CN209872398U - Ferrous sulfate crystallization device for sulfate process titanium dioxide - Google Patents

Ferrous sulfate crystallization device for sulfate process titanium dioxide Download PDF

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CN209872398U
CN209872398U CN201920505437.9U CN201920505437U CN209872398U CN 209872398 U CN209872398 U CN 209872398U CN 201920505437 U CN201920505437 U CN 201920505437U CN 209872398 U CN209872398 U CN 209872398U
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acid
tank
crystallizer
vacuum ejector
sulfuric acid
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卢星
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Abstract

The utility model belongs to the technical field of sulfuric acid process titanium white powder production facility, a sulfuric acid process titanium white ferrous sulfate crystallization device is disclosed, including the crystallizer, the top of crystallizer is connected with first elevated tank, the bottom of crystallizer is equipped with into discharge gate, the lower part of crystallizer is equipped with side agitating unit, the upper portion of crystallizer is connected with the vacuum ejector, the top of vacuum ejector is connected with the second elevated tank, the bottom of vacuum ejector links to each other with the acid circulation groove, the acid circulation groove is through the acid pump, the heat exchanger links to each other with the top of vacuum ejector, be equipped with the mouth of mending acid on the acid circulation groove, be connected with cooling circulation system on the heat exchanger, be equipped with between the top of heat exchanger and vacuum ejector and arrange sour mouth. The device combines the gravity action of materials with the characteristics of easy water absorption and low saturated vapor pressure of concentrated sulfuric acid to create a vacuum environment, realizes the crystallization of ferrous sulfate without using steam, and achieves the purpose of separating from titanium liquid.

Description

Ferrous sulfate crystallization device for sulfate process titanium dioxide
Technical Field
The utility model belongs to the technical field of sulfuric acid process titanium white powder production facility, concretely relates to sulfuric acid process titanium white ferrous sulfate crystallization device.
Background
Titanium dioxide is the best white pigment in the world and is widely applied to the fields of coatings, plastics, paper making and the like. Titanium dioxide has two production processes of a sulfuric acid method and a chlorination method, and the sulfuric acid method still occupies a leading position at present.
In the process of industrially producing titanium dioxide by using a sulfuric acid method, a large amount of iron elements are brought by ilmenite raw materials, so that ferrous sulfate crystals need to be formed in production and separated and removed, the iron content of a titanium dioxide finished product is in a proper range, and the whiteness and the application performance of the titanium dioxide are ensured. Because the temperature is an important factor influencing the crystallization of ferrous sulfate, in industrial production, the clear titanium liquid (commonly called as precipitated titanium liquid) obtained by sedimentation is cooled after the acidolysis of ilmenite is completed, so that the iron element in the titanium liquid is separated out in the form of ferrous sulfate heptahydrate.
At present, the separation of ferrous sulfate in the sulfuric acid method titanium dioxide industry mainly adopts a cooling method and a vacuum cooling method, commonly called freezing crystallization and vacuum crystallization, and compared with the freezing crystallization, the vacuum crystallization has the advantages of simple process flow, high production capacity, concentration of titanium liquid while crystallization, reduction of burden of a concentration process, good safety and the like. Specifically, the vacuum crystallization is to form negative pressure in a crystallizer by using a steam ejector, at the moment, moisture in the titanium liquid is evaporated due to the reduction of a boiling point, heat is taken away, the temperature of the titanium liquid is reduced, the solubility of ferrous sulfate is reduced by controlling the temperature of a titanium liquid system, the ferrous sulfate is crystallized and separated out, and then the filtration is carried out. Although vacuum crystallization has many advantages, the method consumes a large amount of steam and electricity and consumes high energy.
SUMMERY OF THE UTILITY MODEL
In view of the above situation, the utility model aims at providing a sulfuric acid process titanium dioxide ferrous sulfate crystallization device. Through reasonable structure setting, utilize the material gravity to combine together with the easy water absorption of concentrated sulfuric acid, the characteristic of low saturated vapor pressure, build vacuum environment, need not to use steam, realize the crystallization of ferrous sulfate promptly, reach the purpose with the separation of titanium liquid, reduce cost by a wide margin.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
the utility model provides a sulfuric acid process titanium dioxide ferrous sulfate crystallization device, includes the crystallizer, the top of crystallizer is connected with first elevated tank, and the bottom of crystallizer is equipped with into discharge gate, and the lower part of crystallizer is equipped with side agitating unit, and the upper portion of crystallizer is connected with vacuum ejector, and vacuum ejector's top is connected with the second elevated tank, vacuum ejector's bottom links to each other with sour circulation tank, sour circulation tank links to each other through the top of acid pump, heat exchanger and vacuum ejector, be equipped with the mouth of mending acid on the sour circulation tank, be connected with cooling circulation system on the heat exchanger, be equipped with the mouth of arranging acid between the top of heat exchanger and vacuum ejector.
The utility model discloses in, the bottom of first elevated tank is equipped with the first clean mouth of putting, and upper portion is equipped with first overflow mouth, first elevated tank links to each other with the crystallizer tank top through first valve.
The utility model discloses in, the bottom of second elevated tank is equipped with the second and puts clean mouth, and upper portion is equipped with the second overflow mouth, the second elevated tank links to each other with the vacuum ejector top through the second valve.
According to the utility model discloses, the acid discharge pipe liquid outlet of vacuum ejector bottom is located below the acid circulation groove liquid level, forms acid seal, guarantees vacuum ejector's vacuum.
The utility model discloses in, setting up of crystallizer tank highly makes material gravity be far greater than atmospheric pressure, can satisfy and form the vacuum through the action of gravity, and equally, the difference in height of vacuum ejector and acid circulation groove makes sulphuric acid gravity be far greater than atmospheric pressure, forms sulphuric acid and sprays the chamber. The heights of the crystallization tank and the vacuum ejector are specifically set according to the factors such as material specific gravity, acid spraying amount and the like.
The utility model discloses in, the heat exchanger can adopt conventional cooling circulation system, preferably, cooling circulation system includes circulating water pond and circulating pump, the circulating water pond top is equipped with the cooling tower.
According to the utility model discloses, be equipped with the third valve between crystallizer tank upper portion and vacuum ejector.
The utility model discloses in still including other subassemblies that can make this sulfuric acid process titanium white ferrous sulfate crystallization device normal use, set up the valve like the business turn over material mouth at the crystallizer, set up the valve on the connecting line of vacuum ejector and sour circulation groove and all belong to the conventional selection in this field. In addition, the device or the assembly which is not limited in the utility model adopts the conventional means in the field, for example, the side stirring device, the acid pump and the like can be arranged according to the prior art.
The utility model discloses a sulfuric acid process titanium dioxide ferrous sulfate crystallization device's effect principle does:
1. opening a fourth valve arranged at a feed inlet and a discharge outlet at the bottom of the crystallization tank, closing a first valve at the top of the crystallization tank, adding the titanium liquid with the temperature of 40-60 ℃ into the crystallization tank from the feed inlet and the discharge outlet at the bottom of the crystallization tank until the first head tank contains a part of the titanium liquid, closing the first valve, stopping feeding, and allowing the material in the crystallization tank to flow out from the feed inlet and the discharge outlet when the pressure of the material in the crystallization tank formed by the height of the liquid level is greater than atmospheric pressure, wherein when the titanium liquid in the crystallization tank reaches (20-30 m)3) When the process is required, the fourth valve is closed, the upper closed space of the crystallization tank forms high vacuum, the water begins to evaporate, the temperature of the titanium liquid begins to decrease, and the ferrous sulfate tends to crystallize;
2. adding concentrated sulfuric acid into an acid circulation tank, closing a fifth valve arranged between the acid circulation tank and a vacuum ejector, opening a second valve and a sixth valve arranged between a heat exchanger and the top of the vacuum ejector, adding the acid in the acid circulation tank into the vacuum ejector through an acid pump until a second head tank contains sulfuric acid at a certain liquid level, closing the second valve and the sixth valve, opening the fifth valve, discharging a part of sulfuric acid, and inserting an acid discharge pipe at the bottom of the vacuum ejector into the acid solution, so that the whole sulfuric acid system is a closed space, forms high vacuum and is close to the vacuum degree of a crystallization tank;
3. opening a third valve and a sixth valve, continuously absorbing water in the evaporation process of the titanium liquid by concentrated sulfuric acid through a vacuum ejector under the action of an acid pump, breaking the dynamic balance of water evaporation above a crystallization tank, continuously reducing the temperature of the titanium liquid, gradually crystallizing and separating ferrous sulfate, and ensuring the stable operation of the iron removal process of the titanium liquid; the concentration of the sulfuric acid absorbing the water drops and the temperature rises, at the moment, concentrated sulfuric acid is continuously added into the acid circulating tank from the acid supplementing port, and dilute sulfuric acid is discharged from the acid discharging port, and the dilute sulfuric acid can be used for relevant processes such as the production of premixed acid or sulfuric acid for titanium dioxide acidolysis by a sulfuric acid method; in addition, a heat exchanger (in a water circulation heat exchange mode) is adopted to remove heat;
4. when the temperature of the titanium liquid is reduced to the technological requirement of (15-25 ℃), the third valve is closed, the liquid in the first elevated tank is emptied, the first valve is opened, the crystallization tank is communicated with the atmosphere, the fourth valve is opened, and the material is put into the next working procedure, so that the circulation is completed, and the process is repeated.
The utility model discloses a sulfuric acid process titanium dioxide ferrous sulfate crystallization device has following advantage:
(1) the utility model discloses utilize material action of gravity to produce the vacuum principle, can save traditional steam jet vacuum pump and mechanical vacuum pump, need not steam and power consumption, the cost reduces by a wide margin.
(2) The utility model discloses the low steam partial pressure and the easy hydroscopicity of ingenious utilization concentrated sulfuric acid replace traditional steam to take away the moisture that produces in the titanium liquid evaporation process, when having stopped steam consumption, the sulphuric acid that is utilized can be used to other relevant processes of titanium white powder preparation, can not cause the waste.
(3) The utility model discloses ingenious material gravity that utilizes forms the vacuum, replaces steam to spray and produces the vacuum, does not have steam to participate in, has greatly reduced traditional cooling heat load, has reduced the consumption of cooling water and electric power.
(4) Adopt the utility model discloses a ferrous sulfate granule that crystallization device made is even, and remaining titanium content is low, and ferrous sulfate is of high quality on the one hand, is favorable to the utilization in low reaches, and on the other hand can promote the titanium yield of sulfuric acid process titanium dioxide.
Drawings
Fig. 1 is a schematic structural diagram of a sulfuric acid process titanium dioxide ferrous sulfate crystallization device of an embodiment.
Detailed Description
The technical solution of the present invention will be described clearly and completely with reference to the embodiments of the present invention, and obviously, the described embodiments are only some embodiments of the present invention, not all embodiments.
Examples
As shown in figure 1, a sulfuric acid process titanium dioxide ferrous sulfate crystallization device, including crystallizer 1, the top of crystallizer 1 is connected with first elevated tank 2, and the bottom of crystallizer 1 is equipped with into discharge gate, and the lower part of crystallizer 1 is equipped with side agitating unit 3, and the upper portion of crystallizer 1 is connected with vacuum ejector 4, and the top of vacuum ejector 4 is connected with second elevated tank 5, the bottom of vacuum ejector 4 links to each other with acid circulation groove 6, acid circulation groove 6 links to each other with the top of vacuum ejector 4 through acid pump 7, heat exchanger 8, be equipped with benefit acid mouth 9 on the acid circulation groove 6, be connected with cooling circulation system on the heat exchanger 8, be equipped with between the top of heat exchanger 8 and vacuum ejector 4 and arrange sour mouth 10.
The bottom of the first elevated tank 2 is provided with a first emptying port 11, the upper part of the first elevated tank is provided with a first overflow port 12, and the first elevated tank 2 is connected with the top of the crystallization tank 1 through a first valve 13.
The bottom of the second elevated tank 5 is provided with a second emptying port 14, the upper part of the second elevated tank is provided with a second overflow port 15, and the second elevated tank 5 is connected with the top of the vacuum ejector 4 through a second valve 16.
And a liquid outlet of the acid discharge pipe at the bottom of the vacuum ejector 4 is positioned below the liquid level of the acid circulation tank 6 to form an acid seal, so that the vacuum degree of the vacuum ejector 4 is ensured.
The cooling circulation system comprises a circulation water tank 17 and a circulation pump 18, and a cooling tower 19 is arranged above the circulation water tank 17.
A third valve 20 is arranged between the upper part of the crystallization tank 1 and the vacuum ejector 4.
The sulfuric acid process titanium dioxide ferrous sulfate crystallization device has the following action principle:
1. opening a fourth valve 21 arranged at a feed inlet and a discharge outlet at the bottom of the crystallization tank 1, a first valve 13 at the top of the crystallization tank 1, closing the third valve 20, adding the titanium liquid with the temperature of 40-60 ℃ into the crystallization tank 1 from the feed inlet and the discharge outlet at the bottom of the crystallization tank 1 until the first elevated tank 2 contains a part of the titanium liquid, closing the first valve 13, stopping feeding at the same time, and allowing the material in the crystallization tank 1 to flow out from the feed inlet and the discharge outlet when the pressure of the material in the crystallization tank 1, which is formed by the height of the liquid level, is higher than the atmospheric pressure, so that the titanium liquid reaches (20-3) When the process is requiredClosing the fourth valve 21, forming high vacuum in the upper closed space of the crystallization tank 1, evaporating water, lowering the temperature of the titanium liquid, and making the ferrous sulfate tend to crystallize;
2. adding concentrated sulfuric acid into an acid circulating tank 6, closing a fifth valve 22 arranged between the acid circulating tank 6 and a vacuum ejector 4, opening a second valve 16 and a sixth valve 23 arranged between a heat exchanger 8 and the top of the vacuum ejector 4, adding the acid in the acid circulating tank 6 into the vacuum ejector 4 through an acid pump 7 until the second head tank 5 contains sulfuric acid at a certain liquid level, closing the second valve 16 and the sixth valve 23, opening the fifth valve 22, and discharging a part of sulfuric acid, wherein an acid discharging pipe at the lower part of the vacuum ejector 4 is inserted into the sulfuric acid, so that the whole sulfuric acid system is a closed space, forms high vacuum and has a vacuum degree close to that of a crystallization tank 1;
3. the third valve 20 and the sixth valve 23 are opened, concentrated sulfuric acid continuously absorbs moisture in the evaporation process of the titanium liquid through the vacuum ejector 4 under the action of the acid pump 7, the dynamic balance of the moisture evaporation above the crystallization tank 1 is broken, the temperature of the titanium liquid is continuously reduced, ferrous sulfate is gradually crystallized and separated out, and the iron removal process of the titanium liquid is ensured to be carried out stably; the concentration of the sulfuric acid absorbing the water drops and the temperature rises, at the moment, the acid circulating tank 6 needs to continuously add concentrated sulfuric acid from the acid supplementing port 9 and release dilute sulfuric acid from the acid discharging port 10, and the dilute sulfuric acid can be used for relevant processes such as the production of premixed acid or sulfuric acid for the titanium dioxide acidolysis by a sulfuric acid method; in addition, a heat exchanger 8 (in a water circulation heat exchange mode) is adopted to remove heat;
4. when the temperature of the titanium liquid is reduced to the technological requirement of (15-25 ℃), the third valve 20 is closed, the liquid in the first elevated tank 2 is emptied, the first valve 13 is opened, the crystallization tank 1 is communicated with the atmosphere, the fourth valve 21 is opened, and the material is put into the next working procedure to reciprocate.
This sulfuric acid process titanium dioxide ferrous sulfate crystallization device has following advantage:
(1) the crystallization device utilizes the principle that the gravity action of materials generates vacuum, can save a traditional steam jet vacuum pump and a mechanical vacuum pump, does not need steam and power consumption, and greatly reduces the cost.
(2) The crystallization device ingeniously utilizes the low water vapor partial pressure and the easy water absorbability of concentrated sulfuric acid to replace the traditional method that steam takes away the water generated in the evaporation process of titanium liquid, and when the steam consumption is stopped, the utilized sulfuric acid can be used for other related processes of titanium dioxide preparation, and the waste can not be caused.
(3) The crystallizing device ingeniously utilizes the gravity of the materials to form vacuum to replace steam to jet and generate vacuum, no steam participates, the traditional cooling heat load is greatly reduced, and the consumption of cooling water and electric power is reduced.
(4) The ferrous sulfate prepared by the crystallization device has uniform particles and low residual titanium content, on one hand, the ferrous sulfate has good quality, which is beneficial to downstream utilization, and on the other hand, the titanium yield of titanium white prepared by a sulfuric acid method can be improved.
The foregoing description of the embodiments of the invention has been presented for purposes of illustration and not limitation, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the illustrated embodiments.

Claims (6)

1. The utility model provides a sulfuric acid process titanium dioxide ferrous sulfate crystallization device, includes the crystallizer tank, its characterized in that: the top of crystallizer is connected with first elevated tank, and the bottom of crystallizer is equipped with into discharge gate, and the lower part of crystallizer is equipped with side agitating unit, and the upper portion of crystallizer is connected with vacuum ejector, and vacuum ejector's top is connected with the second elevated tank, vacuum ejector's bottom links to each other with the acid circulation groove, the acid circulation groove links to each other with vacuum ejector's top through acid pump, heat exchanger, be equipped with the mouth of mending acid on the acid circulation groove, be connected with cooling circulation system on the heat exchanger, be equipped with the mouth of discharging acid between the top of heat exchanger and vacuum ejector.
2. The apparatus for crystallizing ferrous sulfate as titanium white by sulfuric acid process according to claim 1, wherein: the bottom of first elevated tank is equipped with first net mouth of putting, and upper portion is equipped with first overflow mouth, first elevated tank links to each other with the crystallizer tank top through first valve.
3. The apparatus for crystallizing ferrous sulfate as titanium white by sulfuric acid process according to claim 1, wherein: and a second emptying port is arranged at the bottom of the second elevated tank, a second overflow port is arranged at the upper part of the second elevated tank, and the second elevated tank is connected with the top of the vacuum ejector through a second valve.
4. The apparatus for crystallizing ferrous sulfate as titanium white by sulfuric acid process according to claim 1, wherein: and a liquid outlet of an acid discharge pipe at the bottom of the vacuum ejector is positioned below the liquid level of the acid circulation tank.
5. The apparatus for crystallizing ferrous sulfate as titanium white by sulfuric acid process according to claim 1, wherein: the cooling circulation system comprises a circulation water tank and a circulation pump, and a cooling tower is arranged above the circulation water tank.
6. The apparatus for crystallizing ferrous sulfate as titanium white by sulfuric acid process according to claim 1, wherein: and a third valve is arranged between the upper part of the crystallization tank and the vacuum ejector.
CN201920505437.9U 2019-04-15 2019-04-15 Ferrous sulfate crystallization device for sulfate process titanium dioxide Active CN209872398U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109850954A (en) * 2019-04-15 2019-06-07 卢星 A kind of sulfate process titanium dioxide ferrous sulfate crystallization device

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109850954A (en) * 2019-04-15 2019-06-07 卢星 A kind of sulfate process titanium dioxide ferrous sulfate crystallization device
CN109850954B (en) * 2019-04-15 2023-11-24 卢星 Sulfuric acid process titanium white ferrous sulfate crystallization device

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