, TiC powder cost of material it is high.Also, research hair
Existing, sintering temperature, which is 1600~2000 DEG C, can just obtain qualified titaniferous composite anodes, sintering temperature require it is high, cause energy consumption at
This height.
Method 2 and its shortcoming.First using titaniferous materials such as low-grade ilmenite, high titanium slag, synthetic rutiles
Oxidation of coal titanium or carbon titanium oxynitride are prepared in 1100~1300 DEG C of temperature ranges, after removing the magazines such as reduced iron, silicate,
What is obtained is oxidation of coal titanium or carbon titanium oxynitride titaniferous powder, these titaniferous powders are used further to fused salt electricity after needing sinter molding
Solution.For existing step sinter molding titaniferous composite anode in the case where not adding adhesive, sinter molding temperature needs 1600
~2000 DEG C or so, sintering temperature requires height, causes energy consumption cost high；In the case where adding organic bond, by carbon oxygen
Sintering temperature can be reduced after titanium or carbon titanium oxynitride powder addition pitch, the organic bonds such as phenolic resin by changing, but pitch,
The carbon that the organic bonds such as phenolic resin are brought into can pollute the Titanium of molten salt electrolyte and extraction, reduce product quality.
Therefore, in order to reduce the temperature and energy consumption of composite anode forming and sintering, and guarantee the matter of the composite anode of preparation
Under the requirement of amount, on the Process ba- sis of method 2, a kind of method that the present invention proposes low temperature preparation titaniferous composite anode.
Summary of the invention
The present invention is in view of the above-mentioned problems, provide a kind of method for preparing titaniferous composite anode at a lower temperature.
Inventor is the study found that the oxidation of coal titanium or carbon oxygen prepared with titaniferous ores such as ilmenite, rutile
Nitride powder itself contains the impurity such as a small amount of silica, aluminium oxide, titanium dioxide, and in Molten, these are miscellaneous
Matter is difficult to dissolve into fused salt, and fused-salt bath is finally removed in the form of anode slime.Therefore, these impurity will not pollute
Fused salt and metal titanium products.
In addition, experimental studies have found that, by silicon dioxide gel, Aluminum sol, sodium silicate aqueous solution, TiO 2 sol
The inorganic binder of one or more combination, can be effectively reduced the sintering temperature containing Ni―Ti anode.Also, these inorganic binders
Silica, aluminium oxide, sodium metasilicate, the titanium dioxide inside contained will not be dissolved in Molten into fused salt, can be with
It is removed fused-salt bath in the form of anode slime, is able to satisfy the quality requirement of molten-salt electrolysis.It is therefore proposed that following technical side
Case.
Technical solution used by the present invention solves the above problems is:
A method of preparing titaniferous composite anode, comprising the following steps:
Step S1, prepares slurry, and the inorganic binder of the titaniferous powder of 80~97%wt, 3~20%wt is uniformly mixed
Prepare slurry, wherein titaniferous powder is oxidation of coal titanium (TiCxOy, 0 < x≤y≤1, x+y=1) or carbon titanium oxynitride
(TiCxOyNz, 0 < x≤y≤1,0 < z < 1, x+y+z=1) one or more of combination；Inorganic binder is dioxy
The combination of one or more of SiClx colloidal sol, Aluminum sol, sodium silicate aqueous solution, TiO 2 sol；
Slurry after mixing is sent into compression moulding in the molding die of moulding press by step S2, compression molding；
Preferably, titaniferous powder and inorganic binder stir 20~40min in high-speed mixer, in rectangular or cylinder
Shape mold energy compression moulding.
Step S3, dry, the blank after compression molding is dried at a temperature of 30-150 DEG C, and the time 1~48 hour；
Preferably, the blank after compression molding is dried at a temperature of 80-120 DEG C, and the time 2~4 hours；It is further preferable that
Blank is dried using 80-120 DEG C of dry flue gas.
Step S4, sinter molding, molding mass after the drying sinter molding under vacuum, nitrogen or inert gas shielding,
850-1250 DEG C of sintering temperature；
Preferably, the molding mass after drying under nitrogen protection, the sinter molding in tunnel oven.
Step S5, surface machining are trimmed to titaniferous composite anode finished product.
During titaniferous composite anode sinter molding, part-structure can be caused to deform, need to set by grindings such as cutting machines
It is standby to titaniferous composite anode recontour, in favor of the electrolysis of next step.
In step S1, the titaniferous powder average grain diameter is 80~900 mesh.
Preferably, the titaniferous powder average grain diameter is 300~600 mesh.
In step S1, the silica colloidal particles average diameter in the silicon dioxide gel is 5-300nm, quality
Percentage composition is 25%~40%.
Preferably, the silica colloidal particles average diameter in the silicon dioxide gel is 10-100nm.
It is further preferable that the silica colloidal particles average diameter in the silicon dioxide gel is 10-30nm.
In step S1, the alumina gel average particle diameter of the Aluminum sol is 5-200nm, and mass percentage is
15%~30%.
Preferably, the alumina gel average particle diameter of the Aluminum sol is 10-50nm.
In step S1, the sodium metasilicate mass percentage in the sodium silicate aqueous solution is 20%~35%.
In step S1, the colloidal particle average diameter of the TiO 2 sol is 5-500nm, and mass percentage is
15%~30%.
Preferably, the colloidal particle average diameter of the TiO 2 sol is 10-30nm.
In step S2, pressure added by the moulding press is 5~200MPa.
Preferably, pressure added by the moulding press is 100~200MPa.
It is further preferable that pressure added by the moulding press is 150~200MPa.
In step S4, heating rate and rate of temperature fall are 5~10 DEG C/min in the sintering process, and sintering time is
0.5-6 hours.
The beneficial effects of the present invention are:
1. the present invention can be used low with ilmenite, high titanium slag, synthetic rutile, natural rutile, vanadium titano-magnetite etc.
The oxidation of coal titanium or carbon titanium oxynitride powder of grade titanium-containing materials preparation are raw material, and cost of material is low；
2. the inorganic binder being composed of silicon dioxide gel, Aluminum sol, sodium silicate aqueous solution, TiO 2 sol
Sintering temperature is reduced to 850-1250 DEG C, energy saving.
Specific embodiment
The embodiment of the present invention is described in detail below, but what the present invention can be defined by the claims and cover
Multitude of different ways is implemented.
Firstly, embodiment prepares oxidation of coal titanium, carbon titanium oxynitride powder.The existing a variety of method preparations of titaniferous composite granule,
Such as patent CN106315584A, CN106744960A.The titaniferous composite granule that present example uses is prepared by the following method.
Titanium dioxide (99%TiO2, 0.4 micron of average grain diameter) and graphite powder (99.8% phosphorus content, 50 microns of average grain diameter) with mass ratio
8: 2 ratio ground and mixed 3 hours in ball mill, obtained mixed material are pressed under 60MPa pressure directly in steel mold
The particle of 12 millimeters of diameter 10mm height.By particle in 1000-1500 DEG C of range, with argon atmosphere or nitrogen and argon gas
After preparing 2-18 hours in atmosphere, titanium containing composite material, chemical composition TiC are obtainedxOy(0 < x≤y≤1, x+y=1), or
TiCxOyNz(0 < x≤y≤1,0 < z < 1, x+y+z=1)；Chemical composition is determined by XRD analysis.Finally, titaniferous is compound
Grinding obtains varigrained oxidation of coal titanium, carbon titanium oxynitride powder in material ball mill.
Embodiment 1
By the 45%wt titaniferous composite granule TiC of gross mass 5kg0.3O0.7, 45%wt titaniferous composite granule
TiC0.3O0.5N0.2, silicon dioxide gel 5%wt, Aluminum sol 5%wt mixture stirs 30min in high-speed mixer.Titaniferous is multiple
It is 300 mesh that powder, which is closed, as partial size；Silica colloid particles average diameter is 20nm in silicon dioxide gel, and mass percentage is
25%, pH are neutral；Silica colloid particles average diameter is 20nm, mass percentage 20% in Aluminum sol.
Slurry after mixing is sent into compression moulding in the molding die of moulding press, pressure 150MPa, obtain 200 ×
The blank of 100 × 50mm.Blank is 4 hours dry in 110 DEG C of baking ovens.Blank after drying under protection of argon gas, in Muffle
Sinter molding in furnace.Heating rate and rate of temperature fall are 5 DEG C/min in sintering process, and 1050 DEG C of temperature, sintering time is 4 small
When.Finally, obtaining molding titaniferous composite anode to titaniferous composite anode recontour by cutting machine.
Embodiment 2
By the 90%wt titaniferous composite granule TiC of gross mass 5kg05O0.5, the mixture of silicon dioxide gel 10%wt is in height
40min is stirred in fast blender.Titaniferous composite granule is that partial size is 600 mesh；Silica colloid particles are average in silicon dioxide gel
Diameter is 15nm, mass percentage 30%, pH alkalinity.
Slurry after mixing is sent into compression moulding in the molding die of moulding press, pressure 100MPa, obtain 200 ×
The blank of 100 × 50mm.Blank is 10 hours dry in 60 DEG C of baking ovens.Molding mass after drying under nitrogen protection, in height
Sinter molding in warm graphite furnace.Heating rate and rate of temperature fall are 10 DEG C/min in sintering process, 1100 DEG C of temperature, when sintering
Between be 3 hours.Finally, obtaining molding titaniferous composite anode to titaniferous composite anode recontour by cutting machine.
Comparative example 2-1
Without using inorganic bond listed by the present invention, with the silicon dioxide gel in deionized water alternate embodiment 2,
Remaining experiment condition is same as Example 2, and blank is loose after sintering, is unable to sinter molding titaniferous composite anode.Comparative example card
Inorganic bond, which is illustrated, reduces the effect of sintering temperature.
Comparative example 2-2
It is burnt without using inorganic bond listed by the present invention with the silicon dioxide gel in deionized water alternate embodiment 1
1750 DEG C of junction temperature, remaining experiment condition is same as Example 2, and molding titaniferous composite anode is prepared.
Embodiment 3~12
Pulp components and sintering temperature in following table prepare titaniferous composite anode, remaining condition is same as Example 1, point
Titaniferous composite anode 3~12 is not prepared.
Wherein, oxidation of coal titanium titaniferous composite granule chemical composition is TiC0.33O0.67, partial size is 500 mesh；Carbon titanium oxynitride contains
Titanium composite granule chemical composition is TiC0.3O0.5N0.2, partial size is 600 mesh；Silica colloid particles average diameter in silicon dioxide gel
For 20nm, mass percentage 35%, pH alkalinity；Silica colloid particles average diameter is 30nm in Aluminum sol, and quality percentage contains
Amount is 20%；Sodium metasilicate mass percentage in sodium silicate aqueous solution is 35%；Colloidal particle is average in TiO 2 sol
Diameter is 50nm, mass percentage 15%.
Embodiment 13
The titaniferous composite anode of above embodiments preparation is subjected to the experiment of electroextraction by molten salt electrolysis titanium.Experiment condition is,
The metallic titanium plate of 2mm thickness is cathode, with LiCl-NaCl-KCl-TiCl2Fused salt is electrolyte, titanium ion content 4%wt.Electricity
It is protected in solution slot with argon gas, is electrolysed under the conditions of 550 DEG C.Bath voltage is 4.1V, anodic current density 0.1A/cm2,
Negative electricity current density is 0.2A/cm2.After electrolysis 10 hours, under protection of argon gas, cooling cathode is to 100 DEG C hereinafter, after taking out cathode
The Titanium for scraping cathode surface deposition, is cleaned using deionized water.Finally, drying under vacuum conditions, prepared
Titanium.Oxygen content elemental analysis is carried out to Titanium, cathode efficiency is calculated according to faraday's principle.Experimental result
It is as follows.
As can be seen from the above table, the molten-salt electrolysis of the titaniferous composite anode of embodiment 1-12 preparation prepares the experiment of Titanium
As a result close with the experimental result of the titaniferous composite anode of existing high temperature sintering preparation, and the burning of titaniferous composite anode of the invention
Junction temperature is significantly less than existing method.
These are only the preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art
For member, the invention may be variously modified and varied.All within the spirits and principles of the present invention, it is made it is any modification,
Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of method of low temperature preparation titaniferous composite anode, which comprises the following steps:
Step S1, prepares slurry, and the inorganic binder of the titaniferous powder of 80~97%wt, 3~20%wt is uniformly mixed preparation
Slurry, wherein titaniferous powder is oxidation of coal titanium (TiCxOy, 0 < x≤y≤1, x+y=1) or carbon titanium oxynitride (TiCxOyNz, 0
< x≤y≤1,0 < z < 1, x+y+z=1) one or more of combination；Inorganic binder is silicon dioxide gel, aluminium
One of colloidal sol, sodium silicate aqueous solution, TiO 2 sol or the combination of more kinds；
Slurry after mixing is sent into compression moulding in the molding die of moulding press by step S2, compression molding；
Step S3, dry, the blank after compression molding is dried at a temperature of 30-150 DEG C, and the time 1~48 hour；
Step S4, sinter molding, molding mass after drying sinter molding, sintering temperature under vacuum or inert gas shielding
850-1250℃；
Step S5, surface machining are trimmed to titaniferous composite anode finished product.
2. the method for low temperature preparation titaniferous composite anode according to claim 1, which is characterized in that described in step S1
Titaniferous powder average grain diameter be 80~900 mesh, preferably 300-600 mesh.
3. the method for low temperature preparation titaniferous composite anode according to claim 1, which is characterized in that described in step S1
Silicon dioxide gel in silica colloidal particles average diameter be 5-300nm, mass percentage be 25%~40%.
4. the method for low temperature preparation titaniferous composite anode according to claim 1, which is characterized in that described in step S1
Aluminum sol alumina gel average particle diameter be 5-200nm, mass percentage be 15%~30%, preferably 10-
50nm。
5. the method for low temperature preparation titaniferous composite anode according to claim 1, which is characterized in that described in step S1
Sodium silicate aqueous solution in sodium metasilicate mass percentage be 20%~35%.
6. the method for low temperature preparation titaniferous composite anode according to claim 1, which is characterized in that described in step S1
TiO 2 sol colloidal particle average diameter be 5-500nm, mass percentage be 15%~30%.
7. the method for low temperature preparation titaniferous composite anode according to claim 1, which is characterized in that described in step S2
Moulding press added by pressure be 5~200MPa, preferably 100-200Mpa, more preferable 150-200Mpa.
8. the method for low temperature preparation titaniferous composite anode according to claim 1, which is characterized in that be molded into step S3
Blank after type is dried at a temperature of 80-120 DEG C, and the time 2~4 hours；Preferably, using 80-120 DEG C of dry flue gas to base
Material is dried.
9. the method for low temperature preparation titaniferous composite anode according to claim 3, which is characterized in that described in step S1
Silica colloidal particles average diameter in silicon dioxide gel is 10-100nm；Preferably, the silicon dioxide gel
In silica colloidal particles average diameter be 10-30nm.
10. the method for low temperature preparation titaniferous composite anode according to claim 1, which is characterized in that described in step S4
Sintering process in heating rate and rate of temperature fall be 5~10 DEG C/min, sintering time is 0.5-6 hours.
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