CN107935042A - One kind is used to remove VOCl3Middle TiCl4System and method - Google Patents

One kind is used to remove VOCl3Middle TiCl4System and method Download PDF

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Publication number
CN107935042A
CN107935042A CN201711328415.1A CN201711328415A CN107935042A CN 107935042 A CN107935042 A CN 107935042A CN 201711328415 A CN201711328415 A CN 201711328415A CN 107935042 A CN107935042 A CN 107935042A
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China
Prior art keywords
vocl
storage tank
pocl
purifying column
ticl
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CN201711328415.1A
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Inventor
韩志彪
邓君
曹志成
冯鲁兴
员晓
刘亮
唐敬坤
吴道洪
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Jiangsu Province Metallurgical Design Institute Co Ltd
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Jiangsu Province Metallurgical Design Institute Co Ltd
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Priority to CN201711328415.1A priority Critical patent/CN107935042A/en
Publication of CN107935042A publication Critical patent/CN107935042A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/18—Absorbing units; Liquid distributors therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26—Drying gases or vapours
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26—Drying gases or vapours
    • B01D53/28—Selection of materials for use as drying agents
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Treating Waste Gases (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

It is used to remove VOCl the present invention provides one kind3Middle TiCl4System, the system include reaction purifying column, POCl3Feed arrangement, thick VOCl3Feed arrangement, N2Purifier and VOCl3Condense refining plant.Present invention also offers remove VOCl using said system3Middle TiCl4Method.The technological operation of the system and method for the present invention is easy, suitable for large-scale industrial production, TiCl4The removal effect of impurity is good, and the product of whole process can recycle, and be nearly free from discarded object, meet the requirement of circular economy.

Description

One kind is used to remove VOCl3Middle TiCl4System and method
Technical field
This patent disclosure relates generally to for removing VOCl3Middle TiCl4System and method.
Background technology
There are many vanadium extractions of chlorination containing vanadium raw materials and chlorizate VOCl at present3Prepare high-purity V2O5Relevant report.But it is worth It is noted that except containing 10~20% V in the vanadium slag of converter extracting vanadium output2O5Outside, also containing 10% or so TiO2。 Under the conditions of vanadium slag carburizing chlorination, TiO2Also it is chlorinated, the TiCl of generation4Into thick VOCl3, this will necessarily reduce VOCl3And V2O5The purity of product.However, existing vanadium slag chlorination vanadium extraction correlation technique removes VOCl almost without offer3In TiCl4's Method.And will be with the VOCl of vanadium slag chlorination output3High-purity V is prepared for raw material2O5, just must fully remove TiCl4。
Existing production practices have fully shown that rectifying cannot efficiently separate VOCl3And TiCl4, it is thus impossible to use rectifying Method removes VOCl3In TiCl4。
The content of the invention
It is used to remove VOCl the object of the present invention is to provide one kind3Middle TiCl4System and method.
It is disclosed by the invention to be used to remove VOCl3Middle TiCl4System include：
Purifying column is reacted, agitating device, heating unit and filtration apparatus are provided with its reative cell, filtration apparatus, which is located at, to be stirred Mix the lower section of device and heating unit；
POCl3Feed arrangement, it includes POCl3Storage tank, POCl3Storage tank is connected with reaction purifying column；
Thick VOCl3Feed arrangement, it includes thick VOCl3Storage tank, thick VOCl3Storage tank is connected with reaction purifying column；
N2Purifier, it includes N2Drying device, compressor and high pressure N2Storage tank, high pressure N2Storage tank is purified with reaction Tower connects；And
VOCl3Refining plant is condensed, it includes condensing tower and essence VOCl3Storage tank, import and the reaction purifying column of condensing tower Outlet connection, the outlet of condensing tower and essence VOCl3Storage tank connects.
In a preferred embodiment of the invention, N2Drying device includes compressor and drying tower.
In a preferred embodiment of the invention, which further comprises tail gas absorption tank, and condensing tower further includes out Gas port, the gas outlet of condensing tower are connected with the air inlet of tail gas absorption tank, the gas outlet of tail gas absorption tank and N2Drying device Compressor connects.
In a preferred embodiment of the invention, POCl3Storage tank, VOCl3Storage tank, high pressure N2Storage tank, reaction purifying column with And the outlet of condensing tower is equipped with control valve.
In a preferred embodiment of the invention, POCl3Spinner flowmeter is equipped between storage tank and reaction purifying column, slightly VOCl3Spinner flowmeter also is provided between storage tank and reaction purifying column.
In a preferred embodiment of the invention, heating unit is annular coil pipe, its be located at the top 3 of filtration apparatus~ At 10cm, agitating device is located above heating coil at 5~10cm, and reaction purification tower height degree is 1.5~3.5 with diameter ratio, only It is 0.02~0.1 to change tower outlet diameter d and purification tower body diameter D ratios.
In a preferred embodiment of the invention, the drier in drying tower includes but not limited to soda lime, silica gel, dense Sulfuric acid, P2O5Deng.
According to another aspect of the present invention, there is provided one kind removes VOCl3Middle TiCl4Method, this method includes following step Suddenly：
1) in proportion by POCl3POCl in storage tank3And VOCl3VOCl in storage tank3Reaction purifying column is introduced respectively In reative cell；
2) POCl that will be added using heating unit in step 1)3And VOCl3Heating, while stirred using agitating device Mix；
3) stood after stirring；
4) it is passed through N to reative cell top2Carry out pressure filtration；
5) filtrate is made to flow into condensing tower and by the VOCl of volatilization3Gas is condensed into liquid；
6) liquid in condensing tower is made to flow into essence VOCl3Storage tank.
In a preferred embodiment of the invention, POCl in step 1)3And VOCl3Molar ratio be (1.02~1.06): 1。
In a preferred embodiment of the invention, the temperature in step 2) after heating is 40~60 DEG C；And/or stirring Rotating speed is 50~200 turns/min, and mixing time is 20~40min.
In a preferred embodiment of the invention, time of repose is 120~240min in step 3).
In a preferred embodiment of the invention, the N of step 4) pressure filtration2Pressure is controlled in 0.5~1MPa, and/ Or step 5) condensation is that gas phase is cooled to 5~15 DEG C using brine ice.
In a preferred embodiment of the invention, N used during pressure filtration2It is the N by dry and pressurized treatments2, its Middle N2Moisture content is below 0.2%.
In a preferred embodiment of the invention, this method further comprises leading to the gas that condensing tower gas outlet is discharged Enter tail gas absorption tank, the gas that tail gas absorption tank is discharged is returned to N afterwards2Drying device is recycled.
In a preferred embodiment of the invention, tail gas absorption can use alkaline solution, and alkaline solution is included but not It is limited to ammonium hydroxide, sodium hydroxide, potassium hydroxide etc..
In a preferred embodiment of the invention, this method further comprises filtering gained filter mud being heated to 140 DEG C It is set to be decomposed into TiCl4And POCl3, carry out condensation and TiCl be separately recovered4And POCl3。
By using the systems and methods of the present invention, following multiple beneficial effect can be obtained：
(1) technological operation is easy, suitable for large-scale industrial production, TiCl4The removal effect of impurity is good；
(2) product that cleans is in solid phase, it is easy to and VOCl3Liquid separates, and can obtain high-purity VOCl3, can be directly used for Chemical industry prepares high-purity V2O5；
(3) composition of removal of impurities gained solid product is very simple, can recycle；
(4) product of whole process can recycle, and be nearly free from discarded object, meet the requirement of circular economy.
Brief description of the drawings
Fig. 1 shows according to an embodiment of the invention for removing VOCl3Middle TiCl4System schematic diagram；
Fig. 2 shows according to an embodiment of the invention for removing VOCl3Middle TiCl4Method flow signal Figure.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to specific embodiment and attached Figure, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only explaining this hair It is bright, it is not intended to limit the present invention.
It has been investigated that TiCl4With VOCl3Mixed system in be not present stable compound, and POCl3Can and TiCl4 It is combined into TiCl4·POCl3And TiCl4·2POCl3, both fusing points are respectively 110 DEG C and 107 DEG C, and VOCl3Fusing point for- 78.9 DEG C, this shows the VOCl in a certain temperature range3It is in a liquid state and TiCl4·POCl3And TiCl4·2POCl3Consolidate in stable State.Therefore POCl can be utilized3By VOCl3In TiCl4Precipitation, then separated both with the method for filtering, so as to effectively remove VOCl3In TiCl4, significantly improve VOCl3Purity.On the other hand, VOCl3Even if trace P OCl is remained in3, also can be VOCl3Oxidation prepares high-purity V2O5During be oxidized to P2O5And be volatized into gas phase, so not interfering with V2O5Product Purity.
Conceived based on foregoing invention, the present invention provides a kind of for removing VOCl3Middle TiCl4System.As described in Figure 1, should System includes reaction purifying column 10, POCl3Storage tank 6, thick VOCl3Storage tank 5, N2Purifier and VOCl3Condense refining plant.
Reaction purifying column 10 includes POCl3Feed inlet, thick VOCl3Feed inlet (POCl in this embodiment3Feed inlet and thick VOCl3Feed inlet shares a feed inlet), high pressure N2Entrance, filtrate (liquid, blender 12, filter bed 14, heater 11, reaction Room, thermometer 9 and liquid level gauge 13.POCl3Feed inlet and high pressure N2For entrance positioned at reaction purifying column top, heater 11 is ring Shape coil pipe, at more than filter bed 12 3~10cm, blender 12 is located at more than 11 5-10cm of heating coil, and reaction is net The tower body height and tower body diameter ratio (H/D) for changing tower are 1.5~3.5, and the filtrate (liquid of reaction purifying column 10 is equipped with valve, with control Equipment pressure and speed during pressure filtration processed, filtrate (liquid are connected with the import of condensing tower 15, the diameter of purifying column outlet Ratio (d/D) with tower body diameter is 0.05~0.3.
N2Purifier includes sequentially connected air compressor 1, drier 2, air compressor 3, high pressure N2Storage tank 4.It is high Press N2The outlet of storage tank 4 is equipped with control valve and the high pressure N with reacting purifying column2Entrance is connected.
POCl3Feed arrangement includes POCl3Storage tank 6, flowmeter 7 and control valve.POCl3The outlet of storage tank 6 is equipped with control valve, To control POCl3Inlet amount.POCl3The POCl of outlet and reaction purifying column 103Feed inlet is connected.
Thick VOCl3Feed arrangement includes thick VOCl3Storage tank 5, control valve and flowmeter 8, VOCl3The outlet of storage tank 5 with it is anti- Answer the VOCl of purifying column 103Feed inlet is connected.
VOCl3Condensing refining plant includes condensing tower 15, essence VOCl3Storage tank 16 and tail gas absorption fill 17.Condensing tower 15 Outlet of the import with reacting purifying column 10 is connected, outlet and the essence VOCl of condensing tower 153Storage tank 16 is connected, the outlet of condensing tower 15 The air inlet that mouth fills 17 with tail gas absorption is connected, and the gas outlet that tail gas absorption fills 17 is connected with the air inlet of compressor 1.
Fig. 2 is to remove VOCl using said system3Middle TiCl4Method flow chart.It is generally included to thick VOCl3In Add POCl3So that TiCl therein4With POCl3It is combined into TiCl4·POCl3And TiCl4·2POCl3, after through stand and mistake Filter isolated essence VOCl3And filter residue.
The thick VOCl that the present invention mentions3The including but not limited to product of the chlorination containing vanadium raw materials, thick VOCl3Molar fraction one As be 60~90%.Can also be product of the above-mentioned chlorizate after rectifying, preferably VOCl3Molar fraction be not less than 90%, TiCl4Mole percent be 0.1%~10%.
To thick VOCl3Middle addition POCl3After need stirring mixture to promote POCl3And TiCl4Impurity is fully combined into solid The TiCl of state4·POCl3And TiCl4·2POCl3, while 40~60 DEG C are heated the mixture to, the excessive system of heating-up temperature is waved Hair is serious, and the too low system viscosity of temperature is excessive, is unfavorable for follow-up solid-liquor separation.Stand to promote POCl3And TiCl4Impurity is abundant It is combined into solid TiCl4·POCl3And TiCl4·2POCl3.In reaction process, the valve of reaction purifying column outlet is closed.
In filtering by the way of pressure filtration.Concrete operations are after insulation, open purification tower reactor 10 The valve of outlet, dry N is passed through by the top of purifying column 102, VOCl will be suspended in3Solid impurity in liquid is filtered with organic phase Membrane filtration removes.Due to VOCl3Volatile, suction filtration easily causes VOCl3A large amount of volatilizations, are unfavorable for collecting, so the present invention uses The mode of press filtration is accelerated to filter.N in purifying column in pressure-filtering process2Pressure control is in 0.5~1MPa, until after pressure-filtering process Close N2Valve.Filtering gained filter mud main component is TiCl4·POCl3And TiCl4·2POCl3, it can divide at 140 DEG C or so Solve as TiCl4And POCl3, TiCl4And POCl3It is gaseous state, it is condensed, TiCl can be separately recovered4And POCl3。
In order to improve VOCl3Yield, the VOCl that will be obtained by filtration3Solution is passed through condensing tower 15.Set in condensing tower cold Solidifying pipe, is cooled to 5~15 DEG C by gas phase with brine ice, promotes the VOCl in gas phase3Fully it is condensed into liquid.Final gained VOCl3 Middle TiCl4Mole percent be 0.01~0.05%, meet high-purity V2O5Ingredient requirement.
The product that cleans is mainly solid-state TiCl4·POCl3And TiCl4·2POCl3, can further handle, be separately recovered TiCl4And POCl3.The tail gas main component escaped from condensing tower 15 is N2, contain a small amount of uncooled VOCl3Gas, tail gas are inhaled Receipts can use alkaline solution, include but not limited to ammonium hydroxide, sodium hydroxide, potassium hydroxide etc..Tail gas passes through in tourie 17 After lye absorbs, N2Press filtration process can be returned to after 2 purge drying of air compressor machine 1 and drying tower, absorbing liquid can be returned further Receive vanadium.Whole dedoping step is discharged almost without discarded object, meets the requirement of circular economy.
The removing VOCl that the present invention will be described in detail in embodiment below3Middle TiCl4System and method.
Embodiment 1
N2Dehydrated by air compressor machine 1 and drying tower 2, it is desirable to dewatered N2Moisture content is 0.1%, Ran Houtong Overcompression machine 3 is stored in high pressure N after being pressurized2It is spare in storage tank 4.First by POCl3By POCl3Storage tank 6 and spinner flowmeter 7 draw Enter purifying column 10, then will contain TiCl4The thick VOCl of impurity3By VOCl3Storage tank 5 introduces purifying column 10, control through spinner flowmeter 8 Make the POCl added3And TiCl4The molar ratio of impurity is 1.02:1, then 40 DEG C are heated the mixture to by heating tube 11.Stir The rotating speed for mixing device 12 is 50 turns/min, mixing time 20min.120min is stood after stirring.By purifying after insulation The top of tower 10 is passed through dry N2, VOCl will be suspended in3Solid impurity organic phase filter membrane 14 in liquid is filtered to remove.Press filtration During N2Pressure is 0.5MPa.With condenser pipe by the gas cooling that purifying column 10 is discharged to 5 DEG C, promote the VOCl in gas phase3Fill Condensation is divided to enter essence VOCl3In storage tank 16.Tail gas main component after the absorption of tourie 17 is N2, use can be recycled.
Smart VOCl after the above method is handled3In TiCl4Mole percent be 0.05%.
Embodiment 2
N2Dehydrated by air compressor machine 1 and drying tower 2, it is desirable to dewatered N2Moisture content is 0.2%, Ran Houtong Overcompression machine 3 is stored in high pressure N after being pressurized2It is spare in storage tank 4.First by POCl3By POCl3Storage tank 6 and spinner flowmeter 7 draw Enter purifying column 10, then will contain TiCl4The thick VOCl of impurity3Purifying column 10 is introduced through spinner flowmeter 8 by storage tank 5, control adds POCl3And TiCl4The molar ratio of impurity is 1.06:1, then 60 DEG C are heated the mixture to by heating tube 11.12 turns of blender Speed 200 turns/min, mixing time 40min.240min is stood after stirring.It is dry by being passed through at the top of purifying column 10 after insulation Dry N2, VOCl will be suspended in3Solid impurity organic phase filter membrane 14 in liquid is filtered to remove.N in pressure-filtering process2Pressure is 1MPa.With condenser pipe by the gas cooling that purifying column 10 is discharged to 15 DEG C, promote the VOCl in gas phase3Fully condensation enters essence VOCl3In storage tank 16.Tail gas main component after the absorption of tourie 17 is N2, use can be recycled.
Smart VOCl after the above method is handled3Middle TiCl4Mole percent be 0.01%.
Embodiment 3
N2Dehydrated by air compressor machine 1 and drying tower 2, it is desirable to dewatered N2Moisture content is 0.1%, Ran Houtong Overcompression machine 3 is stored in high pressure N after being pressurized2It is spare in storage tank 4.First by POCl3By POCl3Storage tank 6 and spinner flowmeter 7 draw Enter purifying column 10, then will contain TiCl4The thick VOCl of impurity3Purifying column 10 is introduced through spinner flowmeter 8 by storage tank 5, control adds POCl3And TiCl4The molar ratio of impurity is 1.03:1, then 50 DEG C are heated the mixture to by heating tube 11.Blender turns Speed 100 turns/min, mixing time 30min.180min is stood after stirring.It is dry by being passed through at the top of purifying column 10 after insulation Dry N2, VOCl will be suspended in3Solid impurity organic phase filter membrane 14 in liquid is filtered to remove.N in pressure-filtering process2Pressure is 0.7MPa.With condenser pipe by the gas cooling that purifying column 10 is discharged to 10 DEG C, promote the VOCl in gas phase3Fully condensation enters essence VOCl3In storage tank 16.Tail gas main component after the processing of tourie 17 is N2, use can be recycled.
Smart VOCl after the above method is handled3Middle TiCl4Mole percent be 0.03%.
Embodiment described above only expresses embodiments of the present invention, its description is more specific and detailed, but can not Therefore it is interpreted as the limitation to the scope of the claims of the present invention.It should be pointed out that for those of ordinary skill in the art, Without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection model of the present invention Enclose.

Claims (10)

1. one kind is used to remove VOCl3Middle TiCl4System, it is characterised in that the system comprises：
Purifying column is reacted, agitating device, heating unit and filtration apparatus are provided with its reative cell, filtration apparatus is filled positioned at stirring Put the lower section with heating unit；
POCl3Feed arrangement, it includes POCl3Storage tank, POCl3Storage tank is connected with reaction purifying column；
Thick VOCl3Feed arrangement, it includes thick VOCl3Storage tank, thick VOCl3Storage tank is connected with reaction purifying column；
N2Purifier, it includes N2Drying device, compressor and high pressure N2Storage tank, high pressure N2Storage tank connects with reaction purifying column Connect；And
VOCl3Refining plant is condensed, it includes condensing tower and essence VOCl3Storage tank, the import of condensing tower and going out for reaction purifying column Mouth connection, outlet and the essence VOCl of condensing tower3Storage tank connects.
2. system according to claim 1, it is characterised in that the N2Drying device includes compressor and drying tower.
3. system according to claim 2, it is characterised in that the system further comprises tail gas absorption tank, condensing tower Including gas outlet, the gas outlet of condensing tower is connected with the air inlet of tail gas absorption tank, the gas outlet of tail gas absorption tank and N2It is dry The compressor connection of device.
4. system according to claim 2, it is characterised in that POCl3Storage tank, VOCl3Storage tank, high pressure N2Storage tank, reaction are net The outlet for changing tower and condensing tower is equipped with control valve.
5. system according to claim 2, it is characterised in that POCl3Spinner is equipped between storage tank and reaction purifying column Meter, thick VOCl3Spinner flowmeter also is provided between storage tank and reaction purifying column.
6. a kind of system using as described in claim 1-5 removes VOCl3Middle TiCl4Method, it is characterised in that include The following steps：
1) in proportion by POCl3POCl in storage tank3And VOCl3VOCl in storage tank3The reaction of reaction purifying column is introduced respectively It is indoor；
2) POCl that will be added using heating unit in step 1)3And VOCl3Heating, while be stirred using agitating device；
3) stood after stirring；
4) it is passed through N to reative cell top2Carry out pressure filtration；
5) filtrate is made to flow into condensing tower and by the VOCl of volatilization3Gas is condensed into liquid；
6) liquid in condensing tower is made to flow into essence VOCl3Storage tank.
7. according to the method described in claim 6, it is characterized in that, POCl in step 1)3And VOCl3Molar ratio for (1.02~ 1.06):1。
8. according to the method described in claim 6, it is characterized in that, the temperature in step 2) after heating is 40~60 DEG C；And/or The rotating speed of stirring is 50~200 turns/min, and mixing time is 20~40min.
9. according to the method described in claim 6, it is characterized in that, time of repose is 120~240min in step 3).
10. the according to the method described in claim 6, it is characterized in that, N of step 4) pressure filtration2Pressure control 0.5~ 1MPa, and/or step 5) condensation is that gas phase is cooled to 5~15 DEG C using brine ice.
CN201711328415.1A 2017-12-13 2017-12-13 One kind is used to remove VOCl3Middle TiCl4System and method Pending CN107935042A (en)

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CN201711328415.1A CN107935042A (en) 2017-12-13 2017-12-13 One kind is used to remove VOCl3Middle TiCl4System and method

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Application Number Priority Date Filing Date Title
CN201711328415.1A CN107935042A (en) 2017-12-13 2017-12-13 One kind is used to remove VOCl3Middle TiCl4System and method

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112142106A (en) * 2020-09-29 2020-12-29 攀钢集团研究院有限公司 Method for separating titanium tetrachloride from vanadium oxytrichloride crude product

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112142106A (en) * 2020-09-29 2020-12-29 攀钢集团研究院有限公司 Method for separating titanium tetrachloride from vanadium oxytrichloride crude product
CN112142106B (en) * 2020-09-29 2022-05-24 攀钢集团研究院有限公司 Method for separating titanium tetrachloride from vanadium oxytrichloride crude product

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