CN106237671A - Process device and the sedimentation method of the crude titanic chloride containing higher solid formation impurity - Google Patents
Process device and the sedimentation method of the crude titanic chloride containing higher solid formation impurity Download PDFInfo
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- CN106237671A CN106237671A CN201610801273.5A CN201610801273A CN106237671A CN 106237671 A CN106237671 A CN 106237671A CN 201610801273 A CN201610801273 A CN 201610801273A CN 106237671 A CN106237671 A CN 106237671A
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- sedimentation
- concentrator
- titanic chloride
- crude titanic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/02—Settling tanks with single outlets for the separated liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/24—Feed or discharge mechanisms for settling tanks
- B01D21/2405—Feed mechanisms for settling tanks
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/24—Feed or discharge mechanisms for settling tanks
- B01D21/245—Discharge mechanisms for the sediments
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/28—Mechanical auxiliary equipment for acceleration of sedimentation, e.g. by vibrators or the like
- B01D21/286—Means for gentle agitation for enhancing flocculation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/30—Control equipment
- B01D21/34—Controlling the feed distribution; Controlling the liquid level ; Control of process parameters
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/02—Halides of titanium
- C01G23/022—Titanium tetrachloride
- C01G23/024—Purification of tetrachloride
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The device of a kind of crude titanic chloride for process containing higher solid formation impurity being titanium technical field of metallurgy industry disclosed by the invention and sedimentation method, this device includes concentrator, it is positioned at the spiral crane of concentrator bottom discharging mouth, and be used for the clear liquid storage tank of the solution after containing sedimentation and collect the slurry tank of settled mud, also include standing sedimentation pond and measuring tank, the top in described standing sedimentation pond is connected with measuring tank by pipeline, described measuring tank is connected to concentrator by pipeline, measuring tank is provided with flow valve and is accurately controlled the flow velocity of liquid entrance concentrator.First solution for solid impurity content >=25g/L carry out standing sedimentation process, then take upper clear supernate and carry out continuous overflow settlement treatment, this mode can directly process the crude titanic chloride of higher solid formation impurity, insoluble solids impurity in continuous-stable separation crude titanic chloride, is greatly improved production efficiency and the quality of production of titanium tetrachloride.
Description
Technical field
The present invention relates to titanium technical field of metallurgy industry, particularly relate to a kind of for processing containing higher solid formation impurity
The device of crude titanic chloride and sedimentation method.
Background technology
Specific strength is high, density is little, high temperature resistant excellent with cryogenic property, acid-alkali-corrosive-resisting etc. owing to having for metal titanium or titanium alloy
The opposite sex can, be widely used in the fields such as Aero-Space, derived energy chemical be metallurgical, civilian, titanium tetrachloride is as preparing titanium white chloride, sea
The important intermediate raw material of continuous titanium, because of chlorination while impurity element in titanium slag or titaniferous ore in its production process so that thick four
Impurity content in titanium chloride increases, if if impurity fails preferably to be removed in crude titanic chloride, then can exist with four times of concentration
Titanium sponge is enriched with, titanium sponge quality is produced extreme influence；Titanium slag for China's Panxi Diqu high contents of calcium and magnesium impurity content is former
Material is often adopted fused salt chlorimation method and is prepared crude titanic chloride, must remove through the sedimentation operation such as remove impurity, run affairs filter remove impurity, refining and edulcoration
AlCl3、FeCl3、SiCl4, the impurity such as VOCl3 to be to obtain up-to-standard refined titanic chloride for titanium sponge, the life of titanium white chloride
Produce.
At present, less to processing method, the research report of crude titanic chloride sedimentation both at home and abroad.Chinese invention patent
CN103505915A discloses a kind of titanium tetrachloride subsider and the method extracting supernatant liquid, and it focuses on introducing subsider
Structure.Chinese invention patent CN103191835A discloses one and comprises titanium-tetrachloride storage tank, casing, support, differential mechanism, electricity
The Titanium tetrachloride slag-liquid separation centrifugal machine of machine, its object is to solve sealing effectiveness during existing titanium tetrachloride solid-liquid separation
The technical problems such as difference, equipment attrition corrosion fast, operation expense height, serious environment pollution.And test proof and use subsider
Continuous sedimentation pattern is difficult to effectively process the crude titanic chloride that solid content is higher；Though centrifuge can realize thick tetrachloro at short notice
Change the insoluble solid formation impurity in titanium, but be difficult to continuous feeding and discharging and large-scale industrial production.
Summary of the invention
For making up the deficiencies in the prior art, the technical problem to be solved is: provide one to process containing higher
The device of the crude titanic chloride of solid formation impurity and sedimentation method.
The technical solution adopted for the present invention to solve the technical problems is: process the thick tetrachloro containing higher solid formation impurity
Change the device of titanium, the spiral crane including concentrator, being positioned at concentrator bottom discharging mouth and molten after containing sedimentation
The clear liquid storage tank of liquid and the slurry tank of collection settled mud, also include standing sedimentation pond and measuring tank, described standing sedimentation pond
Top is connected with measuring tank by pipeline, and described measuring tank is connected to concentrator by pipeline, and measuring tank is provided with flow valve can
Liquid with precise control enters the flow velocity of concentrator.
Described concentrator uses volume to be 55～66m3Model.
Process the sedimentation method of the crude titanic chloride containing higher solid formation impurity, comprise the following steps:
A, classifying crude titanic chloride by solid impurity content, content >=25g/L is divided into a class, content ＜ 25g/
L is divided into a class；
B, the solution of content ＜ 25g/L, first input measuring tank by solution, then feeds to concentrator and carries out continuous overflow
Settlement treatment；
C, the solution of content >=25g/L, before carrying out step b, first solution is put into standing sedimentation pond carry out standing heavy
Fall processes, and the Sedimentation tank top stillness of night was delivered to after sedimentation a period of time measuring tank, then carries out at continuous overflow sedimentation by b step
Reason；
Clear liquid after d, continuous overflow settlement treatment overflows from concentrator top, is delivered to clear liquid storage tank, the mud after sedimentation
Slurry is delivered to slurry tank by the spiral crane bottom Sedimentation tank and concentrator.
Further, when carrying out continuous overflow settlement treatment in stepb, from the charging rate of measuring tank to concentrator
Controlling 1.7～2.1t/h, the speed of rotation of concentrator agitator is 0.4～0.8rmp/min.
Further, the time that solution carries out in step c standing sedimentation process is carried out by y=0.0542x+0.85
Calculating, wherein, y is the standing sedimentation time, its unit be h, x be the solid impurity content of crude titanic chloride before sedimentation, its unit
For g/L.
Further, when step d carries out continuous overflow settlement treatment, spiral crane should be kept to work continuously, turn
Speed controls 5～15rmp/min, avoids concentrator inner bottom part mud to block drainage conduit.
The invention has the beneficial effects as follows: by adding standing sedimentation pond and measuring tank outside traditional concentrator, for solid
First the solution of body impurity content >=25g/L carry out standing sedimentation process, then takes upper clear supernate and carries out at continuous overflow sedimentation
Reason, this mode can directly process the crude titanic chloride of higher solid formation impurity, in continuous-stable separation crude titanic chloride not
Molten solid impurity, is greatly improved the production efficiency of titanium tetrachloride, effectively keeps away liquid delivery process because of impurity content higher band
Line clogging, simultaneously also greatly reduce distillating still resistance wire scaling loss frequency in crude titanic chloride subtractive process.
Accompanying drawing explanation
Fig. 1 is the structural representation of apparatus of the present invention.
Figure is labeled as, 1-concentrator, 2-screw elevator, 3-clear liquid storage tank, 4-slurry tank, 5-standing sedimentation pond, 6-
Measuring tank.
Detailed description of the invention
Below by way of the drawings and specific embodiments, the invention will be further described.
As it is shown in figure 1, the present invention processes the device of crude titanic chloride containing higher solid formation impurity, including concentrator 1,
It is positioned at the spiral crane 2 of concentrator 1 bottom discharging mouth and the clear liquid storage tank 3 of the solution after containing sedimentation and collects
The slurry tank 4 of settled mud, also includes standing sedimentation pond 5 and measuring tank 6, the top in described standing sedimentation pond 5 by pipeline with
Measuring tank 6 is connected, and described measuring tank 6 is connected to concentrator 1 by pipeline, and measuring tank 6 is provided with flow valve and is accurately controlled liquid
Body enters the flow velocity of concentrator.Traditional handicraft the most only carries out overflow by concentrator when carrying out titanium tetrachloride settlement treatment and sinks
Fall processes, but for the higher solution of solid impurity content, depends merely on concentrator effect of settling bad.The present invention is by arranging standing
Sedimentation tank first carries out preliminary sedimentation to solution, carries out overflow sedimentation the most again, is greatly improved overflow effect of settling, and passes through
Flow velocity is accurately controlled by measuring tank, can realize continuous overflow sedimentation, and production efficiency and quality are all significantly improved.According to reality
The border condition of production, general employing volume is 55～66m3Model, effect of settling is good, and production efficiency is high.
Process the sedimentation method of the crude titanic chloride containing higher solid formation impurity, comprise the following steps:
A, classifying crude titanic chloride by solid impurity content, content >=25g/L is divided into a class, content ＜ 25g/
L is divided into a class；
B, the solution of content ＜ 25g/L, first input measuring tank by solution, then feeds to concentrator and carries out continuous overflow
Settlement treatment；
C, the solution of content >=25g/L, before carrying out step b, first solution is put into standing sedimentation pond carry out standing heavy
Fall processes, and the Sedimentation tank top stillness of night was delivered to after sedimentation a period of time measuring tank, then carries out at continuous overflow sedimentation by b step
Reason；
Clear liquid after d, continuous overflow settlement treatment overflows from concentrator top, is delivered to clear liquid storage tank, the mud after sedimentation
Slurry is delivered to slurry tank by the spiral crane bottom Sedimentation tank and concentrator.
Find after long term test is analyzed, only when solid impurity content is less than 25g/L, directly carry out with concentrator
Overflow sedimentation can be only achieved effective effect of settling, for solid impurity content higher than 25g/L, should first carry out at standing sedimentation
Reason, makes fraction solids impurity sedimentation at the bottom of pond, and the clear liquid to top carries out overflow settlement treatment the most again, so can be only achieved pre-
The effect of settling of phase.
Further, when carrying out continuous overflow settlement treatment in stepb, from the charging rate control of measuring tank to concentrator
System is 1.7～2.1t/h, and the speed of rotation of concentrator agitator is 0.4～0.8rmp/min.Draw after test of many times, press
Charging rate and the rotating speed of 0.4～0.8rmp/min according to 1.7～2.1t/h are controlled, and can guarantee that the continuous fortune of concentrator
OK, effect of settling is good, can ensure that bottom mud has good mobility, it is simple to discharge simultaneously.
The time that solution carries out in step c standing sedimentation process is calculated by y=0.0542x+0.85, wherein, and y
For the standing sedimentation time, its unit be h, x be the solid impurity content of crude titanic chloride before sedimentation, its unit is g/L.It is heavy to stand
The fall time is also the conclusion drawn through life-time service and test, carries out settlement treatment according to this time, can reach optimal
Effect of settling and production efficiency.
When step d carries out continuous overflow settlement treatment, spiral crane should be kept to work continuously, rotating speed control 5～
15rmp/min, avoids concentrator inner bottom part mud to block drainage conduit.Screw elevator is mainly used for intermittent entering mud
Row cleaning, discharging period is 2 times/day～4 times/day, when not carrying out discharge operation, carries material spiral and rotates forward operation continuously,
Rotating speed is 5～15rmp/min, avoids concentrator inner bottom part mud to block drainage conduit.
Below by embodiment, the present invention is further described.
Embodiment 1
The solid content crude titanic chloride less than 25g/L is carried out continuous overflow sedimentation, and it is tied before and after controlling parameter and sedimentation
Fruit is as shown in table 1:
Solid content situation of change before and after table 1 excessive sedimentation continuously
It is 0.5rmp/min that continuous overflow infall process controls concentrator agitator speed, and inlet amount is 1.7～2t.h-1,
After sedimentation, crude titanic chloride solid content averagely reduces 2g/L, its value≤4g/L.
Embodiment 2
The crude titanic chloride that first solid impurity content be more than 25g/L carries out independent standing sedimentation process, result such as table 2
Shown in, the solid impurity content before sample A, B, C, D sedimentation is respectively 323g/L, 221g/L, 59.5g/L, 25.5g/L, divides quiet
After putting sedimentation 15h, 8h, 5h, 1.5h, the top stillness of night solid content of crude titanic chloride substantially reduces ,≤10g/L.
Solid content and composition before and after table 2 crude titanic chloride standing sedimentation
After using standing sedimentation, the crude titanic chloride stillness of night carries out continuous overflow sedimentation, reduces thick titanium solid content further, its
Result is as shown in table 3:
Solid content situation of change before and after table 3 excessive sedimentation continuously
Crude titanic chloride solid content≤4g/L after continuous overflow sedimentation.Standing sedimentation combines with continuous overflow sedimentation
Can effectively process the crude titanic chloride of higher solids impurity content, it is achieved solid-liquid efficiently separates.
Both examples above absolutely proves that this device and sedimentation method can effectively process the titanium tetrachloride of high solids content, institute
Obtain solid formation content≤4g/L in the crude titanic chloride stillness of night.After using the method to process, the crude titanic chloride of gained can be greatly improved
Production efficiency, effectively keep away line clogging that liquid delivery process comes because of impurity content higher band, greatly reduce crude titanic chloride essence
Distillating still resistance wire scaling loss frequency during system, has good practicality and application prospect.
Claims (6)
1. process the device of the crude titanic chloride containing higher solid formation impurity, including concentrator (1), be positioned at concentrator (1) end
The spiral crane (2) of portion's discharge gate and the clear liquid storage tank (3) of the solution after containing sedimentation and collection settled mud
Slurry tank (4), is characterized in that: also include that standing sedimentation pond (5) and measuring tank (6), the top of described standing sedimentation pond (5) pass through
Pipeline is connected with measuring tank (6), and described measuring tank (6) is connected to concentrator (1) by pipeline, and measuring tank (6) is provided with flow
Valve is accurately controlled liquid and enters the flow velocity of concentrator.
2. the device processing the crude titanic chloride containing higher solid formation impurity as claimed in claim 1, is characterized in that: described
Concentrator (1) uses volume to be 55～66m3Model.
3. process the sedimentation method of the crude titanic chloride containing higher solid formation impurity, it is characterized in that, comprise the following steps:
A, classifying crude titanic chloride by solid impurity content, content >=25g/L is divided into a class, content ＜ 25g/L's
It is divided into a class；
B, the solution of content ＜ 25g/L, first input measuring tank by solution, then feeds to concentrator and carries out continuous overflow sedimentation
Process；
C, the solution of content >=25g/L, before carrying out step b, first put into solution standing sedimentation pond and carry out at standing sedimentation
Reason, delivers to the Sedimentation tank top stillness of night measuring tank, then carries out continuous overflow settlement treatment by b step after sedimentation a period of time；
Clear liquid after d, continuous overflow settlement treatment overflows from concentrator top, is delivered to clear liquid storage tank, and the mud after sedimentation leads to
Cross the spiral crane bottom Sedimentation tank and concentrator and be delivered to slurry tank.
4. the sedimentation method processing the crude titanic chloride containing higher solid formation impurity as claimed in claim 3, is characterized in that:
When carrying out continuous overflow settlement treatment in stepb, control 1.7～2.1t/h from the charging rate of measuring tank to concentrator,
The speed of rotation of concentrator agitator is 0.4～0.8rmp/min.
5. the sedimentation method processing the crude titanic chloride containing higher solid formation impurity as claimed in claim 3, is characterized in that:
The time that solution carries out in step c standing sedimentation process is calculated by y=0.0542x+0.85, and wherein, y is heavy for standing
The fall time, its unit be h, x be the solid impurity content of crude titanic chloride before sedimentation, its unit is g/L.
6. the sedimentation method processing the crude titanic chloride containing higher solid formation impurity as claimed in claim 3, is characterized in that:
When carrying out continuous overflow settlement treatment in step d, spiral crane should be kept to work continuously, rotating speed controls 5～15rmp/
Min, avoids concentrator inner bottom part mud to block drainage conduit.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610801273.5A CN106237671B (en) | 2016-09-05 | 2016-09-05 | The device and sedimentation method of crude titanic chloride of the processing containing higher solid formation impurity |
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| CN201610801273.5A CN106237671B (en) | 2016-09-05 | 2016-09-05 | The device and sedimentation method of crude titanic chloride of the processing containing higher solid formation impurity |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111659180A (en) * | 2020-06-10 | 2020-09-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Slurry solid-liquid separation device and method for separating vanadium-removing slurry by using same |
| CN112209433A (en) * | 2020-10-26 | 2021-01-12 | 宝钛华神钛业有限公司 | Condensation cooling device capable of effectively reducing titanium tetrachloride solid impurities |
| CN113046580A (en) * | 2021-03-12 | 2021-06-29 | 中国恩菲工程技术有限公司 | Scandium extraction pretreatment system and treatment method of scandium-containing solution |
| CN113666414A (en) * | 2021-07-28 | 2021-11-19 | 洛阳双瑞万基钛业有限公司 | Crude titanium tetrachloride fully-closed centrifugal separation system and separation method |
| CN115253478A (en) * | 2022-07-28 | 2022-11-01 | 攀钢集团攀枝花钛材有限公司 | Environment-friendly high-precision filtering device and sedimentation method for crude titanium tetrachloride |
| CN115612864A (en) * | 2022-11-10 | 2023-01-17 | 中铝矿业有限公司 | Process for reducing content of suspended matters in metal gallium adsorption mother liquor |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111659180A (en) * | 2020-06-10 | 2020-09-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Slurry solid-liquid separation device and method for separating vanadium-removing slurry by using same |
| CN111659180B (en) * | 2020-06-10 | 2022-08-02 | 攀钢集团攀枝花钢铁研究院有限公司 | Slurry solid-liquid separation device and method for separating vanadium-removing slurry by using same |
| CN112209433A (en) * | 2020-10-26 | 2021-01-12 | 宝钛华神钛业有限公司 | Condensation cooling device capable of effectively reducing titanium tetrachloride solid impurities |
| CN113046580A (en) * | 2021-03-12 | 2021-06-29 | 中国恩菲工程技术有限公司 | Scandium extraction pretreatment system and treatment method of scandium-containing solution |
| CN113666414A (en) * | 2021-07-28 | 2021-11-19 | 洛阳双瑞万基钛业有限公司 | Crude titanium tetrachloride fully-closed centrifugal separation system and separation method |
| CN115253478A (en) * | 2022-07-28 | 2022-11-01 | 攀钢集团攀枝花钛材有限公司 | Environment-friendly high-precision filtering device and sedimentation method for crude titanium tetrachloride |
| CN115612864A (en) * | 2022-11-10 | 2023-01-17 | 中铝矿业有限公司 | Process for reducing content of suspended matters in metal gallium adsorption mother liquor |
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