CN106390507B - A kind of the continuous vacuum crystallization system and its application method of black titanium liquid - Google Patents
A kind of the continuous vacuum crystallization system and its application method of black titanium liquid Download PDFInfo
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Abstract
The present invention relates to a kind of continuous vacuum crystallization system of black titanium liquid.It includes the two-stage crystallization elementary cell device being sequentially connected；Include crystallizer, condenser, vacuum pump set and transfering material pump per first degree crystalline elementary cell device；In same first degree crystalline elementary cell device, the crystallizer connects with the condenser, the transfering material pump respectively, and the condenser also connects with the vacuum pump set；In first degree crystalline elementary cell device, first degree crystalline device（1）Also with feeding line（13）Connection, one-level transfering material pump（4）Also with the secondary crystallizer in secondary crystallization elementary cell device（5）Connection；Two level transfering material pump in secondary crystallization elementary cell device（8）Also with discharge pipeline（14）Connection.The present invention is reasonable in design, and can cause crystallization process serialization, realizes the target significantly saved.
Description
Technical field
The present invention relates to true as the ferrous sulfate of crystallization material liquid using black titanium liquid in sulfuric acid method titanium pigment production process
Sky crystallization, more particularly to a kind of the continuous vacuum crystallization system and its application method of black titanium liquid.
Background technology
In sulfuric acid method titanium pigment production process, ilmenite or high titanium slag are cleared up using sulfuric acid, gained resolution
Liquid carries out a series of post processings again, that is, obtains mainly containing the black titanium liquid of titanyl sulfate, ferrous sulfate and sulfuric acid.In black titanium liquid
Ferrous sulfate as a kind of soluble impurity need part remove, its remove method be typically using ferrous sulfate solubility
Bigger characteristic is affected by temperature, black titanium liquid is cooled, ferrous sulfate is separated out in the form of green vitriol crystallizes
And separated.On the other hand, intermittent vacuum crystallization processes are generally used in industry.
Vacuum crystallization is also known as adiabatic evaporation, is the transmission for making solvent and isolation heat, in high vacuum state
Under flashed, solvent evaporation endothermic and make system cooling so as to realizing crystallization process.Its principle is simultaneously by dense
Contracting produces degree of supersaturation with two kinds of effects of cooling.
At present, conventional existing vacuum crystallization system is mainly made up of the part such as crystallizer and vacuum equipment, and it is mainly tied
Structure is as shown in accompanying drawing one, and crystallizer is usually to be exported with the container laterally stirred, container top provided with indirect steam, and bottom is set
Have material into and out of shared interface, be further provided with visor and temperature, pressure sensor interface；And frequently with series winding
Steam jet pump, cooler and oil-sealed rotary pump, as vacuum in offer system, realize indirect steam condensation and gas pumps
Equipment；Wherein, steam jet pump is as the active force for taking indirect steam in crystallizer away, its draining hole end and crystallizer top
Steam (vapor) outlet is directly connected to by pipeline.In production operation, 50~60 DEG C of crystallization stoste enters crystallizer in batches, opens
Open vacuum equipment, steam jet pump use 0.5~0.7MPa saturated vapor or micro- superheated steam as jet media, outlet
Side is sprayed using 25~35 DEG C of recirculated water, by jet steam and drainage steam condensation；With negative pressure liter in crystallizer
Height, material reach boiling point, and heat is taken away in water vapor, and temperature of charge persistently reduces.Titanium liquid temperature degree in device to be crystallized is down to technique
Required temperature, vacuum in crystallizer is removed, material is put to subsequent processing.It is former that crystallization is then pumped into crystallizer again
Liquid, into the production of next batch material.Due to the crystallization process be batch production can not serialization, utilization rate of equipment and installations is low,
Automaticity is not high, low production efficiency, and in order to improve production capacity to reach design requirement, it usually needs in same device factory building
Middle setting covers vacuum crystallization equipment more, so then considerably increases librarian use amount and manual operation load；And the crystallization process
The steam jet pump used is, it is necessary to consume a large amount of steam, and product per ton needs the t of steam about 1.1~2, and supporting steam jet pump uses
Condensation cycle water system be also required to consume a large amount of electric energy, more than the kWh of product power consumption about 80 per ton, enterprise's energy consumption is big, into
This height.
In a kind of titanium white production techniques of Chinese patent 201510724436.X by ferrous sulfate from titanium liquid vacuum crystallization
New method, its disclosed equipment mainly includes crystallization kettle, precools the devices such as system, condenser and vavuum pump.Although it has
There is the consumption removed from and steam energy using high temperature, high steam, is greatly reduced, it is beneficial to reduce the production cost of titanium dioxide etc.
Effect, but it is still suffered from：Crystallization process be batch (-type), can not serialization, utilization rate of equipment and installations is low, and automaticity is not high, raw
It is low to produce efficiency；It need to be switched in its production process between precooling system and condenser, it is cumbersome；Precooling system needs
To use recirculated water, energy consumption is higher；Condenser tube side walks indirect steam, and it is low that shell side walks water at low temperature overall heat-transfer coefficient, steam condensation
Effect has to be hoisted；When it uses more vavuum pumps, vavuum pump need to be repeated operation, the operation behaviour such as opens, stops and switches
Make the problems such as inconvenient.
The content of the invention
The first object of the present invention is to provide a kind of continuous vacuum crystallization system of black titanium liquid, and its is reasonable in design,
And crystallization process serialization can be caused, realize the target significantly saved.
The second object of the present invention is the application method for providing the continuous vacuum crystallization system of above-mentioned black titanium liquid.
The object above of the present invention is achieved through the following technical solutions respectively：
A kind of continuous vacuum crystallization system of black titanium liquid, it is characterised in that：The two-stage crystallization that it includes being sequentially connected is basic
Cell arrangement；Include crystallizer, condenser, vacuum pump set and transfering material pump per first degree crystalline elementary cell device；In same one-level
Crystallize elementary cell device in, the crystallizer connects with the condenser, the transfering material pump respectively, the condenser also with institute
State vacuum pump set connection；In first degree crystalline elementary cell device, first degree crystalline device also connects with feeding line, one-level transfering material pump
Also connected with the secondary crystallizer in secondary crystallization elementary cell device；Two level transfering material pump in secondary crystallization elementary cell device
Also connected with discharging pipeline.
A kind of continuous vacuum crystallization system of black titanium liquid, it is characterised in that：The three-level crystallization that it includes being sequentially connected is basic
Cell arrangement；Include crystallizer, condenser, vacuum pump set and transfering material pump per first degree crystalline elementary cell device；In same one-level
Crystallize elementary cell device in, the crystallizer connects with the condenser, the transfering material pump respectively, the condenser also with institute
State vacuum pump set connection；In first degree crystalline elementary cell device, first degree crystalline device also connects with feeding line；First degree crystalline base
One-level transfering material pump in this cell arrangement, also connected with the secondary crystallizer in secondary crystallization elementary cell device；Secondary crystallization
Two level transfering material pump in elementary cell device, also crystallize the three-level crystallizer in elementary cell device with three-level and connect；Three-level knot
Three-level transfering material pump in brilliant elementary cell device connects with discharging pipeline.
As further optimization, also have additional what is be connected with itself on the crystallizer in every first degree crystalline elementary cell device
Pipeloop, one end of the pipeloop connect with crystalliser feet, and the other end connects with crystallization body portion.By setting up circulation
Pipeline, the temperature further ensured in the crystallizer in every grade of crystallization elementary cell device is constant uniform with material, is advantageous to
Crystallize precipitation process.
As further optimization, the first-stage condenser in above-mentioned first degree crystalline elementary cell device, select for vaporation-type it is cold
Condenser, its support without public circulation；Secondary condenser in above-mentioned secondary crystallization elementary cell device, above-mentioned three
Level crystallization elementary cell device in three-level condenser, selection be shell-and-tube heat exchanger, its using when steam walk shell side, low temperature
Water walks tube side.
Above-mentioned vacuum pump set, Roots type vacuum pump, screw-type vacuum pump, reciprocating vacuum pump, claw vacuum can be selected
One kind in the gas conveying type vavuum pump such as pump, oil sealing mechanical pump, liquid-ring vacuum pump and water-jet pump or by a variety of
The unit that vacuum series connection of pumps is formed.
When being produced using the continuous vacuum crystallization system of above-mentioned black titanium liquid, its whole crystallization process is the two-stage of series connection
Or three-stage process." level " herein is divided according to the temperature difference of material in crystallizer.Do not considering actual motion
Under conditions of temperature fluctuation being present, the material in every grade of crystallizer only has a stationary temperature；Crystallized in two-stage or three-level
Cheng Zhong, material has different steady temperatures not at the same level in crystallizer, forms the thermograde of temperature from high to low, material is by temperature
Higher one-level is spent to the relatively low first mobile of temperature.
The continuous vacuum crystallization system of the above-mentioned black titanium liquid for including the two-stage crystallization elementary cell device being sequentially connected, its
Application method specifically follows the steps below：
（1）First start the condenser in first degree crystalline elementary cell device；It is cold in secondary crystallization elementary cell device
2~5 DEG C of water at low temperature is continually fed into tube side in condenser；Black titanium liquid is then added into crystallizers at different levels respectively, addition
Amount is 1 according to the ratio of the liquid holdup in every one-level crystallizer and inlet amount per hour:1~1.5 calculates, to cause material every
Total residence time is 60 to 40 minutes in first degree crystalline device；Wherein, 35~38 DEG C of black titanium liquid is added in first degree crystalline device, two
16~20 DEG C of black titanium liquid is added in level crystallizer；
（2）50~58 DEG C of black titanium liquid is continuously added into first degree crystalline device through feeding line, while opens one-level and turns material
Pump and two level transfering material pump, keep the feeding amount of transfering material pumps at different levels identical with inlet amount, and control liquid level in first degree crystalline device respectively
Top keeps absolute pressure 4200~5000Pa operating pressure, control in secondary crystallizer ullage keep absolute pressure 1220~
1400Pa operating pressure；Indirect steam in first degree crystalline device is entered cold in first degree crystalline elementary cell device by pipeline
Condenser is condensed, and condensed water is discharged through pipeline, fixed gas from first degree crystalline elementary cell device vacuum pump set extract out row to
Air；Indirect steam in secondary crystallizer is passed through the shell side of the condenser in secondary crystallization elementary cell device through pipeline, with
Water at low temperature is exchanged heat and condensed in pipe outer wall in tube side, and condensed water is discharged through pipeline, and fixed gas is by secondary crystallization elementary cell device
In vacuum pump set extract row out to air.
The continuous vacuum crystallization system of the above-mentioned black titanium liquid for including the three-level crystallization elementary cell device being sequentially connected, its
Application method specifically follows the steps below：
（1）First start the condenser in first degree crystalline elementary cell device；It is cold in secondary crystallization elementary cell device
2~10 DEG C of water at low temperature is continually fed into tube side in condenser；Pipe in the condenser during three-level crystallizes elementary cell device
2~5 DEG C of water at low temperature is continually fed into journey；Black titanium liquid is then added into crystallizers at different levels respectively, the amount of addition is according to each
The ratio of liquid holdup and inlet amount per hour in level crystallizer is 1:1~1.5 calculates, to cause material in every one-level crystallizer
Interior total residence time is 60 to 40 minutes；Wherein, 35~38 DEG C of black titanium liquid is added in first degree crystalline device, in secondary crystallizer
25~28 DEG C of black titanium liquid is added, 16~20 DEG C of black titanium liquid is added in three-level crystallizer；
（2）50~58 DEG C of black titanium liquid is continuously continuously added into first degree crystalline device through feeding line, while opens one-level
Transfering material pump, two level transfering material pump and three-level transfering material pump, keep the feeding amount of transfering material pumps at different levels identical with inlet amount, and control one respectively
Ullage keeps 4200~5000Pa of absolute pressure operating pressure in level crystallizer, controls ullage in secondary crystallizer to keep
2300~2800Pa of absolute pressure operating pressure, control the operation of 1220~1400Pa of ullage holding absolute pressure in three-level crystallizer
Pressure；The condenser that indirect steam in first degree crystalline device is entered in first degree crystalline elementary cell device by pipeline is condensed,
Condensed water is discharged through pipeline, and fixed gas extracts row out to air from the vacuum pump set in first degree crystalline elementary cell device；Two level knot
Indirect steam in brilliant device is passed through the shell side of the condenser in secondary crystallization elementary cell device through pipeline, with water at low temperature in tube side
Exchange heat and condensed in pipe outer wall, condensed water is discharged through pipeline, and fixed gas is by the vacuum pump set in secondary crystallization elementary cell device
Extraction is arranged to air；Indirect steam in three-level crystallizer is passed through the condenser in three-level crystallization elementary cell device through pipeline
Water at low temperature is exchanged heat and condensed in pipe outer wall in shell side, with tube side, and condensed water is discharged through pipeline, and fixed gas is crystallized substantially single by three-level
Vacuum pump set in element apparatus extracts row out to air.
The invention has the advantages that：
The invention provides a kind of continuous vacuum crystallization system of black titanium liquid, its is reasonable in design, and causes with black titanium
Liquid is the ferrous sulfate vacuum crystallization process continuous of crystallization material liquid, has utilization rate of equipment and installations high, and automaticity is high, raw
Efficiency high is produced, realizes the benefits such as the target significantly saved.Evaporation is used in first degree crystalline elementary cell device in the system
Formula condenser, supported without public circulation, investment is more simple to be saved, it is even more important that with traditional " public recirculated water
The combining form of system+dividing wall type heat exchanger " is compared, and can economize on electricity 50 more than %；Per in first degree crystalline elementary cell device
Indirect steam, condensation is completed by single condenser, without carry out in process of production forecooler and condenser it
Between switching, operation is easier, and utilization rate of equipment and installations is high；The vacuum machine of integration is used in per first degree crystalline elementary cell device
Group, it is easy to operation and maintain constant vacuum, operation, the operation simplicity such as open, stop and switch without be repeated vavuum pump.It makes
It is simple and easy with method, certain material liquid level and temperature are kept in every grade of crystallizer in advance, temperature of charge at different levels are formed by height
To low thermograde；Front end high-temperature material, which continuously enters to rise to after crystallizer mixes with its interior feed liquid, flashes cooling at liquid level,
Material is continuously produced through transfering material pump to rear end flow in crystallizer simultaneously.In the process of running, by control material into and out of flow
Material liquid level in crystallizer is set to keep stable, and because charging input heat and flash distillation take away heat relative equilibrium, therefore tie
Temperature of charge can be held essentially constant in brilliant device.Whole crystallization process is the two-stage or three-stage process of series connection, and the crystallization of high temperature is former
Continuous circulation, evaporation progressively are cold step by step from high to low continuously into first order crystallizer and by thermograde in system for liquid
But, final evaporation cools down qualified magma and is continuously sent to subsequent processing by final stage crystallizer.
Brief description of the drawings
Fig. 1 is the ferrous sulfate vacuum using black titanium liquid to crystallize material liquid in existing sulfuric acid method titanium pigment production process
The structural representation of crystal system.
Fig. 2 is the structural representation of the continuous vacuum crystallization system of black titanium liquid described in the embodiment of the present invention 1.
Fig. 3 is the structural representation of the continuous vacuum crystallization system of black titanium liquid described in the embodiment of the present invention 2.
Embodiment
The present invention is specifically described below by specific embodiment, it is pointed out here that following examples are served only for this hair
It is bright to be further described, it is impossible to be interpreted as the limitation to its protection domain, the person skilled in the art of this area can be according to upper
State the content of the invention and some nonessential modifications and adaptations are made to the present invention.
Embodiment 1
As shown in Figure of description 1 and 2, a kind of continuous vacuum crystallization system of black titanium liquid, by the three-level knot being sequentially connected
Brilliant elementary cell device composition；Wherein, first degree crystalline elementary cell device is by first degree crystalline device 1, evaporative condenser 2, one-level
Vacuum pump set 3 and one-level transfering material pump 4 form, and first degree crystalline device 1 turns with feeding line 13, evaporative condenser 2, one-level respectively
Material pump 4 connects, and evaporative condenser 2 also connects with one-level vacuum pump set 3；Secondary crystallization elementary cell device is by secondary crystallizer
5th, two level shell-and-tube heat exchanger 6, secondary vacuum unit 7 and two level transfering material pump 8 form, and secondary crystallizer 5 respectively with diode
Shell heat exchanger 6, two level transfering material pump 8 connect, and two level shell-and-tube heat exchanger 6 also connects with secondary vacuum unit 7；Three-level crystallizes base
This cell arrangement is made up of three-level crystallizer 9, three-level shell-and-tube heat exchanger 10, three-level vacuum pump set 11 and three-level transfering material pump 12,
And three-level crystallizer 9 connects with three-level shell-and-tube heat exchanger 10, three-level transfering material pump 12 respectively, three-level shell-and-tube heat exchanger 10 also with
Three-level vacuum pump set 11 connects；One-level transfering material pump 4 also connects with secondary crystallizer 5；Two level transfering material pump 8 also with three-level crystallizer 9
Connection；Three-level transfering material pump 12 also connects with discharging pipeline 14；On first degree crystalline device 1, secondary crystallizer 5 and three-level crystallizer 9 also
The pipeloop 15 being connected respectively with its own is had additional, one end of pipeloops 15 at different levels and the bottom of this grade of crystallizer connect
Logical, the other end connects with the body portion of this grade of crystallizer.
In actual production operation, when being produced using the continuous vacuum crystallization system of the black titanium liquid in this example, according to
Method used below is operated：
（1）First start the circulated sprinkling water pump and blower fan of evaporative condenser 2 one by one；In two level shell-and-tube heat exchanger 6
Tube side in be continually fed into 2~10 DEG C of water at low temperature；2~5 DEG C are continually fed into tube side in three-level shell-and-tube heat exchanger 10
Water at low temperature；60 m are then added into crystallizers at different levels respectively3Black titanium liquid；Wherein, in first degree crystalline device 1 add 35~
38 DEG C of black titanium liquid, 5 add 25~28 DEG C of black titanium liquid in secondary crystallizer, and 16~20 DEG C black is added in three-level crystallizer 9
Titanium liquid；
（2）50~58 DEG C of black titanium liquid is continuously added to first degree crystalline device 1 through feeding line 13, inlet amount is 90 m3/ h,
One-level transfering material pump 4, two level transfering material pump 8 and three-level transfering material pump 12 are opened simultaneously, keeps the feeding amount and inlet amount of transfering material pumps at different levels
It is identical, and the operating pressure of 4200~5000Pa of ullage holding absolute pressure in first degree crystalline device 1 is controlled respectively, control two level knot
Ullage keeps 2300~2800Pa of absolute pressure operating pressure in brilliant device 5, controls ullage in three-level crystallizer 9 to keep exhausted
Press 1220~1400Pa operating pressure；Indirect steam in first degree crystalline device 1 is cold into evaporative condenser 2 by pipeline
Solidifying, condensed water is discharged through pipeline, and fixed gas is from the row of extraction out of one-level vacuum pump set 3 to air；Indirect steam in secondary crystallizer 5
The shell side of two level shell-and-tube heat exchanger 6 is passed through through pipeline, exchanges heat with water at low temperature in tube side and is condensed in pipe outer wall, condensed water is through pipe
Line is discharged, and fixed gas is from the row of extraction out of secondary vacuum unit 7 to air；Indirect steam in three-level crystallizer 9 is passed through three through pipeline
The shell side of level shell-and-tube heat exchanger 10, discharge, do not coagulate through pipeline with water at low temperature heat exchange in tube side and in pipe outer wall condensation, condensed water
Gas is from the row of extraction out of three-level vacuum pump set 11 to air.
Wherein,（1）The black titanium liquid of 50~58 DEG C of acidolysis continuously enters first degree crystalline device 1 by feed pipe 13, with wherein 35~
38 DEG C of the black titanium liquid mixing of acidolysis, ullage keep 4200~5000Pa of absolute pressure operating pressure, and mixed solution is in the pressure
Feeding belt heat is removed by evaporation process down, material is kept 35~38 DEG C of steady temperature；Material in first degree crystalline device 1, warp
One-level transfering material pump 4 is crossed to be continuously introduced into secondary crystallizer 5 and mix with wherein material.
（2）Ullage keeps 2300~2800Pa of absolute pressure operating pressure in secondary crystallizer 5, and solution is at this pressure
Feeding belt heat is removed by evaporation process, material is kept 25~28 DEG C of steady temperature；Material in secondary crystallizer 5, pass through
Two level transfering material pump 8 is continuously introduced into three-level crystallizer 9 and mixed with wherein material.
（3）Ullage keeps 1220~1400Pa of absolute pressure operating pressure in three-level crystallizer 9, and solution is at this pressure
Feeding belt heat is removed by evaporation process, material is kept 16~20 DEG C of steady temperature, and the temperature is crystallization overall process
Endpoint temperature；Material is continuously introduced into lower step process by three-level transfering material pump 12 and discharging pipeline 14 in three-level crystallizer 9.
（4）Indirect steam in first degree crystalline device 1 is condensed after pipeline enters evaporative condenser 2, and condensed water passes through
Pipeline is discharged, and fixed gas is from the row of extraction out of one-level vacuum pump set 3 to air.
（5）In two level shell-and-tube heat exchanger 6,2~10 DEG C of water at low temperature enters the tube side of the heat exchanger, the high temperature after heat exchange
Water returns to refrigeration unit, is cooled to 2~10 DEG C of Posterior circles and uses；Indirect steam in secondary crystallizer 5 enters two level through pipeline
The shell side of shell-and-tube heat exchanger 6, discharged with water at low temperature heat exchange in tube side and in pipe outer wall condensation, condensed water through pipeline, fixed gas
From the row of extraction out of secondary vacuum unit 7 to air.
（6）In three-level shell-and-tube heat exchanger 10,2~5 DEG C of water at low temperature enters the tube side of the heat exchanger, the high temperature after heat exchange
Water returns to refrigeration unit, is cooled to 2~5 DEG C of Posterior circles and uses；Indirect steam in three-level crystallizer 9 enters triode through pipeline
The shell side of shell heat exchanger 10, with water at low temperature heat exchange in tube side and being condensed in pipe outer wall, condensed water discharges through pipeline, fixed gas by
Three-level vacuum pump set 11 extracts row out to air.
Two level shell-and-tube heat exchanger 6 in this example, the tube side material in three-level shell-and-tube heat exchanger 10 are water at low temperature, and shell side is walked
Tube side in indirect steam, with conventional arrangement walks indirect steam, and shell side is walked water at low temperature and compared, and there is overall heat-transfer coefficient to improve, and steams
Vapour condensation effect is more preferable, and condensed water is easily discharged in time, and vacuum stream is not easy the benefits such as short circuit.
Embodiment 2
As shown in Figure of description 3, a kind of continuous vacuum crystallization system of black titanium liquid, base is crystallized by the two-stage being sequentially connected
This cell arrangement forms；Wherein, first degree crystalline elementary cell device is by first degree crystalline device 1, evaporative condenser 2, one-level vacuum
Unit 3 and one-level transfering material pump 4 form, and first degree crystalline device 1 respectively with feeding line 13, evaporative condenser 2, one-level transfering material pump
4 connections, evaporative condenser 2 also connect with one-level vacuum pump set 3；Secondary crystallization elementary cell device is by secondary crystallizer 5, two
Level shell-and-tube heat exchanger 6, secondary vacuum unit 7 and two level transfering material pump 8 form, and secondary crystallizer 5 respectively with two level shell-and-tube
Heat exchanger 6, two level transfering material pump 8 connect, and two level shell-and-tube heat exchanger 6 also connects with secondary vacuum unit 7；One-level transfering material pump 4 is also
Connected with secondary crystallizer 5；Two level transfering material pump 8 also connects with discharging pipeline 14；Also increase on first degree crystalline device 1, secondary crystallizer 5
Provided with the pipeloop 15 being connected respectively with its own, one end of pipeloops 15 at different levels and the bottom of this grade of crystallizer connect
Logical, the other end connects with the body portion of this grade of crystallizer.
Actual production operation in, when being produced using the continuous vacuum crystallization system of black titanium liquid in this example, according to
Lower application method is operated：
（1）First start the circulated sprinkling water pump and blower fan of evaporative condenser 2 one by one；In two level shell-and-tube heat exchanger 6
Tube side in be continually fed into 2~5 DEG C of water at low temperature；30 m are then added into crystallizers at different levels respectively3Black titanium liquid, wherein,
35~38 DEG C of black titanium liquid is added in first degree crystalline device, 16~20 DEG C of black titanium liquid is added in secondary crystallizer；
（2）50~58 DEG C of black titanium liquid is continuously added to first degree crystalline device 1 through feeding line 13, inlet amount is 30 m3/ h,
One-level transfering material pump 4 and two level transfering material pump 8 are opened simultaneously, keeps the feeding amount of transfering material pumps at different levels identical with inlet amount, and control respectively
Ullage keeps 4200~5000Pa of absolute pressure operating pressure in first degree crystalline device 1 processed, controls in secondary crystallizer 5 on liquid level
Side keeps 1220~1400Pa of absolute pressure operating pressure；Indirect steam in first degree crystalline device 1 is cold into vaporation-type by pipeline
Condenser 2 is condensed, and condensed water is discharged through pipeline, and fixed gas is from the row of extraction out of one-level vacuum pump set 3 to air；In secondary crystallizer 5
Indirect steam the shell side of two level shell-and-tube heat exchanger 6 is passed through through pipeline, with water at low temperature heat exchange in tube side and being condensed in pipe outer wall,
Condensed water is discharged through pipeline, and fixed gas is from the row of extraction out of secondary vacuum unit 7 to air.
Wherein,（1）The black titanium liquid of 50~58 DEG C of acidolysis continuously enters first degree crystalline device 1 by feed pipe 13, with wherein 35~
38 DEG C of the black titanium liquid mixing of acidolysis, ullage keep 4200~5000Pa of absolute pressure operating pressure, and mixed solution is in the pressure
Feeding belt heat is removed by evaporation process down, material is kept 35~38 DEG C of steady temperature；Material in first degree crystalline device 1, warp
One-level transfering material pump 4 is crossed to be continuously introduced into secondary crystallizer 5 and mix with wherein material.
（2）Ullage keeps 1220~1400Pa of absolute pressure operating pressure in secondary crystallizer 5, and solution is at this pressure
Feeding belt heat is removed by evaporation process, material is kept 16~20 DEG C of steady temperature, and the temperature is crystallization overall process
Endpoint temperature；Material is continuously introduced into lower step process by two level transfering material pump 8 and discharging pipeline 14 in secondary crystallizer 5.
（3）Indirect steam in first degree crystalline device 1 is condensed after pipeline enters evaporative condenser 2, and condensed water passes through
Pipeline is discharged；Fixed gas is from the row of extraction out of one-level vacuum pump set 3 to air.
（4）In two level shell-and-tube heat exchanger 6,2~5 DEG C of water at low temperature enters the tube side of the heat exchanger, the high temperature after heat exchange
Water returns to refrigeration unit, is cooled to 2~5 DEG C of Posterior circles and uses；Indirect steam in secondary crystallizer 5 enters diode through pipeline
The shell side of shell heat exchanger 6, discharged with water at low temperature heat exchange in tube side and in pipe outer wall condensation, condensed water through pipeline；Fixed gas by
Secondary vacuum unit 7 extracts row out to air.
Tube side material in this example in two level shell-and-tube heat exchanger 6 is water at low temperature, and shell side walks indirect steam, with conventional arrangement
In tube side walk indirect steam, shell side is walked water at low temperature and compared, have overall heat-transfer coefficient improve, steam condensation effect is more preferable, condensation
Water is easily discharged in time, and vacuum stream is not easy the benefits such as short circuit.
Claims (2)
- A kind of 1. continuous vacuum crystallization system of black titanium liquid, it is characterised in that：The two-stage crystallization that it includes being sequentially connected is substantially single Element apparatus；Include crystallizer, condenser, vacuum pump set and transfering material pump per first degree crystalline elementary cell device；In same one-level knot In brilliant elementary cell device, the crystallizer connects with the condenser, the transfering material pump respectively, the condenser also with it is described Vacuum pump set connects；In first degree crystalline elementary cell device, first degree crystalline device（1）Also with feeding line（13）Connection, one-level Transfering material pump（4）Also with the secondary crystallizer in secondary crystallization elementary cell device（5）Connection；In secondary crystallization elementary cell device Two level transfering material pump（8）Also with discharge pipeline（14）Connection；The pipeloop being connected with itself is also had additional on per the crystallizer in first degree crystalline elementary cell device（15）, the circulation Pipeline（15）One end connected with crystalliser feet, the other end connects with crystallization body portion；First-stage condenser in the first degree crystalline elementary cell device is evaporative condenser（2）；The secondary crystallization is basic Secondary condenser in cell arrangement is shell-and-tube heat exchanger；The application method of the continuous vacuum crystallization system of the black titanium liquid, is specifically followed the steps below：1）First start the condenser in first degree crystalline elementary cell device；In condenser in secondary crystallization elementary cell device Tube side in be continually fed into 2~5 DEG C of water at low temperature；Then add black titanium liquid into crystallizers at different levels respectively, the amount of addition according to The ratio of liquid holdup and inlet amount per hour in every one-level crystallizer is 1:1~1.5 calculates；Wherein, first degree crystalline device（1）In Add 35~38 DEG C of black titanium liquid, secondary crystallizer（5）The middle black titanium liquid for adding 16~20 DEG C；2）Through feeding line（13）To first degree crystalline device（1）50~58 DEG C of black titanium liquid is inside continuously added to, while opens one-level and turns Expect pump（4）With two level transfering material pump（8）, keep the feeding amount of transfering material pumps at different levels identical with inlet amount, and control first degree crystalline respectively Device（1）Interior ullage keeps 4200~5000Pa of absolute pressure operating pressure, controls secondary crystallizer（5）Interior ullage is kept 1220~1400Pa of absolute pressure operating pressure；First degree crystalline device（1）Interior indirect steam is basic into first degree crystalline by pipeline Condenser in cell arrangement is condensed, and condensed water is discharged through pipeline, and fixed gas is by true in first degree crystalline elementary cell device Empty unit extracts row out to air；Secondary crystallizer（5）Interior indirect steam is passed through in secondary crystallization elementary cell device through pipeline Condenser shell side, with water at low temperature heat exchange in tube side and being condensed in pipe outer wall, condensed water discharges through pipeline, and fixed gas is by two level Crystallize the vacuum pump set in elementary cell device and extract row out to air.
- A kind of 2. continuous vacuum crystallization system of black titanium liquid, it is characterised in that：The three-level crystallization that it includes being sequentially connected is substantially single Element apparatus；Include crystallizer, condenser, vacuum pump set and transfering material pump per first degree crystalline elementary cell device；In same one-level knot In brilliant elementary cell device, the crystallizer connects with the condenser, the transfering material pump respectively, the condenser also with it is described Vacuum pump set connects；In first degree crystalline elementary cell device, first degree crystalline device（1）Also with feeding line（13）Connection；One-level Crystallize the one-level transfering material pump in elementary cell device（4）, also with the secondary crystallizer in secondary crystallization elementary cell device（5）Even It is logical；Two level transfering material pump in secondary crystallization elementary cell device（8）, the three-level crystallization in elementary cell device is also crystallized with three-level Device（9）Connection；Three-level transfering material pump in three-level crystallization elementary cell device（12）With the pipeline that discharges（14）Connection；The pipeloop being connected with itself is also had additional on per the crystallizer in first degree crystalline elementary cell device（15）, the circulation Pipeline（15）One end connected with crystalliser feet, the other end connects with crystallization body portion；First-stage condenser in the first degree crystalline elementary cell device is evaporative condenser（2）；The three-level crystallization is basic Three-level condenser in cell arrangement is shell-and-tube heat exchanger；The application method of the continuous vacuum crystallization system of the black titanium liquid, is specifically followed the steps below：1）First start the condenser in first degree crystalline elementary cell device；In condenser in secondary crystallization elementary cell device Tube side in be continually fed into 2~10 DEG C of water at low temperature；Held in tube side in the condenser during three-level crystallizes elementary cell device The continuous water at low temperature for being passed through 2~5 DEG C；Black titanium liquid is then added into crystallizers at different levels respectively, the amount of addition is according to every first degree crystalline The ratio of liquid holdup and inlet amount per hour in device is 1:1~1.5 calculates；Wherein, first degree crystalline device（1）It is middle to add 35~38 DEG C black titanium liquid, secondary crystallizer（5）The middle black titanium liquid for adding 25~28 DEG C, three-level crystallizer（9）Middle 16~20 DEG C of addition Black titanium liquid；2）Through feeding line（13）Continuously to first degree crystalline device（1）50~58 DEG C of black titanium liquid is inside continuously added to, while opens one Level transfering material pump（4）, two level transfering material pump（8）With three-level transfering material pump（12）, keep the feeding amount of transfering material pumps at different levels identical with inlet amount, And first degree crystalline device is controlled respectively（1）Interior ullage keeps 4200~5000Pa of absolute pressure operating pressure, controls secondary crystallization Device（5）Interior ullage keeps 2300~2800Pa of absolute pressure operating pressure, controls three-level crystallizer（9）Interior ullage is kept 1220~1400Pa of absolute pressure operating pressure；First degree crystalline device（1）Interior indirect steam is basic into first degree crystalline by pipeline Condenser in cell arrangement is condensed, and condensed water is discharged through pipeline, and fixed gas is by true in first degree crystalline elementary cell device Empty unit extracts row out to air；Secondary crystallizer（5）Interior indirect steam is passed through in secondary crystallization elementary cell device through pipeline Condenser shell side, with water at low temperature heat exchange in tube side and being condensed in pipe outer wall, condensed water discharges through pipeline, and fixed gas is by two level Crystallize the vacuum pump set in elementary cell device and extract row out to air；Three-level crystallizer（9）Interior indirect steam is passed through through pipeline The shell side of condenser in three-level crystallization elementary cell device, with water at low temperature heat exchange in tube side and in pipe outer wall condensation, condensed water Discharged through pipeline, the vacuum pump set that fixed gas is crystallized from three-level in elementary cell device extracts row out to air.
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