CN112456548A - Titanium tetrachloride production system and method - Google Patents
Titanium tetrachloride production system and method Download PDFInfo
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- CN112456548A CN112456548A CN202011464747.4A CN202011464747A CN112456548A CN 112456548 A CN112456548 A CN 112456548A CN 202011464747 A CN202011464747 A CN 202011464747A CN 112456548 A CN112456548 A CN 112456548A
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- C01G23/00—Compounds of titanium
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- C01G23/022—Titanium tetrachloride
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Abstract
The invention relates to the technical field of titanium dioxide production, in particular to a titanium tetrachloride production system and a titanium tetrachloride production method; the system comprises a chlorination furnace and a cyclone separator, wherein the bottom and the top of the chlorination furnace are respectively provided with an air inlet and a material outlet, and a furnace body of the chlorination furnace is provided with a material inlet; the bottom and the top of the cyclone separator are respectively provided with a slag discharge port and an exhaust port, and a feed inlet is arranged on the body of the cyclone separator; the discharge port of the chlorination furnace is communicated with the feed port of the cyclone separator through a pipeline; the outer walls and the linings of the cyclone separator and the pipeline respectively consist of a carbon steel layer and a fire-resistant layer; the invention provides a system and a method suitable for producing titanium tetrachloride, which can ensure that metal chloride can be effectively separated from unreacted titanium-rich material and petroleum coke, so that the production cost of the titanium tetrachloride can be reduced.
Description
Technical Field
The invention relates to the technical field of titanium dioxide production, in particular to a titanium tetrachloride production system and a titanium tetrachloride production method.
Background
Titanium dioxide, also known as titanium dioxide, is white loose powder, has the function of shielding ultraviolet rays and good dispersibility and weather resistance, and is widely applied to the fields of cosmetics, functional fibers, plastics, coatings, pigments, paints, fine ceramics, rubber and the like. The chlorination process is one of the mainstream production methods of titanium dioxide, and under the condition that the titanium dioxide is blocked by foreign implementation technologies, China grasps part of key technologies through difficult exploration for many years and gradually realizes industrial production. The main procedures of the chlorination method for producing titanium dioxide comprise chlorination, oxidation and post-treatment. The chlorination refers to a process of generating titanium tetrachloride by taking a titanium-rich material, petroleum coke and chlorine as raw materials through chlorination reaction, the oxidation refers to a process of oxidizing the titanium tetrachloride to generate titanium dioxide and realizing dechlorination, and the post-treatment refers to a process of forming a product through steps of pulping, grinding, surface treatment, washing, drying, crushing and the like.
At present, in the chlorination process, after the chlorination reaction of the titanium-rich material, the petroleum coke and the chlorine is completed in the chlorination furnace, products such as gaseous titanium tetrachloride, other gaseous metal chlorides and raw materials such as the titanium-rich material and the petroleum coke which are not completely reacted exist in the chlorination furnace, after the titanium tetrachloride slurry is sprayed reversely, the mixed material is rapidly cooled to 180-250 ℃, and simultaneously, most of the gaseous metal chlorides in the smoke are changed into solid. In the flue gas at the outlet of the chlorination furnace, solid particles carried along with the airflow and gaseous titanium tetrachloride enter a cyclone dust collector for gas-solid separation, so that solid metal chlorides and incompletely reacted titanium-rich materials and petroleum coke are discharged from the bottom of the cyclone dust collector and enter a slag treatment system, and gaseous titanium tetrachloride is discharged from the top of the cyclone separator and enters a subsequent condensation and refining system.
In actual production, about 5-10 wt% of titanium-rich material and petroleum coke in the total amount of raw materials are blown out of the chlorination furnace without reaction, and the industry hopes to save cost by recycling. However, the existence of solid metal chloride can prevent the direct recovery of titanium-rich materials and petroleum coke, and the indirect recovery has the problems of long process, high cost and great environmental pollution.
In the prior art, the following two methods are used for treating slag: firstly, pulping by adding water to dissolve metal chloride, then separating unreacted titanium-rich material and petroleum coke by filter pressing, and then washing, filter pressing and drying the materials to be used for other purposes; secondly, adding water and pulping to dissolve the metal chloride, then adding lime milk to change the metal chloride into hydroxide precipitate, and then performing filter pressing, washing and drying to form a filter cake containing the titanium-rich material, the petroleum coke and the hydroxide. Both the two methods can generate a large amount of filter cakes and waste water, the filter cakes are difficult to recycle, and the environmental protection pressure and the energy consumption for waste water treatment are high.
Disclosure of Invention
The invention aims to provide a titanium tetrachloride production system, which can ensure that metal chloride and unreacted titanium-rich material and petroleum coke are effectively separated when being applied to produce titanium tetrachloride.
A production system of titanium tetrachloride comprises a chlorination furnace and a cyclone separator, wherein the bottom and the top of the chlorination furnace are respectively provided with an air inlet and a material outlet, and a furnace body of the chlorination furnace is provided with a material inlet; the bottom and the top of the cyclone separator are respectively provided with a slag discharge port and an exhaust port, and a feed inlet is arranged on the body of the cyclone separator; the discharge port of the chlorination furnace is communicated with the feed port of the cyclone separator through a pipeline; the outer walls and the linings of the cyclone separator and the pipeline are respectively composed of a carbon steel layer and a fire-resistant layer.
The preferable scheme of the invention is that the carbon steel layer is made of carbon steel material, and the thickness of the carbon steel layer is 10-30 mm.
The preferable scheme of the invention is that the material of the fire-resistant layer is a wear-resistant and high-temperature-resistant material, and the refractoriness of the wear-resistant and high-temperature-resistant material is more than or equal to 1400 ℃.
The preferable scheme of the invention is that the wear-resistant and high-temperature-resistant material is a silicon-aluminum refractory material.
The preferable scheme of the invention is that the thickness of the refractory layer is 100-500 mm.
The preferred scheme of the invention is that the chlorination furnace further comprises a one-way electromagnetic valve connected with the slag discharge port, and the one-way electromagnetic valve is communicated with a material inlet of the chlorination furnace.
It is another object of the present invention to provide a method for producing titanium tetrachloride using the system as described above, comprising the steps of:
(a) the method comprises the following steps that a mixed material containing petroleum coke and a titanium-rich material enters a chlorination furnace from the outside through a material inlet and performs chlorination reaction with chlorine entering the chlorination furnace from an air inlet;
(b) discharging the chlorination reaction product from a discharge outlet, and feeding the chlorination reaction product into a cyclone separator through a pipeline for gas-solid separation treatment;
(c) collecting reclaimed materials from a slag discharge port, and collecting titanium tetrachloride at an exhaust port;
in the step (b), the material temperature of the chlorination reaction product at the discharge outlet is 800-1050 ℃.
The preferable scheme of the invention is that the proportion of the petroleum coke, the titanium-rich material and the chlorine gas is (30-40):100: (140) -.
In the preferred scheme of the invention, the chlorination reaction temperature is 800-1050 ℃.
The preferable scheme of the invention is that the reclaimed material comprises a titanium-rich material, petroleum coke and a metal chloride, wherein the content of the metal chloride is less than or equal to 0.5 wt%.
The main chemical reaction formula involved in the chlorination furnace is as follows:
3/2Ti02(s)+2C(s)+3CI2(g)＝3/2TiCI4(g)+C0(g)+C02(g)
3Ca0(s)+2C(s)+3CI2(g)＝3CaCI2(g)+C0(g)+C02(g)
3Fe0(s)+2C(s)+3CI2(g)＝3FeCI2(g)+C0(g)+C02(g)
3Mn0(s)+2C(s)+3CI2(g)＝3MnCI2(g)+C0(g)+C02(g)
3Mg0(s)+2C(s)+3CI2(g)＝3MgCI2(g)+C0(g)+C02(g)
Fe203(s)+2C(s)+3CI2(g)＝2FeCI3(g)+C0(g)+C02(g)
Al203(s)+2C(s)+3CI2(g)＝2AlCI3(g)+C0(g)+C02(g)
V205(s)+2C(s)+3CI2(g)＝2VOCI3(g)+C0(g)+C02(g)
3/2Si02(s)+2C(s)+3CI2(g)＝3/2SiCI4(g)+C0(g)+C02(g)
the physical characteristics of the metal chloride formed after the chlorination reaction are as follows:
compared with the prior art, the invention has the beneficial effects that:
the invention provides a system and a method suitable for producing titanium tetrachloride, wherein at the temperature of 1050 ℃ below 800-. The structural design of the refractory layers of the inner walls of the pipeline and the cyclone separator can offset the release of thermal stress, and the long-term stable operation of the system is ensured.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment of the present invention;
fig. 2 is a schematic view of the structure of the walls or walls of the cyclone separator 20 and the duct 30 of fig. 1.
Detailed Description
The present invention will be further described with reference to the following examples.
EXAMPLE 1 titanium tetrachloride production System and Process
A production system of titanium tetrachloride comprises a chlorination furnace 10, a cyclone separator 20, a pipeline 30 and a one-way electromagnetic valve 40.
The bottom and the top of the chlorination furnace 10 are respectively provided with an air inlet 11 and a discharge outlet 12, and the furnace body of the chlorination furnace 10 is provided with a material inlet 13.
The bottom and the top of the cyclone separator 20 are respectively provided with a slag discharge port 21 and an exhaust port 22, and the body of the cyclone separator 20 is provided with a feed inlet 23.
The discharge port 12 of the chlorination furnace 10 is communicated with the feed port 23 of the cyclone separator 20 through a pipeline 30; the outer walls and the inner linings of the cyclone separator 20 and the pipeline 30 are respectively composed of a carbon steel layer 01 and a fire-resistant layer 02, one end of the one-way electromagnetic valve 40 is communicated with the slag discharge port 21 through a pipeline, and the other end of the one-way electromagnetic valve 40 is communicated with the material inlet 13 of the chlorination furnace 10 through a pipeline.
The carbon steel layer 01 is made of carbon steel materials, and the thickness of the carbon steel layer 01 is 24 mm. The fire-resistant layer 02 is made of a silicon-aluminum fire-resistant material which can be obtained commercially, and the fire resistance of the silicon-aluminum fire-resistant material is more than or equal to 1400 ℃; the thickness of the refractory layer 02 is 300 mm.
The top of the chlorination furnace 10 is also provided with a temperature sensor for detecting the temperature of the flue gas at the discharge outlet 12.
The method for producing titanium tetrachloride by using the system comprises the following steps:
(a) after petroleum coke and the titanium-rich material are mixed in proportion, the obtained mixed material enters a chlorination furnace 10 from the outside through a material inlet 13, and chlorine enters the chlorination furnace 10 from an air inlet 11 and contacts and reacts with the mixed material at the temperature of 850-;
(b) discharging chlorination reaction products from a discharge port 12, and enabling the chlorination reaction products to enter a cyclone separator 20 through a pipeline 30 for gas-solid separation treatment, wherein the temperature of materials at the discharge port 12 is controlled to be 800 ℃ by adjusting the adding amount of petroleum coke and the supplementing amount of oxygen in a chlorination furnace 10;
(c) collecting reclaimed materials from a slag discharge port 21 and collecting titanium tetrachloride at an exhaust port 22;
the petroleum coke: a titanium-rich material: chlorine 35:100: 145.
EXAMPLE 2 titanium tetrachloride production System and Process
The same technical solution as in example 1 was adopted, except that: in the step (b), the material temperature at the discharge port 12 is adjusted to be 830 ℃ by adjusting the adding amount of the petroleum coke and the supplementing amount of the oxygen in the chlorination furnace 10.
EXAMPLE 3 titanium tetrachloride production System and Process
The same technical solution as in example 1 was adopted, except that: in the step (b), the material temperature at the discharge port 12 is controlled to be 850 ℃ by adjusting the adding amount of the petroleum coke and the supplementing amount of the oxygen in the chlorination furnace 10.
EXAMPLE 4 titanium tetrachloride production System and Process
The same technical solution as in example 1 was adopted, except that: in the step (b), the material temperature at the discharge port 12 is adjusted to 890 ℃ by adjusting the adding amount of the petroleum coke and the supplementing amount of the oxygen in the chlorination furnace 10.
EXAMPLE 5 titanium tetrachloride production System and Process
The same technical solution as in example 1 was adopted, except that: in the step (b), the material temperature at the discharge port 12 is controlled to be 920 ℃ by adjusting the adding amount of the petroleum coke and the supplementing amount of the oxygen in the chlorination furnace 10.
EXAMPLE 6 titanium tetrachloride production System and Process
The same technical solution as in example 1 was adopted, except that: in the step (b), the material temperature at the discharge port 12 is controlled to be 960 ℃ by adjusting the adding amount of the petroleum coke and the supplementing amount of the oxygen in the chlorination furnace 10.
Example 7 titanium tetrachloride production System and Process
The same technical solution as in example 1 was adopted, except that: in the step (b), the material temperature at the discharge port 12 is 990 ℃ by adjusting the adding amount of the petroleum coke and the supplementing amount of the oxygen in the chlorination furnace 10.
EXAMPLE 8 titanium tetrachloride production System and Process
The same technical solution as in example 1 was adopted, except that: in the step (b), the material temperature at the discharge port 12 is 1050 ℃ by adjusting the adding amount of the petroleum coke and the supplementing amount of the oxygen in the chlorination furnace 10.
The recycled materials collected in examples 1 to 8 were tested for metal chloride content in sequence and the equipment after each run was checked, and the results are shown in table 1 below.
TABLE 1
Claims (10)
1. A titanium tetrachloride production system comprising a chlorination furnace (10) and a cyclone (20), characterized in that: the bottom and the top of the chlorination furnace (10) are respectively provided with an air inlet (11) and a discharge outlet (12), and the furnace body of the chlorination furnace (10) is provided with a material inlet (13); the bottom and the top of the cyclone separator (20) are respectively provided with a slag discharge port (21) and an exhaust port (22), and the body of the cyclone separator (20) is provided with a feed inlet (23); a discharge port (12) of the chlorination furnace (10) is communicated with a feed port (23) of the cyclone separator (20) through a pipeline (30); the outer wall and the inner lining of the cyclone separator (20) and the pipeline (30) are respectively composed of a carbon steel layer (01) and a fire-resistant layer (02).
2. The titanium tetrachloride production system according to claim 1, wherein: the carbon steel layer (01) is made of carbon steel materials, and the thickness of the carbon steel layer (01) is 10-30 mm.
3. The titanium tetrachloride production system according to claim 1, wherein: the fire-resistant layer (02) is made of a wear-resistant and high-temperature-resistant material, and the fire resistance of the wear-resistant and high-temperature-resistant material is more than or equal to 1400 ℃.
4. The titanium tetrachloride production system according to claim 3, wherein: the wear-resistant high-temperature-resistant material is a silicon-aluminum refractory material.
5. The titanium tetrachloride production system according to claim 3, wherein: the thickness of the refractory layer (02) is 100-500 mm.
6. The titanium tetrachloride production system according to claim 1, wherein: the device also comprises a one-way electromagnetic valve (40) connected with the slag discharge port (21), and the one-way electromagnetic valve (40) is communicated with the material inlet (13) of the chlorination furnace (10).
7. A method for producing titanium tetrachloride using the system of any one of claims 1 to 6, comprising the steps of:
(a) the method comprises the following steps that a mixed material containing petroleum coke and a titanium-rich material enters a chlorination furnace (10) from the outside through a material inlet (13) and performs chlorination reaction with chlorine entering the chlorination furnace (10) from an air inlet (11);
(b) the chlorination reaction product is discharged from a discharge port (12) and enters a cyclone separator (20) through a pipeline (30) for gas-solid separation treatment;
(c) collecting reclaimed materials from a slag discharge port (21) and collecting titanium tetrachloride at an exhaust port (22);
in the step (b), the material temperature of the chlorination reaction product at the discharge opening (12) is 800-.
8. The process for producing titanium tetrachloride according to claim 7, wherein: the proportion of the petroleum coke, the titanium-rich material and the chlorine gas is (30-40):100: (140-.
9. The process for producing titanium tetrachloride according to claim 7, wherein: the chlorination reaction temperature is 800-1050 ℃.
10. The process for producing titanium tetrachloride according to claim 7, wherein: the reclaimed materials comprise a titanium-rich material, petroleum coke and a metal chloride, wherein the content of the metal chloride is less than or equal to 0.5 wt%.
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Cited By (3)
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| CN110357149A (en) * | 2019-07-17 | 2019-10-22 | 洛阳双瑞万基钛业有限公司 | A kind of raising TiCl4The method and device of deslagging efficiency in production process |
| CN113184900A (en) * | 2021-05-12 | 2021-07-30 | 攀钢集团钒钛资源股份有限公司 | Titanium tetrachloride production method and system and raw material ratio adjusting method |
| CN113277553A (en) * | 2021-06-29 | 2021-08-20 | 蚌埠中瓷纳米科技有限公司 | Two-stage dust removal device and method for preparing titanium tetrachloride |
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