CN106237671B - The device and sedimentation method of crude titanic chloride of the processing containing higher solid formation impurity - Google Patents
The device and sedimentation method of crude titanic chloride of the processing containing higher solid formation impurity Download PDFInfo
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- CN106237671B CN106237671B CN201610801273.5A CN201610801273A CN106237671B CN 106237671 B CN106237671 B CN 106237671B CN 201610801273 A CN201610801273 A CN 201610801273A CN 106237671 B CN106237671 B CN 106237671B
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- concentrator
- sedimentation
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- 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
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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
- B01D21/24—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
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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
- B01D21/30—Control equipment
- B01D21/34—Controlling the feed distribution; Controlling the liquid level ; Control of process parameters
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- 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)
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- Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Disclosed by the invention is a kind of device and sedimentation method for handling the crude titanic chloride containing higher solid formation impurity of titanium technical field of metallurgy industry, the device includes concentrator, positioned at the spiral crane of concentrator bottom discharging mouth, and the slurry tank of the clear liquid storage tank and collection settled mud for containing the solution after settling, further include standing sedimentation pond and measuring tank, the top in the standing sedimentation pond is connected by pipeline with measuring tank, the measuring tank is connected to concentrator by pipeline, measuring tank accurately controls the flow velocity that liquid enters concentrator equipped with flow valve.Standing sedimentation processing is carried out first for the solution of solid impurity content >=25g/L, then upper clear supernate is taken to carry out continuous overflow settlement treatment, this mode can directly handle the crude titanic chloride of higher solid formation impurity, continuous-stable detaches the insoluble solids impurity in crude titanic chloride, and the production efficiency and the quality of production of titanium tetrachloride greatly improved.
Description
Technical field
The present invention relates to titanium technical field of metallurgy industry more particularly to a kind of containing higher solid formation impurity for handle
The device and sedimentation method of crude titanic chloride.
Background technology
Metal titanium or titanium alloy is due to specific strength is high, density is small, high temperature resistant and cryogenic property, acid-alkali-corrosive-resisting etc. are excellent
It is anisotropic can, be widely used in that aerospace, derived energy chemical be metallurgical, fields, the titanium tetrachloride conduct such as civilian prepare 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 production process so that thick four
Impurity content in titanium chloride increases, if if impurity fails preferably to be removed in crude titanic chloride, can be existed with four times of concentration
It is enriched in titanium sponge, extreme influence is generated to titanium sponge quality；It is former for the titanium slag of Chinese Panxi Diqu high contents of calcium and magnesium impurity content
Often adopt fused salt chlorimation method prepares crude titanic chloride to material, must be removed through sedimentation removal of impurities, the processes such as filter removal of impurities, refining and edulcoration of running affairs
AlCl3、FeCl3、SiCl4, the impurity such as VOCl3 to be to obtain life of the up-to-standard refined titanic chloride for titanium sponge, titanium white chloride
Production.
Currently, less to the processing method of crude titanic chloride sedimentation, research report both at home and abroad.Chinese invention patent
A kind of method that CN103505915A discloses titanium tetrachloride subsider and extracts supernatant liquid, focuses on introducing subsider
Construction.Chinese invention patent CN103191835A discloses a kind of comprising titanium-tetrachloride storage tank, casing, engine base, differential mechanism, electricity
The Titanium tetrachloride slag-liquid separation centrifugal machine of machine, its object is to solve sealing effect in existing titanium tetrachloride separation of solid and liquid process
The technical problems such as difference, equipment attrition corrosion is fast, operation expense is high, serious pollution environment.And testing proves to use subsider
Continuous sedimentation pattern is difficult to that the higher crude titanic chloride of solid content is effectively treated；Though centrifuge can realize thick tetrachloro in a short time
Change the insoluble solid formation impurity in titanium, but is difficult to realize continuous feeding and discharging and large-scale industrial production.
Invention content
To make up the deficiencies in the prior art, the technical problem to be solved by the present invention is to：A kind of handle containing higher is provided
The device and sedimentation method of the crude titanic chloride of solid formation impurity.
The technical solution adopted by the present invention to solve the technical problems is：Thick tetrachloro of the processing containing higher solid formation impurity
Change titanium device, including concentrator, positioned at concentrator bottom discharging mouth spiral crane and for contains settle after it is molten
The clear liquid storage tank of liquid and the slurry tank for collecting settled mud, further include standing sedimentation pond and measuring tank, the standing sedimentation pond
Top is connected by pipeline with measuring tank, and the measuring tank is connected to concentrator by pipeline, and measuring tank can equipped with flow valve
Liquid with precise control enters the flow velocity of concentrator.
The concentrator uses volume for 55~66m3Model.
The sedimentation method of crude titanic chloride of the processing containing higher solid formation impurity, includes the following steps：
A, classify by solid impurity content to crude titanic chloride, content >=25g/L's is divided into one kind, content ＜ 25g/
L's is divided into one kind；
B, the solution of content ＜ 25g/L, inputs measuring tank by solution first, then feeds to concentrator and carries out continuous overflow
Settlement treatment；
Solution is first put into standing sedimentation pond and stand and sunk by the c, solution of content >=25g/L before carrying out step b
Drop processing, send the settling tank top stillness of night to measuring tank after settling a period of time, then is carried out at continuous overflow sedimentation by b step
Reason；
D, the clear liquid after continuous overflow settlement treatment is overflowed from concentrator top, is delivered to clear liquid storage tank, the mud after sedimentation
Slurry is delivered to slurry tank by the spiral crane of settling tank and dense motor spindle.
Further, when carrying out continuous overflow settlement treatment in stepb, from measuring tank to the charging rate of concentrator
In 1.7~2.1t/h, the speed of rotation of concentrator blender is 0.4~0.8rmp/min for control.
Further, the time for carrying out standing sedimentation processing to solution in step c is carried out by y=0.0542x+0.85
It calculates, wherein y is the standing sedimentation time, and unit h, x are the solid impurity content of crude titanic chloride before sedimentation, unit
For g/L.
Further, when carrying out continuous overflow settlement treatment in step d, spiral crane continuous work should be kept, is turned
Speed control avoids bottom mud in concentrator from blocking drainage conduit in 5~15rmp/min.
The beneficial effects of the invention are as follows：By adding standing sedimentation pond and measuring tank outside traditional concentrator, for solid
The solution of body impurity content >=25g/L carries out standing sedimentation processing first, and upper clear supernate is then taken to carry out at continuous overflow sedimentation
Reason, this mode can directly handle the crude titanic chloride of higher solid formation impurity, and continuous-stable detaches in crude titanic chloride not
Molten solid impurity, greatly improved the production efficiency of titanium tetrachloride, effectively keep away liquid delivery process because impurity content higher band is come
Line clogging, while also greatly reducing distillation still resistance wire scaling loss frequency in crude titanic chloride subtractive process.
Description of the drawings
Fig. 1 is the structural schematic diagram of apparatus of the present invention.
Label is 1- concentrators, 2- screw elevators, 3- clear liquid storage tanks, 4- slurry tanks, 5- standing sedimentations pond, 6- in figure
Measuring tank.
Specific implementation mode
Below by way of the drawings and specific embodiments, the invention will be further described.
As shown in Figure 1, the device of crude titanic chloride of the present invention processing containing higher solid formation impurity, including concentrator 1,
Positioned at the spiral crane 2 of 1 bottom discharging mouth of concentrator and the clear liquid storage tank 3 for containing the solution after settling and collect
The slurry tank 4 of settled mud, further includes standing sedimentation pond 5 and measuring tank 6, the top in the standing sedimentation pond 5 by pipeline with
Measuring tank 6 is connected, and the measuring tank 6 is connected to concentrator 1 by pipeline, and measuring tank 6 accurately controls liquid equipped with flow valve
Body enters the flow velocity of concentrator.Traditional handicraft only carries out overflow by concentrator mostly when carrying out titanium tetrachloride settlement treatment and sinks
Drop processing, but for the higher solution of solid impurity content, it is bad to depend merely on concentrator effect of settling.The present invention is stood by being arranged
Settling tank first carries out preliminary sedimentation to solution, then carries out overflow sedimentation again, is greatly improved overflow effect of settling, and pass through
Measuring tank accurately controls flow velocity, can realize that continuous overflow settles, production efficiency and quality are all significantly improved.According to reality
The border condition of production generally uses volume for 55~66m3Model, effect of settling is good, and production efficiency is high.
The sedimentation method of crude titanic chloride of the processing containing higher solid formation impurity, includes the following steps：
A, classify by solid impurity content to crude titanic chloride, content >=25g/L's is divided into one kind, content ＜ 25g/
L's is divided into one kind；
B, the solution of content ＜ 25g/L, inputs measuring tank by solution first, then feeds to concentrator and carries out continuous overflow
Settlement treatment；
Solution is first put into standing sedimentation pond and stand and sunk by the c, solution of content >=25g/L before carrying out step b
Drop processing, send the settling tank top stillness of night to measuring tank after settling a period of time, then is carried out at continuous overflow sedimentation by b step
Reason；
D, the clear liquid after continuous overflow settlement treatment is overflowed from concentrator top, is delivered to clear liquid storage tank, the mud after sedimentation
Slurry is delivered to slurry tank by the spiral crane of settling tank and dense motor spindle.
It finds after long term test is analyzed, only when solid impurity content is less than 25g/L, is directly carried 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 to bottom of pond, then carries out overflow settlement treatment to the clear liquid on top again, so can be only achieved pre-
The effect of settling of phase.
Further, when carrying out continuous overflow settlement treatment in stepb, the charging rate control from measuring tank to concentrator
For system in 1.7~2.1t/h, the speed of rotation of concentrator blender is 0.4~0.8rmp/min.It obtains, presses after test of many times
The rotating speed of charging rate and 0.4~0.8rmp/min according to 1.7~2.1t/h is controlled, and can guarantee the continuous fortune of concentrator
Row, effect of settling is good, while can ensure that bottom mud has good mobility, convenient for discharge.
The time for carrying out standing sedimentation processing to solution in step c is calculated by y=0.0542x+0.85, wherein y
For the standing sedimentation time, unit h, x are the solid impurity content of crude titanic chloride before sedimentation, unit g/L.It is heavy to stand
The drop time is also to carry out settlement treatment by being used for a long time and testing the conclusion obtained according to this time, can reach best
Effect of settling and production efficiency.
When carrying out continuous overflow settlement treatment in step d, spiral crane continuous work should be kept, rotating speed control 5~
15rmp/min avoids bottom mud in concentrator from blocking drainage conduit.Screw elevator be mainly used for it is intermittent to mud into
Row cleaning, discharging period is 2 times/day~4 times/day, when not carrying out discharge operation, carries continuous rotate forward of material spiral progress and operates,
Rotating speed is 5~15rmp/min, and bottom mud in concentrator is avoided to block drainage conduit.
Below by embodiment, the present invention is further described.
Embodiment 1
Crude titanic chloride to solid content less than 25g/L carries out continuous overflow sedimentation, control parameter and the front and back knot of sedimentation
Fruit is as shown in table 1：
Table 1, which continuously overflows, settles front and back solid content situation of change
It is 0.5rmp/min that continuous overflow infall process, which controls concentrator agitator speed, and inlet amount is 1.7~2t.h-1,
Crude titanic chloride solid content averagely reduces 2g/L, value≤4g/L after sedimentation.
Embodiment 2
Independent standing sedimentation processing is carried out more than the crude titanic chloride of 25g/L to solid impurity content first, as a result such as table 2
Shown, the solid impurity content before sample A, B, C, D sedimentation is respectively 323g/L, 221g/L, 59.5g/L, 25.5g/L, is divided quiet
The top stillness of night solid content for setting crude titanic chloride after settling 15h, 8h, 5h, 1.5h is substantially reduced ,≤10g/L.
Solid content and ingredient before and after 2 crude titanic chloride standing sedimentation of table
Continuous overflow sedimentation is carried out using the crude titanic chloride stillness of night after standing sedimentation, further decreases thick titanium solid content,
The results are shown in Table 3：
Table 3, which continuously overflows, settles front and back solid content situation of change
Crude titanic chloride solid content≤4g/L after continuous overflow sedimentation.Standing sedimentation is combined with continuous overflow sedimentation
The crude titanic chloride of higher solids impurity content is can effectively deal with, realizes that solid-liquid efficiently separates.
Both examples above absolutely proves that the present apparatus and sedimentation method can effectively deal with the titanium tetrachloride of high solids content, institute
Obtain solid formation content≤4g/L in the crude titanic chloride stillness of night.The crude titanic chloride of gained can greatly improve after being handled using this method
Production efficiency effectively keeps away line clogging, very big reduction crude titanic chloride essence that liquid delivery process comes by impurity content higher band
Distillation still resistance wire scaling loss frequency during system has good practicability and application prospect.
Claims (4)
1. the sedimentation method of crude titanic chloride of the processing containing higher solid formation impurity, including processing contain higher solid formation impurity
Crude titanic chloride device, the device include concentrator (1), be located at concentrator (1) bottom discharging mouth spiral crane
(2) and for contain sedimentation after solution clear liquid storage tank (3) and collect settled mud slurry tank (4), further include standing
The top of settling tank (5) and measuring tank (6), the standing sedimentation pond (5) is connected by pipeline with measuring tank (6), the metering
Tank (6) is connected to concentrator (1) by pipeline, and measuring tank (6) accurately controls liquid equipped with flow valve and enters concentrator
Flow velocity, characterized in that include the following steps：
A, classify by solid impurity content to crude titanic chloride, content >=25g/L's is divided into one kind, content ＜ 25g/L's
It is divided into one kind；
B, the solution of content ＜ 25g/L, inputs measuring tank by solution first, then feeds to concentrator and carries out continuous overflow sedimentation
Processing；
Solution is first put into standing sedimentation pond and carried out at standing sedimentation by the c, solution of content >=25g/L before carrying out step b
Reason send the settling tank top stillness of night to measuring tank after settling a period of time, then carries out continuous overflow settlement treatment by b step；
D, the clear liquid after continuous overflow settlement treatment is overflowed from concentrator top, is delivered to clear liquid storage tank, and the mud after sedimentation is logical
The spiral crane for crossing settling tank and dense motor spindle is delivered to slurry tank.
2. the sedimentation method of crude titanic chloride of the processing containing higher solid formation impurity as described in claim 1, it is characterized in that：
When carrying out continuous overflow settlement treatment in stepb, controlled in 1.7~2.1t/h from measuring tank to the charging rate of concentrator,
The speed of rotation of concentrator blender is 0.4~0.8rmp/min.
3. the sedimentation method of crude titanic chloride of the processing containing higher solid formation impurity as described in claim 1, it is characterized in that：
The time for carrying out standing sedimentation processing to solution in step c is calculated by y=0.0542x+0.85, wherein y is to stand to sink
It drops the time, unit h, x are the solid impurity content of crude titanic chloride before sedimentation, unit g/L.
4. the sedimentation method of crude titanic chloride of the processing containing higher solid formation impurity as described in claim 1, it is characterized in that：
When carrying out continuous overflow settlement treatment in step d, spiral crane continuous work, rotating speed should be kept to control in 5~15rmp/
Min avoids bottom mud in concentrator from blocking drainage conduit.
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| CN112209433B (en) * | 2020-10-26 | 2021-05-28 | 宝钛华神钛业有限公司 | Condensation cooling device capable of effectively reducing titanium tetrachloride solid impurities |
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