CN104891560A - Producing process and equipment for crude titanium tetrachloride - Google Patents
Producing process and equipment for crude titanium tetrachloride Download PDFInfo
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Abstract
A producing process for crude titanium tetrachloride is disclosed. The producing process includes a) adding a titanium-rich material into a high-temperature chlorination furnace and chlorinating; b) feeding chlorinated flue gas obtained after chlorination into a first flue gas purification system, with the temperature of chlorinated flue gas discharged from the first flue gas purification system being 150-180 DEG C; c) feeding the chlorinated flue gas discharged from the first flue gas purification system to a second flue gas purification system, with the solid content of chlorinated flue gas discharged from the second flue gas purification system being not more than 10 mg/Nm<3>; and d) feeding the chlorinated flue gas discharged from the second flue gas purification system into a leaching tower, cooling, and separating to finally obtain the crude titanium tetrachloride. Producing equipment for the crude titanium tetrachloride is also disclosed. The crude titanium tetrachloride having a low impurity content can be finally obtained by the producing process and the producing equipment. The producing equipment is saved in the process, thus reducing the production cost.
Description
Technical field
The present invention relates to titanium field of metallurgy, be specifically related to a kind of production technique and equipment thereof of crude titanic chloride.
Background technology
Metal titanium excellent performance, be widely used in the fields such as aerospace, national defense industry, petrochemical complex, medicine equipment and sports equipment, China's titanium resource owning amount accounts for 30% of global proven reserve, in China, development titanium resource processing and utilization industry has advantageous condition, along with the economy of China constantly increases, the consumption of titanium is also in quick growth.Titanium tetrachloride is as the main production raw material of titanium sponge and titanium dioxide, and its demand also increases thereupon.Traditional titanium tetrachloride Production Flow Chart is as follows: with rich titanium material, (" rich titanium material " mainly comprises natural rutile, titanium slag, artificial rutile and ilmenite) put into chlorination furnace as raw materials for production, the mixed chlorinated flue gas containing titanium tetrachloride is obtained after superchlorination operation, described mixed chlorinated flue gas is through gathering dust, drip washing, sedimentation, filter the operation of a series of condensation separation and obtain crude titanic chloride, finally the crude titanic chloride of gained is finally obtained refining titanic chloride through purification operations, foreign matter content wherein in crude titanic chloride directly has influence on the purity of final obtained refined titanic chloride, the quality of the titanium sponge that final impact is produced and titanium dioxide.In actual production, after drip washing gained titanium tetrachloride feed liquid in solid impurity content very high, feed liquid is caused to be muddy, therefore needed to carry out settlement treatment by thickener to the silt particle in feed liquid before carrying out filter operation, in treating processes, the mud lifting gear of thickener inside very easily breaks down, parking maintenance difficulty after breaking down, need to take a long time just to make thickener again normally work, and titanium tetrachloride very easily leaks in maintenance process, cause environmental pollution, the titanium tetrachloride loss caused in order to avoid stopping, factory is multiple thickener for subsequent use often, but this kind of method considerably increases production cost, after settling operation, mud is separated to a certain extent with titanium tetrachloride chlorination flue gas, part factory is directly by mud discharger, this kind of mode is also inadvisable, mud can cause environmental pollution, mud is back to chlorination furnace or one-level gravity dust-precipitator by some factory, high temperature is utilized to be gasified by mud, raw slag is collected after eventually passing dust-precipitator cooling, this kind of mode is slurry process in main at present titanium tetrachloride process, but mud affects greatly for chlorination furnace and follow-up dust collection device, easily cause the damage of aforesaid device, in the crude titanic chloride finally obtained, impurity particle content is higher, be unfavorable for that subsequent fine titanium tetrachloride is produced.
Summary of the invention
Technical problem to be solved by this invention is that providing a kind of produces the less crude titanic chloride production technique of impurity, present invention also offers a kind of crude titanic chloride production unit realizing above-mentioned production technique.
In order to solve the problem of above-mentioned prior art, the present invention realizes by the following technical solutions:
The invention provides a kind of crude titanic chloride production technique, its step comprises:
A, in high-temp chlorination stove, add rich titanium material carry out chlorination operation;
B, chlorination operated after the chlorination flue gas of gained pass in the first flue gas purification system, from the first flue gas purification system, chlorination flue-gas temperature is out 150 ~ 180 DEG C;
C, pass into the second flue gas purification system by chlorination flue gas out in the first flue gas purification system, from the second flue gas purification system, the solid content of chlorination flue gas is out≤10mg/Nm
3;
D, the chlorination flue gas exported from the second flue gas purification system enter into eluting column refrigerated separation and finally obtain crude titanic chloride.
Rich titanium material, chlorine and coke react and discharge high-temp chlorination flue gas from chlorination furnace roof in chlorination furnace, the steam that now in chlorination flue gas, main component comprises steam that solid impurity particle, titanium tetrachloride and some other metal chloride formed, boiling point is formed lower than the material of titanium tetrachloride higher than the material of titanium tetrachloride and boiling point, also comprises the Cl in chlorination furnace
2, CO, CO
2, COCl
2deng waste gas.In order to make to produce without mud in crude titanic chloride production process, the chlorination flue-gas temperature controlled before drip washing from the first flue gas purification system is out 150 ~ 180 DEG C, boiling point due to aluminum chloride in metal chloride is 180.2 DEG C, the boiling point of iron(ic) chloride is 318.9 DEG C, therefore before chlorination flue gas is discharged from the first flue gas purification system, under this temperature condition, all transfer solid particulate to higher than metal chlorides such as the iron(ic) chloride of titanium tetrachloride boiling point, aluminum chloride, and the solid particulate of a part is removed in the first flue gas purification system.The second flue gas purification system is passed into afterwards, chlorination flue gas solid content≤10mg/Nm out from the second flue gas purification system from the first flue gas purification system chlorination flue gas out
3, enter thus in the chlorination flue gas in eluting column and only contain a small amount of lower-boiling impurity and crude titanic chloride, can not mud be produced after eluting column drip washing, finally obtain the crude titanic chloride that foreign matter content is less.
Particularly, described first flue gas purification system comprises at least one-level machinery dust-precipitator and/or at least first level filtering device, it is 150 ~ 180 DEG C by controlling chlorination flue-gas temperature out from last step machinery dust-precipitator or filtration unit, under this temperature condition, all transfer solid particulate to higher than metal chlorides such as the iron(ic) chloride of titanium tetrachloride boiling point, aluminum chloride, solid particulate is partly deposited in mechanical dust-precipitator or is tackled in filtration unit.
Particularly, described second flue gas purification system comprises at least first level filtering device, chlorination flue gas solid content≤10mg/Nm out from last step filtration unit
3, nearly all solid particulate is filtered device and filters out, for follow-up drip washing provides the less refrigerated separation raw material of impurity.
As the further improvement of above-mentioned crude titanic chloride production technique, in described filtration unit, the mean pore size of filter core is 10 ~ 40 μm, porosity is 20 ~ 70%, thickness is 1 ~ 5mm, under this Parameter Conditions, the filtering accuracy of filtration unit is the highest, and the chlorination flue gas impurity entered thus in eluting column is minimum.
As the further improvement of above-mentioned crude titanic chloride production technique, powder sintered porous filtering alloy or powder sintered porous ceramic film material are formed.Study discovery according to the present inventor, under the temperature condition of 150 ~ 180 DEG C, aluminum chloride and iron(ic) chloride and other high boiling substance are all converted into solid particulate state, these solid particulates and above-mentioned Cl
2, CO, CO
2, COCl
2jointly form the chlorination flue gas with severe corrosive under the high temperature conditions Deng waste gas, the anticorrosive filter core therefore adopting powder sintered porous filtering alloy or powder sintered porous ceramic film material to form can realize above-mentioned chlorination smoke filtration.
Particularly, described powder sintered porous filtering alloy be substantially by by mass percentage 14 ~ 17% Cr, the Fe of 6 ~ 10%, C, the Si of 0 ~ 0.5%, Mn, Cu, the Al of 0 ~ 5% of 0 ~ 0.05%, the Ni of the Ti of 0 ~ 1.5% and surplus of 0 ~ 1% of 0 ~ 0.15% form.In prior art, from mechanical dust-precipitator, high-temp chlorination flue gas out comprises other metal chlorides such as titanium tetrachloride, iron(ic) chloride and aluminum chloride, also comprises some lower-boiling impurities and Cl
2, CO, CO
2, COCl
2deng waste gas, the boiling point of the metal chlorides such as above-mentioned iron(ic) chloride and aluminum chloride all higher than titanium tetrachloride and under smoke behavior with Cl
2, CO, CO
2, COCl
2the chlorination flue gas had compared with severe corrosive is mixed into Deng waste gas, therefore from mechanical dust-precipitator, chlorination flue gas out generally first passes into in eluting column in the prior art, feed liquid is translated into through eluting column drip washing, a large amount of mud can be produced in this process, after drip washing, feed liquid is through recycle pump groove, need through thickener sedimentation before filtration from recycle pump groove feed liquid out, finally just obtain crude titanic chloride by filtration devices, thickener easily breaks down to cause producing and stops in process of production, the foreign matter content of the crude titanic chloride finally obtained is also very high.The filter core that the powder sintered porous filtering alloy that the present invention adopts above-mentioned condition to form is formed has the characteristic of good resistance to chlorine, hydrogen chloride gas corrosion, the gas solid separation be particularly useful under high temperature chlorine, hydrogenchloride system is filtered, therefore, it is possible to filter out the chlorination flue gas with severe corrosive.
Present invention also offers a kind of crude titanic chloride production unit, comprise high-temp chlorination stove, described high-temp chlorination stove is connected with the first flue gas purification system of discharge 150 ~ 180 DEG C of chlorination flue gases, described first flue gas purification system comprises at least one-level machinery dust-precipitator and/or at least first level filtering device, and described first flue gas purification system is connected with discharge solid content≤10mg/Nm
3second flue gas purification system of chlorination flue gas, described second flue gas purification system comprises at least first level filtering device, and the last step filtration unit of described second flue gas purification system is connected with eluting column.
As the further improvement of above-mentioned crude titanic chloride production unit, the mean pore size of the filter core of described filtration unit is 10 ~ 40 μm, and porosity is 20 ~ 70%, and thickness is 1 ~ 5mm.
Further, in described filtration unit, filter core is made up of powder sintered porous filtering alloy or powder sintered porous ceramic film material.
Further, described powder sintered porous filtering alloy be substantially by by mass percentage 14 ~ 17% Cr, the Fe of 6 ~ 10%, C, the Si of 0 ~ 0.5%, Mn, Cu, the Al of 0 ~ 5% of 0 ~ 0.05%, the Ni of the Ti of 0 ~ 1.5% and surplus of 0 ~ 1% of 0 ~ 0.15% form.
Below by way of the drawings and specific embodiments, the present invention is further described.
Accompanying drawing explanation
Fig. 1 is a kind of crude titanic chloride production unit process flow sheet of the present invention.
Fig. 2 is another kind of crude titanic chloride production unit process flow sheet of the present invention.
Fig. 3 is the crude titanic chloride production unit process flow sheet in comparative example 3.
Embodiment
As shown in Figure 1, provide a kind of production technique of crude titanic chloride in the present embodiment, its processing step is as follows:
A, pass into rich titanium material ilmenite, chlorine and coke in high temperature chlorine stove 1a, the throat temperature of described high-temp chlorination stove 1a is 850 DEG C, and titanium slag, chlorine and coke form high-temp chlorination flue gas after reacting under this hot conditions;
B, high-temp chlorination flue gas out in high-temp chlorination stove 1a is passed into one-level gravity dust-precipitator 2a1 and secondary gravity dust-precipitator 2a2 successively, control is 350 ~ 550 DEG C from one-level gravity dust-precipitator 2a1 chlorination flue-gas temperature out, solid particulate is transferred to higher than the material of titanium tetrachloride at this temperature condition next section boiling point, in these solid particulates, major part is discharged bottom one-level gravity dust-precipitator 2a1 with the form of dust-slag collection, rest part enters secondary gravity dust-precipitator 2a2 together with chlorination flue gas, controlling chlorination flue-gas temperature out from secondary gravity dust-precipitator 2a2 is 150 ~ 180 DEG C, higher than the iron(ic) chloride of titanium tetrachloride boiling point under this temperature condition, the metal chlorides such as aluminum chloride all transfer solid particulate to,
C, in secondary gravity dust-precipitator 2a2, a part of solid particulate is discharged bottom secondary gravity dust-precipitator 2a2 with the form of dust-slag collection, another part enters filtration unit 3a together with chlorination flue gas, and from filtration unit 3a, chlorination flue gas solid content is out≤10mg/Nm
3, the titanium tetrachloride only containing steam condition from the chlorination flue gas after filtration unit 3a filters, small part are compared to the low-boiling point material of titanium tetrachloride and waste gas, and described waste gas is Cl
2, CO, CO
2, COCl
2deng;
D, chlorination flue gas after filtration unit 3a filters enter eluting column 4a and carry out, in eluting column 4a, the temperature of leacheate controls at normal temperature, titanium tetrachloride in chlorination flue gas and some low-boiling point materials transfer solid as silicon tetrachloride to and are mixed to form feed liquid with leacheate in eluting column 4a, finally obtain crude titanic chloride;
For the equipment of above-mentioned crude titanic chloride production technique, comprise high-temp chlorination stove 1a, described high-temp chlorination stove 1a is connected with one-level gravity dust-precipitator 2a1 successively, discharges the secondary gravity dust-precipitator 2a2 of 150 ~ 180 DEG C of chlorination flue gases, discharges solid content≤10mg/Nm
3chlorination filtrating equipment of flue gas 3a, described filtration unit is connected with eluting column 4a.
In the present invention, from secondary gravity dust-precipitator 2a2, the thermal creep stress standard of chlorination flue gas is out: make chlorination flue gas when discharging secondary gravity dust-precipitator 2a2, the metal chloride such as iron(ic) chloride, aluminum chloride wherein higher than titanium tetrachloride boiling point all transfers solid particulate to, is convenient to subsequent filter device thus and filters.
Embodiment 1 ~ 4 and comparative example 1 ~ 2 (see next page table 1)
Form 1
By embodiment 1 ~ 4 wherein according to the diameter of solid particulate in chlorination flue gas, determine that the filter core mean pore size that nickel-based intermetallic compound material is formed is 15 μm, porosity is 45%, thickness is 3mm, under above-mentioned parameter condition embodiment 1 and embodiment 2 from first level filtering device in chlorination flue gas out solid content be 5mg/Nm
3, in embodiment 3 and embodiment 4, in chlorination flue gas out, solid content is 8mg/Nm
3.
In above-described embodiment 1 ~ 4 crude titanic chloride production technique, solid impurity most in chlorination flue gas removes by filtration unit under smoke behavior, and corrosion can not be produced to filter core, the feed liquid produced in eluting column can not be slurry condition, the crude titanic chloride that final acquisition foreign matter content is less, simplify titanium tetrachloride production technique program, decrease the production units such as the thickener easily broken down, eliminate source of trouble on the one hand, make production can continue to carry out, save crude titanic chloride production cost on the other hand, treating process for follow-up crude titanic chloride provides good raw material.
When in embodiment 1 ~ 4, from secondary gravity dust-precipitator, chlorination flue-gas temperature is out between 150 DEG C ~ 180 DEG C as shown in Table 1, be waste gas and titanium tetrachloride chlorination flue gas from filtration unit chlorination smoke components out, crude titanic chloride can be obtained after this chlorination flue gas enters follow-up eluting column, and produce without mud in process, in the final crude titanic chloride obtained, foreign matter content is less; In comparative example 1, when from secondary gravity dust-precipitator, chlorination flue-gas temperature is out 130 DEG C, because part titanium tetrachloride transforms before filtration in order to liquid state, although do not have mud to produce in process, but because titanium tetrachloride transforms in this process in order to liquid titanium tetrachloride, be not easy to follow-up acquisition crude titanic chloride product; In comparative example 2, when from secondary gravity dust-precipitator, chlorination flue-gas temperature is out 190 DEG C, because temperature is higher than the boiling point of aluminum chloride, aluminum chloride and some boiling points are still chlorination smoke behavior higher than titanium tetrachloride but lower than the material of this temperature, after now chlorination flue gas enters follow-up eluting column, have mud produce and in the crude titanic chloride obtained foreign matter content apparently higher than embodiment 1 ~ 4, draw best results between 150 DEG C ~ 180 DEG C by embodiment 1 ~ 4 paired observation.
From filtration unit chlorination flue gas out, main component is TiCl
4, AlCl
3, FeCl
3deng metal chloride and Cl
2, CO, CO
2, COCl
2deng gas, this chlorination flue gas has stronger corrodibility, the filter core be made up of powder sintered porous filtering alloy or powder sintered porous ceramic film material can overcome above-mentioned chlorination flue gas corrosion, powder sintered porous filtering alloy described in this test is by the Cr of 14%, Fe, the Si of 0.2%, Mn, Cu, the Al of 2% of 0.02%, the Ni of the Ti of 0.5% and surplus of 0.5% of 6% form, or adopt Al series metal compounds porous material as titanium aluminium or intermetallic Fe-Al compound porous material by mass percentage substantially.Above-mentioned filter core is hung in the airtight chamber being full of described chlorination flue gas, the temperature of chlorination flue gas controls at 350 DEG C, now flue gas major part material is in steam condition, it is below the test-results of one-period, one-period is 30 days, its anti-chlorination flue gas corrosion test of the filter core be made up of powder sintered porous filtering alloy is in table 2, and its anti-chlorination flue gas corrosion test of the filter core be made up of intermetallic Fe-Al compound porous material under equivalent assay conditions is in table 3 (see next page table 2 and form 3).
Form 2
Repeat above-mentioned test, find within a test period, the filter core be made up of powder sintered porous filtering alloy is all unchanged in outward appearance, color, microtexture and ultimate compression strength, even if extend a test period more also without considerable change, illustrate that the filter core be made up of above-mentioned powder sintered porous filtering alloy can resist chlorination flue gas corrosion and withstand high temperatures.
Form 3
Repeat above-mentioned test, when finding that test period reaches 30 days, the filter core outside surface be made up of intermetallic Fe-Al compound porous material has parts against wear, color part blackening, observe filter core section and find that the inner aperture of filter core becomes large and has dust to infiltrate, test ultimate compression strength is also compared to dying down before, and the filter core be made up of intermetallic Fe-Al compound porous material when reaching 30 days between illustrating at the trial has corrosion phenomenon to occur.
Contrast table 2 and table 3, the anti-chlorination flue gas corrosion of the filter core be made up of powder sintered porous filtering alloy and resistance to elevated temperatures are all better than intermetallic Fe-Al compound.
Embodiment 5
As shown in Figure 2, provide production technique and the equipment thereof of another kind of crude titanic chloride in the present embodiment, its technical process is as follows:
A, pass into neutral red metal and stone, chlorine and coke in high temperature chlorine stove 1a, the throat temperature of described high-temperature chlorine steam stove 1a is 850 DEG C, and neutral red metal and stone, chlorine and coke form high-temp chlorination flue gas after reacting under this hot conditions;
B, high-temp chlorination flue gas out in high-temp chlorination stove 1a is passed into first level filtering device 3a1, the chlorination flue-gas temperature controlled in first level filtering device 3a2 is 400 DEG C, under this temperature condition, chlorination flue gas mid-boiling point transfers solid particulate to higher than the material of titanium tetrachloride and is tackled by first level filtering device, solid particulate and the chlorination flue gas of residue high boiling substance enter two-stage filter 3a2, control from two-stage filter 3a2 chlorination flue-gas temperature be out 150 DEG C, higher than the iron(ic) chloride of titanium tetrachloride boiling point under this temperature condition, the metal chlorides such as aluminum chloride all transfer solid particulate to,
A part of solid particulate in c, above-mentioned two-stage filter 3a2 is tackled by two-stage filter 3a2, another part together enters three-level filter device 3a3 with chlorination flue gas now, now the solid particulate of 99.9% is filtered out by three-level filter device 3a3, only containing titanium tetrachloride chlorination flue gas and the small part low-boiling point material compared to titanium tetrachloride from the chlorination flue gas after three-level filter device 3a3 filters;
D, chlorination flue gas after described three-level filter device 3a3 filters enter eluting column, in eluting column 4a, the temperature of leacheate controls as normal temperature, titanium tetrachloride in chlorination flue gas and some low-boiling point materials transfer solid as silicon tetrachloride to and are mixed to form feed liquid with leacheate in eluting column, and the waste gas entering eluting column 4a with chlorination flue gas is discharged from eluting column 4a top;
The filter core of above-mentioned filtration unit is made up of powder sintered porous filtering alloy, described powder sintered porous filtering alloy according to by mass percentage 17% Cr, the Fe of 10%, C, the Si of 0.5%, Mn, Cu, the Al of 5% of 0.05%, the Ni of the Ti of 1.5% and surplus of 1% of 0.15% form.Wherein according to the diameter of solid particulate in chlorination flue gas, the mean pore size determining the filter core that powder sintered porous filtering alloy is formed is 25 μm, porosity is 50%, and thickness is 4mm, under this Parameter Conditions from the solid content of three-level filter device chlorination flue gas be out 10mg/Nm
3.
In above-mentioned crude titanic chloride production technique, solid impurity nearly all in chlorination flue gas removes by filtration unit under smoke behavior, and corrosion can not be produced to filter core, the feed liquid produced in eluting column can not be obvious slurry condition, the crude titanic chloride that final acquisition foreign matter content is less, simplify titanium tetrachloride production technique program, decrease the production units such as the thickener easily broken down, eliminate source of trouble on the one hand, make production can continue to carry out, save crude titanic chloride production cost on the other hand, for the refining of follow-up crude titanic chloride provides good raw material.
The present embodiment additionally provides a kind of equipment for above-mentioned crude titanic chloride production technique, draw together high-temp chlorination stove 1a, described high-temp chlorination stove 1a is connected with first level filtering device 3a1 successively, two-stage filter 3a2, three-level filter device 3a3, described three-level filter device 3a3 is connected with eluting column 4a, described first level filtering device 3a1, two-stage filter 3a2, filter core in three-level filter device 3a3 is formed by anti-chlorination flue gas corrosion porous material, filter core is made up of powder sintered porous filtering alloy, described powder sintered porous filtering alloy according to by mass percentage 17% Cr, the Fe of 10%, the C of 0.15%, the Si of 0.5%, the Mn of 1%, the Cu of 0.05%, the Al of 5%, the Ti of the 1.5% and Ni of surplus is formed.The mean pore size of the filter core of described filtration unit 3a is 25 μm, and porosity is 50%, and thickness is 4mm.
Comparative example 3
As shown in Figure 3 in this comparative example, crude titanic chloride production craft step is as follows:
A, the employing raw materials for production identical with embodiment 1 join in chlorination furnace 1b, and the throat temperature of chlorination furnace 1b controls at 850 ~ 900 DEG C equally;
The chlorination flue gas produced in b, chlorination furnace 1b enters in dust-precipitator 2b, and the chlorination flue-gas temperature of dust-precipitator 2b entrance is 400 ~ 500 DEG C, some high boiling materials condensation under this temperature condition, and discharges with the mode sedimentation of dust-slag collection in dust-precipitator 2b;
C, from dust-precipitator 2b, chlorination flue gas out enters to eluting column 4b, the chlorination flue-gas temperature entering eluting column 4b is 450 DEG C, now chlorination smoke components comprises metal chloride and some lower-boiling impurities such as titanium tetrachloride, iron(ic) chloride, aluminum chloride, and similarly in eluting column 4b, the temperature of leacheate controls at normal temperature;
D, be converted into mud and waste gas by the post chlorization flue gas of eluting column 4b drip washing, waste gas is discharged from eluting column 4b top;
E, the feed liquid of discharging from eluting column 4b enter thickener 5 and carry out sedimentation, and device 3b filters after filtration afterwards, finally obtains crude titanic chloride.
Wherein filtration unit adopts the filtration unit used in existing crude titanic chloride production system.
Iron(ic) chloride in step c, the metal chlorides such as aluminum chloride all enter eluting column and form mud, in order to isolate the titanium tetrachloride in mud, in step e, the mud of formation is carried out sedimentation in thickener, because the mud amount produced in process is larger, mechanicalness and corrodibility stronger, very easily cause thickener fault, a large amount of mud waste residues is produced after separation, direct discharge mud waste residue can produce environment and pollute, mud waste residue to be back in chlorination furnace chlorination again and easily to cause the structure deteriorate such as chlorination furnace and dust-precipitator, part mud is still mixed with in feed liquid after sedimentation, therefore need to pass through filtration devices, but because mud easily causes filtration unit to block, make filter effect undesirable.
In the crude titanic chloride finally obtained by the crude titanic chloride production technique in this comparative example 3, impurity particle content is higher, be unfavorable for that subsequent fine titanium tetrachloride is produced, and thickener very easily breaks down in production process, titanium tetrachloride is caused to lose larger, production process is discontinuous, and production cost is increased.
Claims (10)
1. crude titanic chloride production technique, its step is as follows:
A, in high-temp chlorination stove (1a), add rich titanium material carry out chlorination operation;
B, chlorination operated after the chlorination flue gas of gained pass in the first flue gas purification system (2a), be 150 ~ 180 DEG C from the first flue gas purification system (2a) chlorination flue-gas temperature out;
C, chlorination flue gas out in the first flue gas purification system (2a) is passed into the second flue gas purification system (3a), the solid content≤10mg/Nm of chlorination flue gas out from the second flue gas purification system (3a)
3;
D, the chlorination flue gas exported from the second flue gas purification system (3a) enter into eluting column (4a) refrigerated separation and finally obtain crude titanic chloride.
2. crude titanic chloride production technique as claimed in claim 1, is characterized in that: described first flue gas purification system (2a) comprises at least one-level machinery dust-precipitator and/or at least first level filtering device.
3. crude titanic chloride production technique as claimed in claim 1, is characterized in that: described second flue gas purification system (3a) comprises at least first level filtering device.
4. crude titanic chloride production technique as claimed in claim 2 or claim 3, it is characterized in that: in described filtration unit, the mean pore size of filter core is 10 ~ 40 μm, porosity is 20 ~ 70%, and thickness is 1 ~ 5mm.
5. crude titanic chloride production technique as claimed in claim 2 or claim 3, is characterized in that: in described filtration unit, filter core is made up of powder sintered porous filtering alloy or powder sintered porous ceramic film material.
6. crude titanic chloride production technique as claimed in claim 5, is characterized in that: its be substantially by by mass percentage 14 ~ 17% Cr, the Fe of 6 ~ 10%, C, the Si of 0 ~ 0.5%, Mn, Cu, the Al of 0 ~ 5% of 0 ~ 0.05%, the Ni of the Ti of 0 ~ 1.5% and surplus of 0 ~ 1% of 0 ~ 0.15% form.
7. crude titanic chloride production unit, comprise high-temp chlorination stove (1a), it is characterized in that: described high-temp chlorination stove (1a) is connected with first flue gas purification system (2a) of discharge 150 ~ 180 DEG C of chlorination flue gases, described first flue gas purification system (2a) comprises at least one-level machinery dust-precipitator and/or at least first level filtering device, and described first flue gas purification system (2a) is connected with discharge solid content≤10mg/Nm
3second flue gas purification system (3a) of chlorination flue gas, described second flue gas purification system (3a) comprises at least first level filtering device, and in described second flue gas purification system (3a), last step filtration unit is connected with eluting column (4a).
8. crude titanic chloride production unit as claimed in claim 7, is characterized in that: the mean pore size of the filter core of described filtration unit is 10 ~ 40 μm, and porosity is 20 ~ 70%, and thickness is 1 ~ 5mm.
9. crude titanic chloride production unit as claimed in claim 7, is characterized in that: the filter core in described filtration unit is made up of powder sintered porous filtering alloy or powder sintered porous ceramic film material.
10. crude titanic chloride production unit as claimed in claim 9, is characterized in that: its be substantially by by mass percentage 14 ~ 17% Cr, the Fe of 6 ~ 10%, C, the Si of 0 ~ 0.5%, Mn, Cu, the Al of 0 ~ 5% of 0 ~ 0.05%, the Ni of the Ti of 0 ~ 1.5% and surplus of 0 ~ 1% of 0 ~ 0.15% form.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106495211A (en) * | 2016-11-29 | 2017-03-15 | 河南佰利联新材料有限公司 | A kind of method for reducing titanium tetrachloride production cost |
| CN106586962A (en) * | 2016-11-23 | 2017-04-26 | 昆明理工大学 | Method for recycling hydrochloric acid through vapor neutral hydrolysis of titanium tetrachloride dust collection residues |
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| CN106586962A (en) * | 2016-11-23 | 2017-04-26 | 昆明理工大学 | Method for recycling hydrochloric acid through vapor neutral hydrolysis of titanium tetrachloride dust collection residues |
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| CN113880136A (en) * | 2020-07-03 | 2022-01-04 | 新疆硅基新材料创新中心有限公司 | Zirconium tetrachloride and/or silicon tetrachloride, preparation method and preparation device thereof |
| CN113880136B (en) * | 2020-07-03 | 2024-03-22 | 新疆硅基新材料创新中心有限公司 | Zirconium tetrachloride and/or silicon tetrachloride, preparation method and preparation device thereof |
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| CN112892097A (en) * | 2021-01-30 | 2021-06-04 | 成都易态科技有限公司 | Method for treating mixed gas |
| CN112892097B (en) * | 2021-01-30 | 2022-05-13 | 成都易态科技有限公司 | Method for treating mixed gas |
| CN112807921B (en) * | 2021-01-30 | 2022-05-13 | 成都易态科技有限公司 | Mixed gas processing system |
| CN112892147B (en) * | 2021-01-30 | 2022-05-13 | 成都易态科技有限公司 | Method for treating mixed gas |
| CN113247947A (en) * | 2021-06-08 | 2021-08-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for removing vanadium from crude titanium tetrachloride |
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