CN103896329B - Prepare the system of titanium tetrachloride - Google Patents
Prepare the system of titanium tetrachloride Download PDFInfo
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- CN103896329B CN103896329B CN201310664770.1A CN201310664770A CN103896329B CN 103896329 B CN103896329 B CN 103896329B CN 201310664770 A CN201310664770 A CN 201310664770A CN 103896329 B CN103896329 B CN 103896329B
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Abstract
The present invention discloses the system preparing titanium tetrachloride, comprising: chlorination reactor, is supplied in chlorination reactor there is chlorination reaction in described chlorination reactor by titaniferous ore, reductive agent; First gas-solid separating device, for carrying out gas solid separation process to chlorination reaction mixture, to obtain the gaseous mixture containing titanium tetrachloride; Condensing works, for carrying out condensation process to the gaseous mixture containing titanium tetrachloride, to obtain liquid titanium tetrachloride; And titanium tetrachloride storing device, for storing described liquid crude titanium tetrachloride; Control device, described control device is connected with described condensing works, and condensing works is controlled by the amount for the chlorination reaction mixture containing titanium tetrachloride gases produced according to chlorination reactor. This system is utilized can effectively to prepare the titanium tetrachloride that can be used for preparing titanium dioxide.
Description
Technical field
The present invention relates to chemical field. More specifically, it relates to prepare the system of titanium tetrachloride.
Background technology
The method producing titanium dioxide at present mainly contains sulfuric acid process and chlorination process. Due to the long flow path of sulfuric acid process, seriously polluted, poor product quality and be progressively chlorinated method replace.
CN1066043 discloses a kind of processing method preparing Rutile type Titanium Dioxide, it comprises 1), chlorination furnace is put into by after titanium slag and refinery coke Homogeneous phase mixing, lead to chlorine at 800��900 DEG C of temperature, carry out fluidizing chlorination, 2), the rough titanium tetrachloride obtained after chlorination carries out separation purification remove, magnesium, iron, the impurity such as silicon and vanadium, obtain refining titanic chloride, 3), obtained refining titanic chloride liquid is in vaporizer, it is converted into gas phase, and it is preheated to 450��800 DEG C, 4), gas phase titanium tetrachloride and a small amount of compound modifying agent gas phase aluminum chloride are mixed into oxidized still, oxygen enters oxidized still through plasma generator heating, at 1300��1500 DEG C of temperature, it is less than in 0.1 second and carries out oxidizing reaction generation solid phase titanium dioxide, 5), rapidly titanium dioxide pressed powder is moved out of reaction zone and reaction heat is gone in shifting rapidly, collect titanium dioxide generation chlorine and return chlorination furnace, 6), the titanium dioxide granule powder of collection is beaten into liquid, through two-stage sorting, the fine particle titanium dioxide being less than 1 micron carries out aftertreatment again, coarse particles grinding and then classification, 7), used additives pH=7��8 at 50��70 DEG C of temperature are made to carry out coating aftertreatment, 8), by titanium dioxide slurries after aftertreatment, through twice filtration, charging is moisture is less than 45%, discharging is moisture is less than 1%, 9) dry at 120��160 DEG C of temperature, micronizing, product mean particle size accounts for 70% below 0.3 ��m.
But, the means preparing titanium dioxide at present still have much room for improvement.
Summary of the invention
The present invention is intended to one of technical problem at least solving existence in prior art. For this reason, it is an object of the present invention to propose a kind of system that can effectively prepare titanium tetrachloride.
The present invention proposes a kind of system preparing titanium tetrachloride. According to embodiments of the invention, this system comprises: chlorination reactor, described chlorination reactor is provided with titanium ore entrance, reductive agent entrance, oxygen intake, gas inlet and chlorine entrance, titaniferous ore, reductive agent are supplied in described chlorination reactor, and to oxygen gas-supplying in described chlorination reactor, air and chlorine, there is chlorination reaction in described chlorination reactor, and obtain the chlorination reaction mixture containing titanium tetrachloride gases, wherein, described reductive agent is refinery coke, and described titaniferous ore is titanium slag or rutile titanium ore; First gas-solid separating device, described first gas-solid separating device is connected with described chlorination reactor, for described chlorination reaction mixture is carried out gas solid separation process, to obtain the gaseous mixture containing titanium tetrachloride; Condensing works, described condensing works is connected with described first gas-solid separating device, for the described gaseous mixture containing titanium tetrachloride is carried out condensation process, to obtain liquid titanium tetrachloride; Titanium tetrachloride storing device, described titanium tetrachloride storing device is connected with described condensing works, for storing described liquid crude titanium tetrachloride; Control device, described control device is connected with described condensing works, and described condensing works is controlled by the amount for the chlorination reaction mixture containing titanium tetrachloride gases produced according to described chlorination reactor. Thus, it is possible to realize continuous production titanium tetrachloride.
According to embodiments of the invention, the above-mentioned system for the preparation of titanium tetrachloride can also have following additional technical feature further:
In one embodiment of the invention, described condensing works comprises further: adverse current cooling unit, described adverse current cooling unit is provided with chlorination reaction mixture entrance and liquid titanium tetrachloride entrance, so that by a part for described liquid titanium tetrachloride and the described gaseous mixture counter current contact containing titanium tetrachloride in described adverse current cooling unit, to carry out the first cooling process; And tubular heat exchanger, described tubular heat exchanger is connected with described adverse current cooling unit, and utilize refrigerant that the gaseous mixture through the first cooling process is carried out the 2nd cooling process, to obtain described liquid titanium tetrachloride, wherein, described refrigerant is the R507 cooling medium of temperature-23 degrees Celsius. Contriver finds, by this method of cooling, it is possible to effectively cooled by the gaseous mixture containing titanium tetrachloride, thus realizes being further purified titanium tetrachloride. Wherein, for the first cooling process, the liquid titanium tetrachloride obtaining cooling can be effectively utilized cool, thus reduce the production cost producing titanium dioxide, in addition, adopting the R507 cooling medium of temperature-23 degrees Celsius as refrigerant, being that contriver is unexpected by a large amount of screening operation obtains, and finding, it can play a role to be significantly better than the cooling medium of other temperature and type.
In one embodiment of the invention, described condensing works comprises: one-level direct condenser, and described one-level direct condenser has the first gas inlet, first liquid entrance and gas liquid outlet; Receiving tank, the import of described receiving tank is connected with described gas liquid outlet; Two grades of direct condensers, described two grades of direct condensers have the 2nd gas inlet, second liquid entrance and pneumatic outlet, and described 2nd gas inlet is connected with the outlet of described receiving tank; Indirect condenser, described indirect condenser has inlet mouth, air outlet and liquid outlet, and described inlet mouth is connected with described pneumatic outlet; Blower fan, described blower fan is connected to described air outlet place; Storage groove, described storage groove is connected with described liquid outlet.
In one embodiment of the invention, described condensing works also comprises droplet separator, and described droplet separator is connected between described air outlet and described blower fan, and described droplet separator is connected with described storage groove.
In one embodiment of the invention, described condensing works also comprises self-acting valve, and one end of described self-acting valve is connected between described droplet separator and described blower fan and the other end is connected to the exit of described blower fan.
In one embodiment of the invention, described condensing works also comprises controller, first gas inlet place of described one-level direct condenser is provided with the first pressure detector, described controller is connected with described self-acting valve with described first pressure detector, described blower fan respectively, and described controller controls the rotating speed of described blower fan and the opening and closing of described self-acting valve according to the detected pressure value of described first pressure detector.
In one embodiment of the invention, described blower fan is roots blower, when the detected pressure value of described first pressure detector is more than or equal to scheduled pressure value, described controller controls described self-acting valve and cuts out and the rotating speed that controls described blower fan is greater than desired speed, when the detected pressure value of described first pressure detector is less than described scheduled pressure value, described controller controls described self-acting valve and opens and the rotating speed that controls described blower fan is less than described desired speed.
In one embodiment of the invention, the gas outlet of described two grades of direct condensers is provided with the 2nd pressure detector, the 3rd pressure detector it is provided with between described droplet separator and described blower fan, and described 3rd pressure detector is between described droplet separator and described self-acting valve, the exit of described blower fan is provided with the 4th pressure detector.
In one embodiment of the invention, described condensing works also comprises the first pressure detector, the 2nd pressure detector and the 3rd pressure detector, described first pressure detector is connected with described 2nd pressure detector with described first pressure detector respectively, described 2nd pressure detector is connected with described 3rd pressure detector with described 2nd pressure detector respectively, and described 3rd pressure detector is connected with described 4th pressure detector with described 3rd pressure detector respectively.
The additional aspect of the present invention and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by the practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or the additional aspect of the present invention and advantage from accompanying drawing below combining to the description of embodiment becoming obviously and it should be readily understood that wherein:
Fig. 1 is the schematic flow sheet of the method preparing titanium dioxide according to an embodiment of the invention;
Fig. 2 is the structural representation of the system preparing titanium dioxide according to an embodiment of the invention;
Fig. 3 is the structural representation of the condensing works of the titanium tetrachloride being embodiment according to the present invention one; And
Fig. 4 is the structural representation of the system preparing titanium tetrachloride being embodiment according to the present invention one.
Embodiment
Being described below in detail embodiments of the invention, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has element that is identical or similar functions from start to finish. It is exemplary below by the embodiment being described with reference to the drawings, only for explaining the present invention, and limitation of the present invention can not be interpreted as.
In the present invention, unless otherwise clearly defined and limited, term " is connected ", " connection ", the term such as " fixing " should be interpreted broadly, and such as, it is possible to be fixedly connected with, it is also possible to be removably connect, or connects integratedly; Can be mechanically connected, it is also possible to be electrical connection; Can be directly be connected, it is also possible to be indirectly connected by intermediary, it is possible to be the connection of two element internals. For the ordinary skill in the art, it is possible to understand above-mentioned term concrete implication in the present invention according to particular case.
It should be noted that, term " first ", " the 2nd " are only for describing object, and can not be interpreted as instruction or hint relative importance or imply the quantity indicating indicated technology feature. Thus, be limited with " first ", the feature of " the 2nd " can express or implicit comprise one or more these features.
In a first aspect of the present invention, the present invention proposes a kind of system preparing titanium tetrachloride. According to embodiments of the invention, with reference to Fig. 4, this system comprises: chlorination reactor 2, the first gas-solid separating device 3, condensing works 1, titanium tetrachloride storing device 4, control device 8. Utilize this system, it is possible to realize the continuous production of titanium tetrachloride.
According to embodiments of the invention, described chlorination reactor 2 is provided with titanium ore entrance, reductive agent entrance, oxygen intake, gas inlet and chlorine entrance, titaniferous ore, reductive agent are supplied in described chlorination reactor 2, and to oxygen gas-supplying in described chlorination reactor 2, air and chlorine, there is chlorination reaction in described chlorination reactor 2, and obtain the chlorination reaction mixture containing titanium tetrachloride gases, wherein, described reductive agent is refinery coke, and described titaniferous ore is titanium slag or rutile titanium ore.
According to embodiments of the invention, described first gas-solid separating device 3 is connected with described chlorination reactor 2, for described chlorination reaction mixture is carried out gas solid separation process, to obtain the gaseous mixture containing titanium tetrachloride;
According to embodiments of the invention, described condensing works 1 is connected with described first gas-solid separating device 3, for the described gaseous mixture containing titanium tetrachloride is carried out condensation process, to obtain liquid titanium tetrachloride;
According to embodiments of the invention, described titanium tetrachloride storing device 4 is connected with described condensing works 1, for storing described liquid crude titanium tetrachloride;
According to embodiments of the invention, described control device 8 is connected with described condensing works 1, and described condensing works 1 is controlled by the amount for the chlorination reaction mixture containing titanium tetrachloride gases produced according to described chlorination reactor.
In one embodiment of the invention, described condensing works 1 comprises further: adverse current cooling unit, described adverse current cooling unit is provided with chlorination reaction mixture entrance and liquid titanium tetrachloride entrance, so that by a part for described liquid titanium tetrachloride and the described gaseous mixture counter current contact containing titanium tetrachloride in described adverse current cooling unit, to carry out the first cooling process; And tubular heat exchanger, described tubular heat exchanger is connected with described adverse current cooling unit, and utilize refrigerant that the gaseous mixture through the first cooling process is carried out the 2nd cooling process, to obtain described liquid titanium tetrachloride, wherein, described refrigerant is the R507 cooling medium of temperature-23 degrees Celsius. Contriver finds, utilizes this condensing works 1, it is possible to effectively cooled by the gaseous mixture containing titanium tetrachloride, thus realizes being further purified titanium tetrachloride. Wherein, for the first cooling process, the liquid titanium tetrachloride obtaining cooling can be effectively utilized cool, thus reduce the production cost producing titanium dioxide, in addition, adopting the R507 cooling medium of temperature-23 degrees Celsius as refrigerant, being that contriver is unexpected by a large amount of screening operation obtains, and finding, it can play a role to be significantly better than the cooling medium of other temperature and type.
The condensing works 1 of titanium tetrachloride gases according to embodiments of the present invention is described below with reference to Fig. 3. As shown in Figure 3, the condensing works 1 of titanium tetrachloride gases according to embodiments of the present invention comprises one-level direct condenser 100, receiving tank 200, two grades of direct condensers 300, indirect condenser 400, blower fan 500 and storage groove 600.
One-level direct condenser 100 has the first gas inlet 110, first liquid entrance 120 and gas liquid outlet 130. The import 210 of receiving tank 200 is connected with gas liquid outlet 130. Two grades of direct condensers 300 have the 2nd gas inlet 310, second liquid entrance 320 and pneumatic outlet the 330, two gas inlet 310 and are connected with the outlet 220 of receiving tank 200. Indirect condenser 400 has inlet mouth 410, air outlet 420 and liquid outlet 430, and inlet mouth 410 is connected with pneumatic outlet 330. Blower fan 500 is connected to air outlet 420 place. Storage groove 600 is connected with liquid outlet 430.
The working process of the condensing works 1 of titanium tetrachloride gases according to embodiments of the present invention is described below. the mixed gas containing titanium tetrachloride that chlorination furnace produces first enters one-level direct condenser 100 from the first gas inlet 110 and directly contacts with the liquid titanium tetrachloride entered from first liquid entrance 120, part gaseous titanium tetrachloride is condensed into liquid titanium tetrachloride, uncooled gas and liquid titanium tetrachloride together discharge one-level direct condenser 100 by gas liquid outlet 130, and enter receiving tank 200 by the import 210 of receiving tank 200. in receiving tank 200, uncooled mixed gas is through outlet 220 discharge receiving tank 200, and enter two grades of direct condensers 300 by the 2nd gas inlet 310, contact with the liquid titanium tetrachloride entered from second liquid entrance 320, carry out condensation further, liquid titanium tetrachloride flows back to receiving tank 200, uncooled gas discharges two grades of direct condensers 300 through pneumatic outlet 330, indirect condenser 400 is entered again by inlet mouth 410, again carry out condensation, condensed liquid titanium tetrachloride enters storage groove 600 by liquid outlet 430, residual gas discharges indirect condenser 400 by air outlet 420, blower fan 500 will be sent to follow-up chlorinated exhaust washing system after residual gas supercharging.
The condensing works 1 of titanium tetrachloride gases according to embodiments of the present invention, by air outlet 420 place at indirect condenser 400, blower fan 500 is set, can utilize blower fan 500 that tail gas is carried out supercharging and be sent to follow-up vent gas washing system, so that tail gas has the resistance that enough pressure overcomes subsequent handling system, to ensure the continuous operation of subsequent reactions, significantly improve production efficiency. Therefore, the condensing works 1 of titanium tetrachloride gases according to embodiments of the present invention has and tail gas can carry out supercharging, the normal operation that ensures follow-up system, improves the advantages such as production efficiency.
Fig. 3 shows the condensing works 1 of the titanium tetrachloride gases according to the present invention's specific embodiment. As shown in Figure 3, the condensing works 1 of titanium tetrachloride gases can also comprise droplet separator 700, and droplet separator 700 can be connected between air outlet 420 and blower fan 500, and droplet separator 700 can be connected with storage groove 600. By the titanium tetrachloride drop separation discharged from the air outlet 420 of indirect condenser 400 out, to avoid, liquid titanium tetrachloride drop and tail gas together can be discharged from the condensing works 1 of titanium tetrachloride gases, avoid waste like this.
Advantageously, as shown in Figure 3, the condensing works 1 of titanium tetrachloride gases can also comprise self-acting valve 800, and one end of self-acting valve 800 can be connected between droplet separator 700 and blower fan 500 and the other end can be connected to outlet 520 place of blower fan 500. In other words, one end of self-acting valve 800 can be connected to import 510 place of blower fan 500 and the other end can be connected to outlet 520 place of blower fan 500. A loop in parallel with blower fan 500 can be formed like this, by controlling the opening and closing of self-acting valve 800, it is possible to the break-make of control loop, to regulate blower fan 500 to the actual pressurized effect of tail gas pressure. Thus can increase blower fan 500 to the regulation range of tail gas pressure and sharpness of regulation.
Fig. 3 shows the condensing works 1 of the titanium tetrachloride gases according to the present invention's concrete example. As shown in Figure 3, the condensing works 1 of titanium tetrachloride gases can also comprise controller (not shown), first gas inlet 110 place of one-level direct condenser 100 can be provided with the first pressure detector 900, described controller can be connected with self-acting valve 800 with the first pressure detector 900, blower fan 500 respectively, and described controller can according to the rotating speed of detected pressure value control blower fan 500 of the first pressure detector 900 and the opening and closing of self-acting valve 800. Described controller can be utilized like this blower fan 500 and self-acting valve 800 to be controlled according to the pressure at the first gas inlet 110 place of one-level direct condenser 100, to realize the automatic adjustment of the pressure of the condensing works 1 of whole titanium tetrachloride gases.
Specifically, blower fan 500 can be roots blower, and namely the air quantity of leading of blower fan 500 is directly proportional to rotating speed. When the detected pressure value of the first pressure detector 900 is more than or equal to scheduled pressure value, described controller can control self-acting valve 800 and cut out and the rotating speed of blower fan 500 is greater than desired speed, when the detected pressure value of the first pressure detector 900 is less than described scheduled pressure value, described controller can control self-acting valve 800 and open and the rotating speed of blower fan 500 is less than described desired speed. Like this can pressure in the condensing works 1 of titanium tetrachloride gases higher time, self-acting valve 800 is closed, blower fan 500 rotating speed increases, to improve the wind effect of blower fan 500. And pressure in the condensing works 1 of titanium tetrachloride gases lower time, self-acting valve 800 is opened, blower fan 500 rotating speed reduces, to reduce the wind effect of blower fan 500, such that it is able to guarantee the pressure of the condensing works 1 of whole titanium tetrachloride gases.
Advantageously, as shown in Figure 3, pneumatic outlet 330 place of two grades of direct condensers 300 can be provided with the 2nd pressure detector 1000, the 3rd pressure detector 1100 can be provided with between droplet separator 700 and blower fan 500, and the 3rd pressure detector 1100 can between droplet separator 700 and self-acting valve 800, that is, the 3rd pressure detector 1100 can be positioned at the downstream of droplet separator 700 and be positioned at self-acting valve 800 and the upstream of blower fan 500. Outlet 520 place of blower fan 500 can be provided with the 4th pressure detector 1200. The 2nd pressure detector 1000, the 3rd pressure detector 1100 and the 4th pressure detector 1200 can be utilized like this to detect the pressure exporting 520 places of the pressure at inlet mouth 410 place of indirect condenser 400, the pressure at import 510 place of blower fan 500 and blower fan 500 respectively, so that the magnitude of pressure differential between detection each several part.
Further, as shown in Figure 3, the condensing works 1 of titanium tetrachloride gases can also comprise the first pressure detector 1300, the 2nd pressure detector 1400 and the 3rd pressure detector 1500, first pressure detector 1300 can be connected with the 2nd pressure detector 1000 with the first pressure detector 900 respectively, 2nd pressure detector 1400 can be connected with the 3rd pressure detector 1100 with the 2nd pressure detector 1000 respectively, and the 3rd pressure detector 1500 can be connected with the 4th pressure detector 1200 with the 3rd pressure detector 1100 respectively. The first pressure detector 1300, the 2nd pressure detector 1400 and the 3rd pressure detector 1500 can be utilized like this to detect the pressure difference between the pressure difference between one-level direct condenser 100 and two grades of direct condensers 300, two grades of direct condensers 300 and indirect condenser 400 and the pressure difference between indirect condenser 400 and blower fan 500 respectively, thus can be convenient to the magnitude of pressure differential detected between each several part further, so that by the setting range of the pressure difference control between each several part.
Specifically, the first pressure detector 900, the 2nd pressure detector 1000, the 3rd pressure detector 1100 and the 4th pressure detector 1200 can be tensimeter. First pressure detector 1300, the 2nd pressure detector 1400 and the 3rd pressure detector 1500 can be pressure reduction meter.
Specifically, the set(ting)value of the first pressure detector 1300 can be 40mbar, the set(ting)value of the 2nd pressure detector 1400 can be 20mbar, the set(ting)value of the 3rd pressure detector 1500 can be 10mbar, when pressure difference between each several part of the condensing works 1 of titanium tetrachloride gases deviates set(ting)value, the amount of the liquid titanium tetrachloride that can enter one-level direct condenser 100 and two grades of direct condensers 300 by regulating regulates the value of the first pressure detector 1300, the value of the 2nd pressure detector 1400 is regulated by filling into nitrogen between two grades of direct condensers 300 and indirect condenser 400.
Correspondingly, as shown in Figure 3, pipeline between two grades of direct condensers 300 and indirect condenser 400 can be provided with nitrogen inlet 1600. Like this between indirect condenser 400 and two grades of direct condensers 300 pressure deviation set(ting)value time, it is possible to by from nitrogen inlet 1600 fill into nitrogen regulate pressure equilibrium.
Can selection of land, as shown in Figure 3, the condensing works 1 of titanium tetrachloride gases can also comprise temperature detector 1700, and temperature detector 1700 is located on blower fan 500. Like this can so that detection blower fan 500 temperature, to prevent cause system shutdown because temperature is too high, it is to increase the reliability of the condensing works 1 of titanium tetrachloride gases.
The compress control method of the condensing works 1 of titanium tetrachloride gases according to embodiments of the present invention is described below. The compress control method of the condensing works of titanium tetrachloride gases comprises the following steps:
A) the gas feed place pressure of the condensing works of titanium tetrachloride gases is detected:
B) when the pressure of gas feed place of the condensing works of titanium tetrachloride gases is more than or equal to scheduled pressure value, reduce the pressure at the offgas outlet place of the condensing works of titanium tetrachloride gases, when the pressure of gas feed place of the condensing works of titanium tetrachloride gases is less than described scheduled pressure value, increase the pressure at the offgas outlet place of the condensing works of described titanium tetrachloride gases.
For convenience of understanding, below the system and method for the titanium tetrachloride utilizing the present invention to prepare for the preparation of titanium dioxide is described.
In a first aspect of the present invention, the present invention proposes a kind of method preparing titanium dioxide. With reference to figure 1, according to embodiments of the invention, the method comprises:
S100: chlorination reaction
In this step, titaniferous ore, reductive agent are supplied in chlorination reactor, and to oxygen gas-supplying in described chlorination reactor, air and chlorine, there is chlorination reaction in described chlorination reactor, and obtain the chlorination reaction mixture containing titanium tetrachloride gases, wherein, described reductive agent is refinery coke, and described titaniferous ore is titanium slag or rutile titanium ore. Specifically, interpolation titanium ore (titanium slag or the rutile) reducing substances (refinery coke) that the production of titanium tetrachloride gases is mainly successive in chlorination reactor, and successive leading to into oxygen, pressurized air, Cl in reactor2; And temperature (titanium slag or rutile) and chlorine when 850 DEG C recur, and reaction is lasting generates TiCl4Gas, reaction equation is: 2TiO2+3C+4Cl2=2TiCl4+2CO+CO2. In one embodiment of the invention, described chlorination reaction carries out at the temperature of 700��900 degrees Celsius. Preferably, chlorination reaction carries out at the temperature of 850 degrees Celsius. Contriver, through the unexpected discovery of a large amount of experiment, carries out chlorination reaction under 850 degrees Celsius, it is possible to generate titanium tetrachloride to be significantly better than the efficiency of other temperature.
S200: the first gas solid separation
In this step, the chlorination reaction mixture obtained in preceding step is carried out gas solid separation process, to obtain the gaseous mixture containing titanium tetrachloride. According to embodiments of the invention, the method and the device that carry out the first gas solid separation can be any known means in this area.
S300: condensation process
In this step, the described gaseous mixture containing titanium tetrachloride is carried out condensation process, to obtain liquid titanium tetrachloride. In one embodiment of the invention, in this step, comprise further: by a part for described liquid titanium tetrachloride and the described gas mixture contacts containing titanium tetrachloride, to carry out the first cooling process; And utilize refrigerant that the gaseous mixture through the first cooling process is carried out the 2nd cooling process, to obtain described liquid titanium tetrachloride, wherein, described refrigerant is the R507 cooling medium of temperature-23 degrees Celsius. Contriver finds, by this method of cooling, it is possible to effectively cooled by the gaseous mixture containing titanium tetrachloride, thus realizes being further purified titanium tetrachloride. Wherein, for the first cooling process, the liquid titanium tetrachloride obtaining cooling can be effectively utilized cool, thus reduce the production cost producing titanium dioxide, in addition, adopting the R507 cooling medium of temperature-23 degrees Celsius as refrigerant, being that contriver is unexpected by a large amount of screening operation obtains, and finding, it can play a role to be significantly better than the cooling medium of other temperature and type.
S400: store
In this step, described liquid crude titanium tetrachloride preceding step obtained is stored in titanium tetrachloride storing device.
S500: except vanadium process
In this step, mineral oil is adopted to be carried out by described liquid crude titanium tetrachloride except vanadium process, to be refined by described liquid crude titanium tetrachloride, to obtain through refining refined titanic chloride, wherein, in the titanium tetrachloride that described process is refining, the content of vanadium is below 3ppm.
S600: oxidizing reaction
In this step, the refined titanic chloride obtained in preceding step and oxygen are supplied in oxidation reactor, there is oxidizing reaction TiCl in described oxidation reactor4+O2=TiO2+2Cl2, to obtain the oxidation mixtures containing titanium dioxide and chlorine. In one embodiment of the invention, before being supplied in oxidation reactor by the refined titanic chloride obtained and oxygen, in advance described refined titanic chloride and oxygen are carried out thermal pretreatment respectively. In one embodiment of the invention, in advance by described refined titanic chloride and oxygen preheat to being not less than 350 degrees Celsius and be not less than 1500 degrees Celsius. Thus, it is possible to improve the efficiency preparing titanium dioxide further, the cost preparing titanium dioxide is reduced. Contriver finds, is not less than 350 degrees Celsius with being not less than 1500 degrees Celsius by refined titanic chloride and oxygen being preheated to respectively, it is possible to significantly effectively reduce the cost preparing titanium dioxide. When temperature is too high, the cost required for preheating can significantly increase, and when the temperature is too low, then can consume too much energy in oxidation reactor.
S700: the two gas solid separation
The described oxidation mixtures obtained in preceding step is carried out gas solid separation, to obtain solid titanium dioxide and chlorine respectively. Contriver finds, utilizes the method can effectively prepare titanium dioxide, and then by titanium dioxide is carried out coating process, it is possible to effectively obtain the titanium dioxide of size-grade distribution excellence. In one embodiment of the invention, comprise further: the chlorine obtained in preceding step is back in chlorination reaction step and carries out chlorination reaction. Contriver finds, by the chlorine obtained after the 2nd gas solid separation, it is possible to be directly used in chlorination reaction, thus reduces the cost producing titanium dioxide, decreases pollution.
In a second aspect of the present invention, the present invention proposes a kind of system preparing titanium dioxide. With reference to figure 2, according to embodiments of the invention, this system comprises: chlorination reactor 2, first gas-solid separating device 3, condensing works 1, titanium tetrachloride storing device 4, refining plant 5, oxidation reactor 6 and the 2nd gas-solid separating device 7. According to embodiments of the invention, chlorination reactor 2 is provided with titanium ore entrance, reductive agent entrance, oxygen intake, gas inlet and chlorine entrance, titaniferous ore, reductive agent are supplied in described chlorination reactor, and to oxygen gas-supplying in described chlorination reactor, air and chlorine, there is chlorination reaction in described chlorination reactor, and obtain the chlorination reaction mixture containing titanium tetrachloride gases, wherein, described reductive agent is refinery coke, and described titaniferous ore is titanium slag or rutile titanium ore. First gas-solid separating device 3 is connected with chlorination reactor 2, for described chlorination reaction mixture is carried out gas solid separation process, to obtain the gaseous mixture containing titanium tetrachloride. Condensing works 1 is connected with the first gas solid separation 3 device, for the described gaseous mixture containing titanium tetrachloride is carried out condensation process, to obtain liquid titanium tetrachloride. Titanium tetrachloride storing device 4 is connected with condensing works 1, for storing described liquid crude titanium tetrachloride. Refining plant 5 is connected with titanium tetrachloride storing device 4, and be suitable for adopting mineral oil to be carried out by described liquid crude titanium tetrachloride except vanadium process, described liquid crude titanium tetrachloride is refined, to obtain through refining refined titanic chloride, wherein, in the titanium tetrachloride that described process is refining, the content of vanadium is below 3ppm. Oxidation reactor 6 is connected with refining plant 5, and it is provided with oxygen intake, for described refined titanic chloride and oxygen are supplied in oxidation reactor 6, there is oxidizing reaction in oxidation reactor 6, to obtain the oxidation mixtures containing titanium dioxide and chlorine. 2nd gas-solid separating device 7 is connected with oxidation reactor 6, for oxidation mixtures is carried out gas solid separation, to obtain solid titanium dioxide and chlorine respectively. Utilize this system, it is possible to effectively implement the aforementioned method preparing titanium dioxide.
In one embodiment of the invention, described condensing works 1 comprises further: adverse current cooling unit, described adverse current cooling unit is provided with chlorination reaction mixture entrance and liquid titanium tetrachloride entrance, so that by a part for described liquid titanium tetrachloride and the described gaseous mixture counter current contact containing titanium tetrachloride in described adverse current cooling unit, to carry out the first cooling process; And tubular heat exchanger, described tubular heat exchanger is connected with described adverse current cooling unit, and utilize refrigerant that the gaseous mixture through the first cooling process is carried out the 2nd cooling process, to obtain described liquid titanium tetrachloride, wherein, described refrigerant is the R507 cooling medium of temperature-23 degrees Celsius. Contriver finds, by this method of cooling, it is possible to effectively cooled by the gaseous mixture containing titanium tetrachloride, thus realizes being further purified titanium tetrachloride. Wherein, for the first cooling process, the liquid titanium tetrachloride obtaining cooling can be effectively utilized cool, thus reduce the production cost producing titanium dioxide, in addition, adopting the R507 cooling medium of temperature-23 degrees Celsius as refrigerant, being that contriver is unexpected by a large amount of screening operation obtains, and finding, it can play a role to be significantly better than the cooling medium of other temperature and type.
In one embodiment of the invention, comprise further: refined titanic chloride primary heater unit (not shown), described refined titanic chloride primary heater unit is connected with described oxidation unit 6 with described refining plant 5, in advance described refined titanic chloride is carried out thermal pretreatment; Oxygen preheat equipment (not shown), described oxygen preheat equipment is connected with described oxidation unit 6, in advance described oxygen is carried out thermal pretreatment. Thus, it is possible to improve the efficiency preparing titanium dioxide further, the cost preparing titanium dioxide is reduced. Contriver finds, is not less than 350 degrees Celsius with being not less than 1500 degrees Celsius by refined titanic chloride and oxygen being preheated to respectively, it is possible to significantly effectively reduce the cost preparing titanium dioxide. When temperature is too high, the cost required for preheating can significantly increase, and when the temperature is too low, then can consume too much energy in oxidation reactor.
In one embodiment of the invention, described 2nd gas-solid separating device 7 is connected with described chlorination reactor 6, carries out chlorination reaction for being back in described chlorination reactor by the chlorine obtained. Contriver finds, by the chlorine obtained after the 2nd gas solid separation, it is possible to be directly used in chlorination reaction, thus reduces the cost producing titanium dioxide, decreases pollution.
In the description of this specification sheets, at least one embodiment that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means to be contained in the present invention in conjunction with concrete feature, structure, material or feature that this embodiment or example describe or example. In this manual, the schematic representation of above-mentioned term is not necessarily referred to identical embodiment or example. And, the concrete feature of description, structure, material or feature can combine in an appropriate manner in any one or more embodiment or example.
Although it has been shown and described that embodiments of the invention, it will be understood by those skilled in the art that: these embodiments can be carried out multiple change, amendment, replacement and modification when not departing from principle and the objective of the present invention, the scope of the present invention by claim and etc. jljl limit.
Claims (7)
1. prepare the system of titanium tetrachloride for one kind, it is characterised in that, comprising:
Chlorination reactor, described chlorination reactor is provided with titanium ore entrance, reductive agent entrance, oxygen intake, gas inlet and chlorine entrance, titaniferous ore, reductive agent are supplied in described chlorination reactor, and to oxygen gas-supplying in described chlorination reactor, air and chlorine, there is chlorination reaction in described chlorination reactor, and obtain the chlorination reaction mixture containing titanium tetrachloride gases, wherein, described reductive agent is refinery coke, and described titaniferous ore is titanium slag or rutile titanium ore;
First gas-solid separating device, described first gas-solid separating device is connected with described chlorination reactor, for described chlorination reaction mixture is carried out gas solid separation process, to obtain the gaseous mixture containing titanium tetrachloride;
Condensing works, described condensing works is connected with described first gas-solid separating device, for the described gaseous mixture containing titanium tetrachloride is carried out condensation process, to obtain liquid titanium tetrachloride; And
Titanium tetrachloride storing device, described titanium tetrachloride storing device is connected with described condensing works, for storing described liquid crude titanium tetrachloride;
Control device, described control device is connected with described condensing works, and described condensing works is controlled by the amount for the chlorination reaction mixture containing titanium tetrachloride gases produced according to described chlorination reactor,
Wherein, described condensing works comprises:
One-level direct condenser, described one-level direct condenser has the first gas inlet, first liquid entrance and gas liquid outlet;
Receiving tank, the import of described receiving tank is connected with described gas liquid outlet;
Two grades of direct condensers, described two grades of direct condensers have the 2nd gas inlet, second liquid entrance and pneumatic outlet, and described 2nd gas inlet is connected with the outlet of described receiving tank;
Indirect condenser, described indirect condenser has inlet mouth, air outlet and liquid outlet, and described inlet mouth is connected with described pneumatic outlet;
Blower fan, described blower fan is connected to described air outlet place;
Storage groove, described storage groove is connected with described liquid outlet;
Droplet separator, described droplet separator is connected between described air outlet and described blower fan, and described droplet separator is connected with described storage groove.
2. system according to claim 1, it is characterised in that, described condensing works comprises further:
Adverse current cooling unit, described adverse current cooling unit is provided with chlorination reaction mixture entrance and liquid titanium tetrachloride entrance, so that by a part for described liquid titanium tetrachloride and the described gaseous mixture counter current contact containing titanium tetrachloride in described adverse current cooling unit, to carry out the first cooling process; And
Tubular heat exchanger, described tubular heat exchanger is connected with described adverse current cooling unit, and utilize refrigerant that the gaseous mixture through the first cooling process is carried out the 2nd cooling process, to obtain described liquid titanium tetrachloride, wherein, described refrigerant is the R507 cooling medium of temperature-23 degrees Celsius.
3. system according to claim 1, it is characterised in that, described condensing works also comprises self-acting valve, and one end of described self-acting valve is connected between described droplet separator and described blower fan and the other end is connected to the exit of described blower fan.
4. system according to claim 3, it is characterized in that, described condensing works also comprises controller, first gas inlet place of described one-level direct condenser is provided with the first pressure detector, described controller is connected with described self-acting valve with described first pressure detector, described blower fan respectively, and described controller controls the rotating speed of described blower fan and the opening and closing of described self-acting valve according to the detected pressure value of described first pressure detector.
5. system according to claim 4, it is characterized in that, described blower fan is roots blower, when the detected pressure value of described first pressure detector is more than or equal to scheduled pressure value, described controller controls described self-acting valve and cuts out and the rotating speed that controls described blower fan is greater than desired speed, when the detected pressure value of described first pressure detector is less than described scheduled pressure value, described controller controls described self-acting valve and opens and the rotating speed that controls described blower fan is less than described desired speed.
6. system according to claim 4, it is characterized in that, the gas outlet of described two grades of direct condensers is provided with the 2nd pressure detector, the 3rd pressure detector it is provided with between described droplet separator and described blower fan, and described 3rd pressure detector is between described droplet separator and described self-acting valve, the exit of described blower fan is provided with the 4th pressure detector.
7. system according to claim 6, it is characterized in that, described condensing works also comprises the first pressure detector, the 2nd pressure detector and the 3rd pressure detector, described first pressure detector is connected with described 2nd pressure detector with described first pressure detector respectively, described 2nd pressure detector is connected with described 3rd pressure detector with described 2nd pressure detector respectively, and described 3rd pressure detector is connected with described 4th pressure detector with described 3rd pressure detector respectively.
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