CN104192894A - Refining method of titanium tetrachloride - Google Patents
Refining method of titanium tetrachloride Download PDFInfo
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- CN104192894A CN104192894A CN201410398848.4A CN201410398848A CN104192894A CN 104192894 A CN104192894 A CN 104192894A CN 201410398848 A CN201410398848 A CN 201410398848A CN 104192894 A CN104192894 A CN 104192894A
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- tower
- valve
- ticl
- condenser
- vanadium
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- 238000000034 method Methods 0.000 title claims abstract description 42
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 title claims abstract description 36
- 238000007670 refining Methods 0.000 title claims abstract description 18
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 54
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 54
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 13
- 239000010703 silicon Substances 0.000 claims abstract description 13
- 150000004671 saturated fatty acids Chemical class 0.000 claims abstract description 10
- 238000004821 distillation Methods 0.000 claims abstract description 7
- 229920000642 polymer Polymers 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000012535 impurity Substances 0.000 claims description 21
- 238000012856 packing Methods 0.000 claims description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000010936 titanium Substances 0.000 claims description 12
- 229910052719 titanium Inorganic materials 0.000 claims description 12
- 229910003902 SiCl 4 Inorganic materials 0.000 claims description 11
- 238000009835 boiling Methods 0.000 claims description 11
- 239000003960 organic solvent Substances 0.000 claims description 10
- 239000003921 oil Substances 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 8
- 239000010949 copper Substances 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- IRFSXVIRXMYULF-UHFFFAOYSA-N 1,2-dihydroquinoline Chemical compound C1=CC=C2C=CCNC2=C1 IRFSXVIRXMYULF-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000012188 paraffin wax Substances 0.000 claims description 5
- 238000010025 steaming Methods 0.000 claims description 5
- 229910001369 Brass Inorganic materials 0.000 claims description 4
- 239000010951 brass Substances 0.000 claims description 4
- 239000002480 mineral oil Substances 0.000 claims description 3
- 235000010446 mineral oil Nutrition 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract description 2
- ZNRLMGFXSPUZNR-UHFFFAOYSA-N 2,2,4-trimethyl-1h-quinoline Chemical compound C1=CC=C2C(C)=CC(C)(C)NC2=C1 ZNRLMGFXSPUZNR-UHFFFAOYSA-N 0.000 abstract 2
- 229910003074 TiCl4 Inorganic materials 0.000 abstract 2
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 239000011265 semifinished product Substances 0.000 abstract 1
- 238000009833 condensation Methods 0.000 description 9
- 230000005494 condensation Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 239000005662 Paraffin oil Substances 0.000 description 4
- 238000003763 carbonization Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 235000003441 saturated fatty acids Nutrition 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 235000010215 titanium dioxide Nutrition 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a refining method of titanium tetrachloride. The refining method comprises the following steps: feeding crude TiCl4 into a heat exchanger from an overhead tank; preparing a mixed organic solution from paroline, saturated fatty acid, p-phenylenediamine and 2,2,4-trimethyl-1,2-dihydroquinoline polymer and feeding the mixed organic solution into a mixer; adding the crude TiCl4 in a semi-finished product tank into a float valve tower from the middle upper part of the tower, heating the float valve tower to the range of 60-100 DEG C so that the high-boiling-point titanium tetrachloride moves downwards to go into a second distillation kettle from the bottom of the float valve tower, and then carrying out next step of refining vanadium removal treatment. The refining method of the titanium tetrachloride has the advantages that the adopted organic matters are cheap and wide in source, a rectification tower has a self-cleaning function so that a copper wire in the tower can be reused, and the byproducts generated such as compounds containing vanadium and silicon are recycled by use of a recovery tank and clean production is realized. The refining method of the titanium tetrachloride succeeds in improving the shortcomings of vanadium removal by use of organic matters at present, and has excellent economic benefit and social benefit.
Description
Technical field
The present invention relates to a kind of production method of titanium tetrachloride, relate in particular to a kind of titanium tetrachloride process for purification.
Background technology
Titanium tetrachloride is the important intermediates of producing titanium white, titanium sponge and titanium series product.Industrial crude titanic chloride is a kind of reddish-brown turbid solution, contains much impurity, and composition is very complicated.Crude titanic chloride must be refined, otherwise because the impact of impurity will affect the processing characteristics of downstream titanium products widely.Refining principle is generally removed FCCl with distillating method
3deng high-boiling-point impurity, remove SiCl with rectificating method
4deng lower-boiling impurity, with the VOCl in the close impurity of chemical process removal boiling point such as displacement
3.The conventional vanadium reagents that removes has copper, aluminium powder, hydrogen sulfide and organism etc. at present, but relative merits are different.Copper wire vanadium removal, the expensive cost of copper product is high; Aluminium powder is except vanadium, and aluminium powder is a kind of explosive material, requires very high to production unit; Hydrogen sulfide is except vanadium, and hydrogen sulfide is highly toxic substance, and production environment is poor, and equipment is had to corrosive nature; Organism is except vanadium, and organism is cheap and easy to get, nontoxic, usage quantity is few, and general industry is produced this kind of method that adopt, but it is many that existing organism removes the residue producing in vanadium production process, easily fouling equipment, blocking pipe and condenser, and products obtained therefrom is impure, there is a small amount of organic substance residues.
Summary of the invention
Undesirable except its effect of vanadium in order to solve existing organism, still contain the technical problems such as the further processing of the impurity such as vanadium, carbon dust, silicon tetrachloride, needs, the invention provides a kind of titanium tetrachloride process for purification of clean, easy, efficient, good impurity removing effect.
The present invention addresses the above problem adopted technical scheme: a kind of titanium tetrachloride process for purification, comprises the following steps:
(1) by thick TiCl
4sent in interchanger thick TiCl in interchanger by header tank
4be heated to 120-140 DEG C, with the thick TiCl of after heat
4be sent in blender;
(2) by 100 parts of paraffin oils, saturated fatty acid 80-100 part, Ursol D 2-4 part, 2,2,4-trimethylammonium 1,2-dihydro quinoline polymer 0.3-0.5 part is made mixed organic solvents and is sent in above-mentioned blender, mixed organic solvents and hot TiCl
4, blending ratio is 1:1, and mixture is sent in the first still kettle and distilled, and keeps distillation temperature in the kettle at 140-150 DEG C, most of foreign matter of vanadium that contains enters vanadium accumulator tank, TiCl by the shore pipe of the first still kettle bottom
4steam and portion gas impurity enter packing tower and the first condenser successively from the vapor pipe at the first still kettle top, form liquid work in-process and are stored in work in-process tank;
(3) the thick TiCl in work in-process tank
4added in tower by valve tray column middle and upper part, valve tray column is heated to 60-100 DEG C, lower boiling SiCl
4be vaporized and become steam and move up, send in silicon accumulator tank after entering the second condenser condenses, high boiling titanium tetrachloride moves down from valve tray column bottom and enters after-fractionating still, carries out next step refine and removing vanadium processing;
(4) containing vanadium TiCl
4after after-fractionating still is by the 3rd condenser condenses, send into the 3rd still kettle, through the 3rd still kettle by TiCl
4steam is sent into essence and is steamed in tower, TiCl
4steam by contacting except the copper ball being rolled into by copper wire in vanadium tower, is deposited on copper wire surface its contained foreign matter of vanadium continuously, the TiCl after refining
4by the TiCl of brass wire tower bottom
4bleed valve is delivered to the 4th condenser condenses, is housed in finished pot, and vanadium-containing water is delivered to vanadium accumulator tank by brass wire tower bottom discharge valve.
Realize the device of above-mentioned titanium tetrachloride process for purification, comprise thick titanium header tank, organism oil groove, flow valve, well heater, blender, still kettle, packing tower, valve tray column, condenser, essence steaming tower; The discharge nozzle of described thick titanium header tank is connected with the feed-pipe of well heater by flow valve, and the discharge nozzle of interchanger is connected with blender; The discharge nozzle of organism oil groove is connected with blender by flow valve, the discharge nozzle of blender is connected with the first still kettle feed-pipe, the vapor pipe at the first distillation tower top is connected with packing tower, and packing tower top vapor pipe is connected with the first condenser, and the first condenser discharge nozzle is connected with work in-process tank; The discharge nozzle of work in-process tank is connected with valve tray column, the discharge nozzle of valve tray column bottom is connected with after-fractionating still, after-fractionating still discharge port Guan Yu tri-condenser opening for feeds connect, the 3rd condenser discharge port is connected with the 3rd still kettle, the 3rd still kettle is steamed tower with essence and is connected, essence is steamed tower bottom discharge port and is connected with the 4th condenser, and the discharge nozzle of the 4th condenser is connected with finished pot.
As preferably, the shore pipe of described the first still kettle bottom is connected with vanadium accumulator tank.
As preferably, described valve tray column bottom is provided with after-fractionating still, and valve tray column top is provided with vapor pipe, and vapor pipe is connected with the second condenser, and the discharge nozzle of the second condenser is connected with silicon accumulator tank, and silicon accumulator tank top is connected with valve tray column.
As preferably, described essence is steamed tower, comprises tower body, water pump, air compressor machine, steam boiler, in described tower body, is provided with multiple sieve plate, is filled with copper wire balls between sieve plate; Tower body bottom and tower body side are all connected with Y-tube, and the Y-tube of described tower body bottom is connected with liquid titanium tetrachloride bleed valve and water discharge valve respectively; The Y-tube of described tower body side enters valve with crude titanic chloride respectively and dry air valve is connected, and dry air valve is connected with instrument air dryer through pipeline, and instrument air dryer is connected with air compressor machine; Tower body top is connected with four-way pipe, four-way pipe is connected with steam valve, water inlet pipe, vent valve respectively, wherein water inlet pipe is connected with water-vapor exchange threeway through pipeline, water-vapor exchange threeway one end is connected with pump outlet through water intaking valve, the water-vapor exchange threeway the other end is connected with air compressor machine exhaust nozzle through pressure lock, and steam valve is connected with steam boiler through steam-pipe.
In blender, paraffin oil, saturated fatty acid can carbonization form gac by VOCl
3reduce and adsorb other impurity, forming higher-boiling compound; And Ursol D and 2,2,4-trimethylammonium 1,2-dihydro quinoline polymer (anti-aging agent RD) can be controlled speed of response, adjust except vanadium efficiency.
The present invention has except vanadium effect is good, pollution-free, the feature of automatically working, it adopts novel organism composition except vanadium technique, except vanadium effect can reach more than 99%, and the residue easy to clean producing, overcome traditional organism and easily produced residue thickness, bulky except vanadium, easily the shortcoming of blocking pipe.In device, three-stage distillation still and packing tower, valve tray column, essence steaming tower can further separate the impurity containing in crude titanic chloride, can well separate various lower boilings and high-boiling-point impurity and solid particle polluter in crude titanic chloride; Novel organism composition and essence are steamed tower and are coordinated except vanadium, except vanadium effect can be increased to more than 99.5%, cheap, the wide material sources of organism that the present invention adopts, essence is steamed tower and is had self-cleaning function, can make copper wire in tower reuse, and the by product that contains the compound such as vanadium, silicon producing also can be recycled by accumulator tank, has realized and has cleaned production.This titanium tetrachloride process for purification has improved the weak point of existing organism except vanadium, has good economic benefit and social benefit.
Brief description of the drawings
Fig. 1 is the structural representation of the thick titanium header tank of the present invention to work in-process tank;
Fig. 2 is the structural representation of work in-process tank of the present invention to finished pot;
Fig. 3 is the structural representation that essence is steamed tower.
Embodiment
Below in conjunction with embodiment, the technical scheme of invention is described in further detail.
Fig. 1 is the structural representation of the thick titanium header tank of the present invention to work in-process tank, and Fig. 2 is the structural representation of work in-process tank of the present invention to finished pot, and Fig. 3 is the structural representation that essence is steamed tower.As shown in the figure, realize this titanium tetrachloride refining device, comprise thick titanium header tank 1, mineral oil groove 2, flow valve 3, well heater 4, blender 5, still kettle (6,61,62), packing tower 8, condenser (9,91,92,93), valve tray column 11, essence steaming tower 13 etc.The discharge nozzle of its thick titanium header tank 1 is connected with the feed-pipe of well heater 4 through flow valve 3, and the discharge nozzle of well heater 4 is connected with blender 5.The discharge nozzle of organism oil groove 2 is connected with blender 5 by flow valve 3.
The discharge nozzle of blender 5 is connected with the first still kettle 6 feed-pipes, and the shore pipe of the first still kettle 6 bottoms is connected with vanadium accumulator tank 7.The vapor pipe at the first distillation tower 6 tops is connected with packing tower 8, and packing tower 8 top vapor pipes are connected with the first condenser 9, and the first condenser 9 discharge nozzles are connected with work in-process tank 10.
The discharge nozzle of work in-process tank 10 is connected with valve tray column 11, valve tray column 11 bottoms are provided with after-fractionating still 61, the vapor pipe at valve tray column 11 tops is connected with the second condenser 91, and the discharge nozzle of the second condenser 91 is connected with silicon accumulator tank 71, and silicon accumulator tank 71 is connected with valve tray column.
The discharge nozzle of valve tray column 11 is connected with after-fractionating still 61, the vapor pipe of after-fractionating still 61 is connected with the 3rd condenser 92, the 3rd condenser 92 is connected with the 3rd still kettle 62, the 3rd still kettle 62 connects vapor pipe and is connected with essence steaming tower 13, the liquid titanium tetrachloride delivery pipe A that essence is steamed tower 13 bottoms is connected with the 3rd condenser 93, and the discharge nozzle of the 3rd condenser 93 is connected with finished pot 12.
Essence is steamed tower 13, comprises tower body 31, water pump 32, air compressor machine 33, steam boiler 34 etc.In its tower body 31, be provided with multiple sieve plate 35, between sieve plate 35, be filled with copper wire balls 36.Tower body 31 bottoms and tower body 31 sides are all connected with Y-tube (37,38), and the Y-tube 37 of described tower body 31 bottoms is connected with liquid titanium tetrachloride bleed valve A and water discharge valve B respectively.The Y-tube 38 of described tower body 31 sides enters valve C with crude titanic chloride respectively and dry air valve D is connected, and dry air valve D is connected with instrument air dryer 39 through pipeline, and instrument air dryer 39 is connected with air compressor machine 33.Tower body 31 tops are connected with four-way pipe 310, four-way pipe 310 is connected with steam valve E, water inlet pipe 311, vent valve F respectively, wherein water inlet pipe 311 is connected with water-vapor exchange threeway 312 through pipeline, water-vapor exchange threeway one end is connected with water pump 32 water outlets through water intaking valve G, water-vapor exchange threeway 312 the other ends are connected with air compressor machine 33 exhaust nozzles through pressure lock H, and steam valve E is connected with steam boiler 34 through steam-pipe.
Below the refining example of this titanium tetrachloride:
Embodiment 1: thick TiCl
4by thick titanium header tank 1, in flow valve 3 is sent into well heater 4, well heater 4 makes thick TiCl
4be heated to 120 DEG C, subsequently thick TiCl
4be sent in blender 5, by 2 parts of 100 parts of paraffin oils, 80 parts of saturated fatty acids, Ursol D, 2,2,4-trimethylammonium 1,0.3 part of 2-dihydro quinoline polymer is made mixed organic solvents and is sent in blender 5, mixed organic solvents and hot TiCl in blender 5
4blending ratio be 1:1, paraffin oil, saturated fatty acid can carbonization form gac by VOCl
3reduce and adsorb other impurity, Ursol D, 2,2,4-trimethylammonium 1,2-dihydro quinoline polymerization physical efficiency control speed of response and contribute to thick TiCl
4in impurity separate out, material is sent in the first still kettle 6 and is distilled subsequently, most of enters vanadium slush-pit launder 7, TiCl containing foreign matter of vanadium by the shore pipe of the first still kettle 6 bottoms
4steam and partial impurities enter packing tower 8 and the first condenser 9 successively from the vapor pipe at the first still kettle 6 tops, form liquid work in-process and are stored in work in-process tank 10.
Material in work in-process tank 10 is added in tower by valve tray column 11 tops, and valve tray column 11 is heated to 60 DEG C of (SiCl
4boiling point), the SiCl of generation
4steam moves up gradually, TiCl
4downward liquid flow, SiCl
4steam is sent in silicon accumulator tank 71 after entering the second condenser 91 condensations; Not containing SiCl
4tiCl
4enter in after-fractionating still 61 TiCl in after-fractionating still from valve tray column 11 bottoms
4steam enters the 3rd still kettle 62 after the 3rd condensing tube condensation 92, carries out next step refine and removing vanadium processing.
Containing vanadium TiCl
4steam is sent into essence through the 3rd still kettle 62 and is steamed in tower 13, TiCl
4gas steams by essence the copper ball 33 being rolled into by copper wire in tower 13 continuously and contacts, and its contained foreign matter of vanadium is deposited on copper wire surface, the TiCl after refining
4steamed the TiCl of tower 13 bottoms by essence
4bleed valve A delivers to the 4th condenser 93 condensations, is housed in finished pot 12.
Embodiment 2: thick TiCl
4by thick titanium header tank 1, in flow valve 3 is sent into well heater 4, well heater 4 makes thick TiCl
4be heated to 130 DEG C, subsequently thick TiCl
4be sent in blender 5; By 3 parts of 100 parts of paraffin oils, 90 parts of saturated fatty acids, Ursol D, 2,2,4-trimethylammonium 1,0.4 part of 2-dihydro quinoline polymer is made mixed organic solvents and is sent in blender 5, mixed organic solvents and hot TiCl in blender 5
4blending ratio be 1:1, paraffin oil, saturated fatty acid can carbonization form gac by VOCl
3reduce and adsorb other impurity, Ursol D, 2,2,4-trimethylammonium 1,2-dihydro quinoline polymerization physical efficiency control speed of response and contribute to thick TiCl
4in impurity separate out, material is sent in the first still kettle 6 and is distilled subsequently, most of enters vanadium slush-pit launder 7, TiCl containing foreign matter of vanadium by the shore pipe of the first still kettle 6 bottoms
4steam and partial impurities enter packing tower 8 and the first condenser 9 successively from the vapor pipe at the first still kettle 6 tops, form liquid work in-process and are stored in work in-process tank 10.
Material in work in-process tank 10 is added in tower by valve tray column 11 tops, and valve tray column 11 is heated to 80 DEG C of (SiCl
4boiling point), the SiCl of generation
4steam moves up gradually, TiCl
4downward liquid flow, SiCl
4steam is sent in silicon accumulator tank 71 after entering the second condenser 91 condensations; Not containing SiCl
4tiCl
4enter in after-fractionating still 61 TiCl in after-fractionating still from valve tray column 11 bottoms
4steam enters the 3rd still kettle 62 after the 3rd condensing tube condensation 92, carries out next step refine and removing vanadium processing.
Containing vanadium TiCl
4steam is sent into essence through the 3rd still kettle 62 and is steamed in tower 13, TiCl
4gas steams by essence the copper ball 33 being rolled into by copper wire in tower 13 continuously and contacts, and its contained foreign matter of vanadium is deposited on copper wire surface, the TiCl after refining
4steamed the TiCl of tower 13 bottoms by essence
4bleed valve A delivers to the 4th condenser 93 condensations, is housed in finished pot 12.
Embodiment 3: thick TiCl
4by thick titanium header tank 1, in flow valve 3 is sent into well heater 4, well heater 4 makes thick TiCl
4be heated to 140 DEG C, subsequently thick TiCl
4be sent in blender 5; By 4 parts of 100 parts of paraffin oils, 100 parts of saturated fatty acids, Ursol D, 2,2,4-trimethylammonium 1,0.5 part of 2-dihydro quinoline polymer is made mixed organic solvents and is sent in blender 5, mixed organic solvents and hot TiCl in blender 5
4blending ratio be 1:1, paraffin oil, saturated fatty acid can carbonization form gac by VOCl
3reduce and adsorb other impurity, Ursol D, 2,2,4-trimethylammonium 1,2-dihydro quinoline polymerization physical efficiency control speed of response and contribute to thick TiCl
4in impurity separate out, material is sent in the first still kettle 6 and is distilled subsequently, most of enters vanadium slush-pit launder 7, TiCl containing foreign matter of vanadium by the shore pipe of the first still kettle 6 bottoms
4steam and partial impurities enter packing tower 8 and the first condenser 9 successively from the vapor pipe at the first still kettle 6 tops, form liquid work in-process and are stored in work in-process tank 10.
Material in work in-process tank 10 is added in tower by valve tray column 11 tops, and valve tray column 11 is heated to 100 DEG C of (SiCl
4boiling point), the SiCl of generation
4steam moves up gradually, TiCl
4downward liquid flow, SiCl
4steam is sent in silicon accumulator tank 71 after entering the second condenser 91 condensations; Not containing SiCl
4tiCl
4enter in after-fractionating still 61 TiCl in after-fractionating still from valve tray column 11 bottoms
4steam enters the 3rd still kettle 62 after the 3rd condensing tube condensation 92, carries out next step refine and removing vanadium processing.
Containing vanadium TiCl
4steam is sent into essence through the 3rd still kettle 62 and is steamed in tower 13, TiCl
4gas steams by essence the copper ball 33 being rolled into by copper wire in tower 13 continuously and contacts, and its contained foreign matter of vanadium is deposited on copper wire surface, the TiCl after refining
4steamed the TiCl of tower 13 bottoms by essence
4bleed valve A delivers to the 4th condenser 93 condensations, is housed in finished pot 12.
Finally, it should be pointed out that above embodiment is only the more representational example of the present invention.Obviously, the invention is not restricted to above-mentioned embodiment, can also have many distortion.Any simple modification, equivalent variations and modification that every foundation technical spirit of the present invention is done above embodiment, all should think and belong to protection scope of the present invention.
Claims (5)
1. a titanium tetrachloride process for purification, is characterized in that comprising the following steps:
(1) by thick TiCl
4sent in interchanger thick TiCl in interchanger by header tank
4be heated to 120-140 DEG C, with the thick TiCl of after heat
4be sent in blender;
(2) by 100 parts of paraffin oils, saturated fatty acid 80-100 part, Ursol D 2-4 part, 2,2,4-trimethylammonium 1,2-dihydro quinoline polymer 0.3-0.5 part is made mixed organic solvents and is sent in above-mentioned blender, mixed organic solvents and hot TiCl
4, blending ratio is 1:1, and mixture is sent in the first still kettle and distilled, and keeps distillation temperature in the kettle at 140-150 DEG C, most of foreign matter of vanadium that contains enters vanadium accumulator tank, TiCl by the shore pipe of the first still kettle bottom
4steam and portion gas impurity enter packing tower and the first condenser successively from the vapor pipe at the first still kettle top, form liquid work in-process and are stored in work in-process tank;
(3) the thick TiCl in work in-process tank
4added in tower by valve tray column middle and upper part, valve tray column is heated to 60-100 DEG C, lower boiling SiCl
4be vaporized and become steam and move up, send in silicon accumulator tank after entering the second condenser condenses, high boiling titanium tetrachloride moves down from valve tray column bottom and enters after-fractionating still, carries out next step refine and removing vanadium processing;
(4) containing vanadium TiCl
4after after-fractionating still is by the 3rd condenser condenses, send into the 3rd still kettle, through the 3rd still kettle by TiCl
4steam is sent into essence and is steamed in tower, TiCl
4steam by contacting except the copper ball being rolled into by copper wire in vanadium tower, is deposited on copper wire surface its contained foreign matter of vanadium continuously, the TiCl after refining
4by the TiCl of brass wire tower bottom
4bleed valve is delivered to the 4th condenser condenses, is housed in finished pot, and vanadium-containing water is delivered to vanadium accumulator tank by brass wire tower bottom discharge valve.
2. realize a titanium tetrachloride refining device for titanium tetrachloride process for purification described in claim 1, comprise that thick titanium header tank, mineral oil groove, flow valve, well heater, blender, still kettle, packing tower, valve tray column, condenser, essence steam tower; The discharge nozzle that it is characterized in that thick titanium header tank is connected with the feed-pipe of well heater by flow valve, and the discharge nozzle of interchanger is connected with blender; The discharge nozzle of mineral oil groove is connected with blender by flow valve, the discharge nozzle of blender is connected with the first still kettle feed-pipe, the vapor pipe at the first distillation tower top is connected with packing tower, and packing tower top vapor pipe is connected with the first condenser, and the first condenser discharge nozzle is connected with work in-process tank; The discharge nozzle of work in-process tank is connected with valve tray column, the discharge nozzle of valve tray column bottom is connected with after-fractionating still, after-fractionating still discharge port Guan Yu tri-condenser opening for feeds connect, the 3rd condenser discharge port is connected with the 3rd still kettle, the 3rd still kettle is steamed tower with essence and is connected, essence is steamed tower bottom discharge port and is connected with the 4th condenser, and the discharge nozzle of the 4th condenser is connected with finished pot;
3. titanium tetrachloride refining device according to claim 2, is characterized in that the shore pipe of described the first still kettle bottom is connected with vanadium accumulator tank;
4. titanium tetrachloride refining device according to claim 2, it is characterized in that described valve tray column bottom is provided with after-fractionating still, valve tray column top is provided with vapor pipe, vapor pipe is connected with the second condenser, the discharge nozzle of the second condenser is connected with silicon accumulator tank, and silicon accumulator tank top is connected with valve tray column;
5. titanium tetrachloride refining device according to claim 2, is characterized in that described essence steaming tower, comprises tower body, water pump, air compressor machine, steam boiler, in described tower body, is provided with multiple sieve plate, is filled with copper wire balls between sieve plate; Tower body bottom and tower body side are all connected with Y-tube, and the Y-tube of described tower body bottom is connected with liquid titanium tetrachloride bleed valve and water discharge valve respectively; The Y-tube of described tower body side enters valve with crude titanic chloride respectively and dry air valve is connected, and dry air valve is connected with instrument air dryer through pipeline, and instrument air dryer is connected with air compressor machine; Tower body top is connected with four-way pipe, four-way pipe is connected with steam valve, water inlet pipe, vent valve respectively, wherein water inlet pipe is connected with water-vapor exchange threeway through pipeline, water-vapor exchange threeway one end is connected with pump outlet through water intaking valve, the water-vapor exchange threeway the other end is connected with air compressor machine exhaust nozzle through pressure lock, and steam valve is connected with steam boiler through steam-pipe.
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| CN109956498A (en) * | 2019-04-29 | 2019-07-02 | 渤海大学 | A kind of crude titanic chloride efficiently removes vanadium compounding organic matter and preparation method thereof |
| CN110040772A (en) * | 2019-04-29 | 2019-07-23 | 渤海大学 | A kind of crude titanic chloride is stable except vanadium compounding organic matter and preparation method thereof |
| CN110054217A (en) * | 2019-04-29 | 2019-07-26 | 渤海大学 | Crude titanic chloride quickly removes vanadium compounding organic matter and preparation method thereof |
| CN110054218A (en) * | 2019-04-29 | 2019-07-26 | 渤海大学 | A kind of more impurity collaboration depth removal compounding organic matters and preparation method thereof of crude titanic chloride |
| KR102017682B1 (en) * | 2018-02-27 | 2019-09-03 | 고등기술연구원연구조합 | Purification method for titanium tetrachloride |
| CN111087017A (en) * | 2018-10-24 | 2020-05-01 | 中国石油化工股份有限公司 | Method for removing vanadium from crude titanium tetrachloride |
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| CN112758977A (en) * | 2020-12-31 | 2021-05-07 | 仙桃市中星电子材料有限公司 | Method for reducing content of tin titanium tetrachloride |
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Application publication date: 20141210 |