CN106943966B - Experimental reaction system for preparing titanium dioxide by titanium tetrachloride gas phase oxidation - Google Patents
Experimental reaction system for preparing titanium dioxide by titanium tetrachloride gas phase oxidation Download PDFInfo
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Abstract
The invention relates to an experimental reaction system for preparing titanium dioxide by titanium tetrachloride vapor phase oxidation. The method comprises a reactor, an oxygen feeding device, a titanium tetrachloride feeding device, a tail gas treatment device and a tail gas detection device, wherein raw material preheating and raw material reaction are integrated together and are realized in the reactor. The invention can realize the collection of key parameters of the laboratory-grade titanium tetrachloride vapor phase oxidation reaction and provide technical support for industrial production.
Description
Technical Field
The invention relates to an experimental reaction system for preparing titanium dioxide by vapor phase oxidation of titanium tetrachloride, belonging to the technical field of chlorination process titanium dioxide industry.
Background
Titanium dioxide is prepared by oxidizing titanium tetrachloride in a gas phase, which is an advanced titanium dioxide manufacturing process commonly known as a chlorination-process titanium dioxide production process, and the process has the advantages of good product quality, environmental friendliness and the like, so that the process is widely adopted by developed countries, but due to technical blockade, the application of the process in China is to be developed, and one of the reasons for restricting the development is the loss of key process parameters. The laboratory-level experiment can obtain key parameters at a lower cost, but the requirements on the experiment are harsh due to the complex conditions of the titanium tetrachloride vapor phase oxidation experiment, and the existing equipment can not meet the experimental requirements, so that the experiment is restricted.
The chemical reaction formula for preparing titanium white by titanium tetrachloride gas phase oxidation is as follows:
TiCl4(g)+O2(g)＝TiO2(R)+2Cl2(g)；△H＝-181.5856kJ/mol。
the reaction can not be carried out basically at normal temperature, and the reaction speed is obviously increased only when the temperature is higher than 600 ℃, and the reaction speed is increased along with the increase of the temperature. The reaction is exothermic, and the heat of reaction released alone is only about two thirds of the heat balance of the process, so the raw material (Ti) must be used firstCl4,O2) Preheating to keep the reaction continuously. Factors influencing the quality of titanium white products produced by the chlorination process are complex, such as: reaction temperature, additive influence, material ratio, etc.
In the current industrial production, titanium tetrachloride is preheated and an additive is fed into a reactor in a gaseous form, and oxygen preheated by a toluene flame is subjected to a meeting reaction in an environment of 1600 ℃, and the pressure in the reactor is maintained at 3 atmospheres. Due to the high reaction temperature and pressure, the process has very high requirements on production equipment, and the strict conditions are difficult to realize in a laboratory.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the experimental reaction system for preparing titanium dioxide by titanium tetrachloride vapor phase oxidation is provided, so that the collection of key parameters of laboratory-grade titanium tetrachloride vapor phase oxidation reaction can be conveniently realized, and technical support is provided for industrial production.
In order to solve the technical problems, the invention adopts the technical scheme that: an experimental reaction system for preparing titanium dioxide by titanium tetrachloride vapor phase oxidation comprises a reactor, wherein the reactor comprises an outer tube, an inner tube, a feeding tube, a heating device and an electric furnace control cabinet; the front end of the outer tube is hermetically connected through a titanium tetrachloride feeding head, the tail end of the outer tube is hermetically connected through a plug, and an oxygen inlet is formed in the side wall of the tail end of the outer tube; the front end of the inner pipe penetrates through the plug and then is sleeved in the outer pipe, a space is reserved between the outer wall of the inner pipe and the inner wall of the outer pipe, and the tail end of the inner pipe is provided with a tail gas outlet and a sampling port; the feeding pipe penetrates through the titanium tetrachloride feeding head and then extends into the inner pipe, and a space is formed between the outer wall of the feeding pipe and the inner wall of the inner pipe; the heating device is sleeved on the outer wall of the outer pipe and is electrically connected with the electric furnace control cabinet.
Further, the method comprises the following steps: the oxygen inlet is connected with an oxygen feeding device, and the oxygen feeding device comprises an oxygen bottle, a three-way joint and an inert gas A bottle; the outlet end of the oxygen cylinder is connected with an oxygen pressure reducing valve and an oxygen rotameter in sequence and then connected with a first connector of the three-way joint; the outlet end of the inert gas A bottle is connected with a second pressure reducing valve and a second rotameter in sequence and then connected with a second connector of the three-way joint; the third interface of the three-way joint is connected with the oxygen inlet.
Further, the method comprises the following steps: the inlet end of the charging pipe is connected with a titanium tetrachloride feeding device, and the titanium tetrachloride feeding device comprises an inert gas B bottle, a three-neck flask and a titanium tetrachloride storage tank; the outlet end of the inert gas B bottle is connected with a third pressure reducing valve and a third rotameter in sequence and then connected with a first connector of the three-neck flask; the outlet end of the titanium tetrachloride storage tank is connected to a second interface of the three-neck flask through a metering pump; the third interface of three-neck flask is connected in the entry end of filling tube, and three-neck flask cover is equipped with the heating jacket.
Further, the method comprises the following steps: a tail gas outlet at the tail end of the inner pipe is connected with a tail gas treatment device, and the tail gas treatment device comprises a leaching tower, a leaching tower head, a leaching box and a leaching pump; the tail gas outlet is communicated with the leaching box, the leaching tower is arranged at the top of the leaching box, the head of the leaching tower is arranged at the top of the leaching tower, the inlet end of the leaching pump is connected to the bottom of the leaching box, and the outlet end of the leaching pump is connected with the head of the leaching tower; and a tail gas discharge port is arranged at the top of the leaching tower.
Further, the method comprises the following steps: the sampling port at the end of the inner pipe is connected with a tail gas detection device, the tail gas detection device comprises a sampling pipe, a gas washing bottle, a gas collecting bottle and a vacuum pump, the sampling pipe stretches into the inner pipe through the sampling port, the sampling pipe is arranged along the axis direction of the inner pipe, and the outlet end of the sampling pipe is sequentially connected with the gas washing bottle, the gas collecting bottle and the vacuum pump.
Further, the method comprises the following steps: the number of the gas washing bottles is at least two.
Further, the method comprises the following steps: the sampling tube is detachable connection structure, so that the length of the sampling tube extending into the inner tube can be adjusted.
Further, the method comprises the following steps: the heating device comprises a plurality of heating zones which are sequentially arranged along the length direction of the outer tube, each heating zone is independently provided with a heating program through an electric furnace control cabinet, and each heating zone is provided with a temperature measuring device.
Further, the method comprises the following steps: the number of the heating zones is two or three.
Further, the method comprises the following steps: the filling tube is detachable connection structure, so that the length of the filling tube extending into the inner tube can be adjusted.
The invention has the beneficial effects that: in the implementation, the reactor is heated by a heating device, and oxygen is introduced into an oxygen inletIntroducing titanium tetrachloride gas into the feeding pipe; oxygen enters from the tail end of the outer pipe and then flows into an inlet of the inner pipe positioned at the front end of the outer pipe until the introduced titanium tetrachloride gas is contacted in the inner pipe, and the preheating of the oxygen can be completed in the process; the titanium tetrachloride gas passes through the feeding pipe until the inner pipe is contacted with the introduced oxygen, and the preheating of the titanium tetrachloride gas can be completed in the process; the preheated oxygen and titanium tetrachloride gas contact in the inner tube and then react, and the TiO obtained after the reaction is tested2Can be collected in the inner wall of the inner pipe and the tail gas treatment device, and the TiO is2Can be used as an experimental sample to detect the performance; the data obtained from the tail gas detection can be used to calculate the reaction rate. The invention can conveniently realize the collection of key parameters of the laboratory-grade titanium tetrachloride gas-phase oxidation reaction and provide technical support for industrial production.
Drawings
FIG. 1 is a schematic structural view of the present invention;
parts, positions and numbers in the drawings: 1-oxygen bottle, 2-oxygen pressure reducing valve, 3-oxygen rotameter, 4-three-way joint, 5-inert gas A bottle, 6-inert gas B bottle, 7-second pressure reducing valve, 8-second rotameter, 9-third pressure reducing valve, 10-third rotameter, 11-three-neck flask, 12-heating jacket, 13-metering pump, 14-titanium tetrachloride storage tank, 15-electric furnace control cabinet, 16-temperature zone I, 17-temperature zone II, 18-temperature zone III, 19-titanium tetrachloride feeding head, 20-outer tube, 21-oxygen inlet, 22-inner tube, 23-sampling tube, 24-leaching tower, 25-leaching tower head, 26-leaching box, 27-leaching pump, 28-tail gas discharge port, 29-gas washing bottle, 30-gas collecting bottle, 31-vacuum pump, 32-charging tube and 33-plug.
Detailed Description
The invention is further explained below with reference to the drawings and examples.
As shown in figure 1, the experimental reaction system for preparing titanium dioxide by vapor phase oxidation of titanium tetrachloride comprises a reactor, wherein the reactor comprises an outer tube 20, an inner tube 22, a feeding tube 32, a heating device and an electric furnace control cabinet 15; the front end of the outer tube 20 is hermetically connected through a titanium tetrachloride feeding head 19, the tail end of the outer tube is hermetically connected through a plug 33, and an oxygen inlet 21 is formed in the side wall of the tail end of the outer tube 20; the front end of the inner tube 22 penetrates through the plug 33 and then is sleeved in the outer tube 20, a space is reserved between the outer wall of the inner tube 22 and the inner wall of the outer tube 20, and the tail end of the inner tube 22 is provided with a tail gas outlet and a sampling port; the feeding pipe 32 passes through the titanium tetrachloride feeding head 19 and extends into the inner pipe 22, and a space is reserved between the outer wall of the feeding pipe 32 and the inner wall of the inner pipe 20; the heating device is sleeved on the outer wall of the outer tube 20 and is electrically connected with the electric furnace control cabinet 15. Wherein, the filling tube 32 is a detachable connection structure, so that the length of the filling tube 32 extending into the inner tube 22 can be adjusted to change the reaction conditions and obtain different experimental data.
In practice, the reactor is heated by a heating device, oxygen is introduced into the oxygen inlet 21, and titanium tetrachloride gas is introduced into the feeding pipe 32; oxygen enters from the end of the outer tube 20 and flows into an inlet of the inner tube 22 at the front end of the outer tube 20 until the inner tube 22 contacts with the introduced titanium tetrachloride gas, and the preheating of the oxygen can be completed in the process; preheating of the titanium tetrachloride gas can be accomplished by passing the titanium tetrachloride gas through the feed tube 32 until the interior tube 22 is contacted with the introduced oxygen; the preheated oxygen and titanium tetrachloride gas are contacted in the inner tube 22 and then react, and the TiO obtained after the reaction is tested2Can be collected on the inner wall of the inner tube 22 and in the exhaust gas treatment device, and the TiO is2Can be used as an experimental sample to detect the performance; the data obtained from the tail gas detection can be used to calculate the reaction rate. The invention can conveniently realize the collection of key parameters of the laboratory-grade titanium tetrachloride gas-phase oxidation reaction and provide technical support for industrial production.
In the invention, the heating device can realize program control heating through the electric furnace control cabinet 15, and the maximum heating temperature is 1200 ℃. The heating device comprises a plurality of heating zones which are sequentially arranged along the length direction of the outer tube 20, each heating zone is independently provided with a heating program through the electric furnace control cabinet 15, and each heating zone is provided with a temperature measuring device. By providing multiple heating zones, more heating temperature test data can be measured. The number of heating zones is usually two or three, preferably three in this embodiment, including zone one 16, zone two 17, and zone three 18. The outer tube 20, the inner tube 22 and the feeding tube 32 are preferably made of quartz glass, and can completely meet the experimental temperature conditions.
The oxygen inlet 21 is connected with an oxygen feeding device, and the preferred embodiment is as follows: the oxygen feeding device comprises an oxygen bottle 1, a three-way joint 4 and an inert gas A bottle 5; the outlet end of the oxygen bottle 1 is connected with an oxygen pressure reducing valve 2 and an oxygen rotameter 3 in sequence and then connected with a first connector of a three-way joint 4; the outlet end of the inert gas A bottle 5 is connected with a second reducing valve 7 and a second rotameter 8 in sequence and then connected with a second connector of the three-way joint 4; the third port of the three-way joint 4 is connected to the oxygen inlet 21. The oxygen feeding device can realize the adjustment of oxygen flow and oxygen concentration and carry out experiments with different parameters. The inert gas A bottle 5 is preferably a nitrogen bottle.
The inlet end of the feeding tube 32 is connected with a titanium tetrachloride feeding device, and the preferred embodiment is as follows: the titanium tetrachloride feeding device comprises an inert gas B bottle 6, a three-neck flask 11 and a titanium tetrachloride storage tank 14; the outlet end of the inert gas B bottle 6 is connected with a third reducing valve 9 and a third rotameter 10 in sequence and then connected with a first connector of a three-neck flask 11; the outlet end of the titanium tetrachloride storage tank 14 is connected to a second interface of the three-neck flask 11 through a metering pump 13; the third interface of the three-neck flask 11 is connected to the inlet end of the feeding pipe 32, and the three-neck flask 11 is sleeved with a heating jacket 12. Wherein, the inert gas B bottle 6 can adopt a nitrogen bottle, and nitrogen is used as driving gas; a measured amount of liquid titanium tetrachloride was heated to a gas in a three-necked flask 11 by a heating mantle 12. Titanium tetrachloride is a liquid at ambient temperature and produces white fumes when exposed to air, and when the temperature rises above 137 ℃, it exists in gaseous form, a difficulty with laboratory scale oxidation reactors is the addition of titanium tetrachloride. By adopting the titanium tetrachloride feeding device, quantitative liquid titanium tetrachloride liquid can be transferred into a gaseous state at the first time and enter the reaction system, and the problem can be effectively solved.
The tail gas outlet at the end of the inner pipe 22 is connected with a tail gas treatment device, and the preferred embodiment thereof is as follows: the tail gas treatment device comprises a leaching tower 24, a leaching tower head 25, a leaching box 26 and a leaching pump 27; the tail gas outlet is communicated with a leaching box 26, a leaching tower 24 is arranged at the top of the leaching box 26, and a leaching tower head 25 is arranged on the leaching tower 24, the inlet end of a leaching pump 27 is connected to the bottom of a leaching box 26, and the outlet end is connected with a leaching tower head 25; the top of the leaching tower 24 is provided with a tail gas discharge port 28. The invention adopts a method of leaching with alkali liquor to treat the tail gas, can absorb harmful substances in the tail gas and collect TiO in the product2. In this embodiment, the leaching tower 24 is a glass tube with a diameter of 50mm and a length of 1m, and the leaching box 26 is a stainless steel box with a diameter of 300mm × 300mm × 300 mm.
The sampling port at the end of the inner tube 22 is connected with an exhaust gas detection device, and the preferred embodiment thereof is as follows: the tail gas detection device comprises a sampling pipe 23, a gas washing bottle 29, a gas collecting bottle 30 and a vacuum pump 31, wherein the sampling pipe 23 extends into the inner pipe 22 through a sampling opening, the sampling pipe 23 is arranged along the axial direction of the inner pipe 22, the outlet end of the sampling pipe 23 is sequentially connected with the gas washing bottle 29, the gas collecting bottle 30 and the vacuum pump 31, and the number of the gas washing bottles 29 is at least two. The inert gas A bottle 5 and the inert gas B bottle 6 both adopt nitrogen bottles, and the tail gas mainly contains N2，O2，TiO2，TiCl4，Cl2In which only TiCl is present4Containing Cl-Can become an interference term, Cl, in the detection process2Is insoluble in saturated saline solution, but the saturated saline solution can absorb TiCl4And most of TiO in the tail gas can be filtered2. In the invention, a two-stage gas washing bottle 29 for containing saturated salt water is adopted for filtering, negative pressure is generated by a vacuum pump 31, tail gas is pumped and filtered into a gas collecting bottle 30, and Cl in the tail gas is filtered2The reaction rate can be obtained by detecting the content. The sampling tube 23 is a detachable connection structure, so that the length of the sampling tube 23 extending into the inner tube 22 can be adjusted to detect samples in different reaction areas. The sampling port at the end of the inner tube 22 and the tail gas outlet can be arranged on the end face of the inner tube 22, and at the moment, the sampling tube 23 enters the middle part of the reaction zone through a flange in the middle part of the leaching box 26.
The implementation steps of the invention are as follows:
1) connecting equipment; in the embodiment, the diameter of the outer tube 20 is 50mm, the diameter of the inner tube 22 is 35mm, and the diameter of the oxygen inlet 21 is 8 mm; the inert gas bottle A5 and the inert gas bottle B6 both adopt nitrogen bottles;
2) the heating device is provided with three sections of heating zones, each section is 30cm long, the temperature of the first temperature zone 16 and the second temperature zone 17 is set to be 950 ℃, and heat preservation is carried out;
3) adjusting the oxygen flow to 0.8m3H, mixed nitrogen gas flow is 0.2m3And/h, the two are merged into an oxygen inlet 21 at the tail end of the reactor through a three-way valve 4.
4) Weighing 200g TiCl4Placing in a titanium tetrachloride storage tank 14 with a capacity of 500ml, adjusting the temperature of a three-neck flask 11 to 150 ℃, starting to drive nitrogen, and driving the nitrogen flow to be 0.2m3Regulating the flow of the metering pump 13 to be 30 g/min;
5) starting a tail gas treatment device and a tail gas detection device;
6) the flow and temperature at each position were recorded.
TiO obtained by experiment2Can be collected in the inner wall of the reactor and the tail gas leacheate2Can be used as an experimental sample to detect the performance; the data obtained from the tail gas detection can be used to calculate the reaction rate.
Claims (7)
1. An experimental reaction system for preparing titanium dioxide by titanium tetrachloride vapor phase oxidation comprises a reactor and is characterized in that: the reactor comprises an outer tube (20), an inner tube (22), a feeding tube (32), a heating device and an electric furnace control cabinet (15); the front end of the outer tube (20) is hermetically connected through a titanium tetrachloride feeding head (19), the tail end of the outer tube is hermetically connected through a plug (33), and an oxygen inlet (21) is formed in the side wall of the tail end of the outer tube (20); the front end of the inner pipe (22) penetrates through the plug (33) and then is sleeved in the outer pipe (20), a space is reserved between the outer wall of the inner pipe (22) and the inner wall of the outer pipe (20), and the tail end of the inner pipe (22) is provided with a tail gas outlet and a sampling port; the feeding pipe (32) penetrates through the titanium tetrachloride feeding head (19) and then extends into the inner pipe (22), and a space is reserved between the outer wall of the feeding pipe (32) and the inner wall of the inner pipe (22); the heating device is sleeved on the outer wall of the outer pipe (20) and is electrically connected with the electric furnace control cabinet (15);
a tail gas outlet at the tail end of the inner pipe (22) is connected with a tail gas treatment device, and the tail gas treatment device comprises a leaching tower (24), a leaching tower head (25), a leaching box (26) and a leaching pump (27); the tail gas outlet is connected into the leaching box (26), the leaching tower (24) is arranged at the top of the leaching box (26), the leaching tower head (25) is arranged at the top of the leaching tower (24), the inlet end of the leaching pump (27) is connected to the bottom of the leaching box (26), and the outlet end of the leaching pump is connected with the leaching tower head (25); the top of the leaching tower (24) is provided with a tail gas discharge port (28);
a sampling port at the tail end of the inner pipe (22) is connected with a tail gas detection device, the tail gas detection device comprises a sampling pipe (23), a gas washing bottle (29), a gas collecting bottle (30) and a vacuum pump (31), the sampling pipe (23) extends into the inner pipe (22) through the sampling port, the sampling pipe (23) is arranged along the axial direction of the inner pipe (22), and the outlet end of the sampling pipe (23) is sequentially connected with the gas washing bottle (29), the gas collecting bottle (30) and the vacuum pump (31); the gas washing bottle (29) is used for containing saturated salt water;
the sampling tube (23) is a detachable connecting structure, so that the length of the sampling tube (23) extending into the inner tube (22) can be adjusted.
2. The experimental reaction system for the vapor phase oxidation of titanium tetrachloride to titanium dioxide according to claim 1, wherein: the oxygen inlet (21) is connected with an oxygen feeding device, and the oxygen feeding device comprises an oxygen bottle (1), a three-way joint (4) and an inert gas A bottle (5); the outlet end of the oxygen bottle (1) is connected with an oxygen pressure reducing valve (2) and an oxygen rotameter (3) in sequence and then is connected with a first connector of a three-way joint (4); the outlet end of the inert gas A bottle (5) is connected with a second reducing valve (7) and a second rotameter (8) in sequence and then is connected with a second connector of the three-way joint (4); the third interface of the three-way joint (4) is connected with the oxygen inlet (21).
3. The experimental reaction system for the vapor phase oxidation of titanium tetrachloride to titanium dioxide according to claim 1, wherein: the inlet end of the feeding pipe (32) is connected with a titanium tetrachloride feeding device, and the titanium tetrachloride feeding device comprises an inert gas B bottle (6), a three-neck flask (11) and a titanium tetrachloride storage tank (14); the outlet end of the inert gas B bottle (6) is connected with a third reducing valve (9) and a third rotameter (10) in sequence and then is connected with a first connector of a three-neck flask (11); the outlet end of the titanium tetrachloride storage tank (14) is connected to a second interface of the three-neck flask (11) through a metering pump (13); the third interface of the three-mouth flask (11) is connected with the inlet end of the feeding pipe (32), and the three-mouth flask (11) is sleeved with a heating sleeve (12).
4. The experimental reaction system for the vapor phase oxidation of titanium tetrachloride to titanium dioxide according to claim 1, wherein: at least two gas washing bottles (29) are provided.
5. The experimental reaction system for preparing titanium dioxide by vapor phase oxidation of titanium tetrachloride according to any one of claims 1 to 4, wherein: the heating device comprises a plurality of heating zones which are sequentially arranged along the length direction of the outer tube, each heating zone is independently provided with a heating program through an electric furnace control cabinet (15), and each heating zone is provided with a temperature measuring device.
6. The experimental reaction system for the vapor phase oxidation of titanium tetrachloride to titanium dioxide according to claim 5, wherein: the number of the heating zones is two or three.
7. The experimental reaction system for preparing titanium dioxide by vapor phase oxidation of titanium tetrachloride according to any one of claims 1 to 4, wherein: the feed pipe (32) is of a detachable connection structure, so that the length of the feed pipe (32) extending into the inner pipe (22) can be adjusted.
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| CN107803169A (en) * | 2017-09-06 | 2018-03-16 | 天津大学 | A kind of fuel reforming system |
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| CN109019681A (en) * | 2018-08-23 | 2018-12-18 | 攀钢集团攀枝花钢铁研究院有限公司 | The titanium white chloride process units and production method of additive pre-atomized |
| CN114029025A (en) * | 2021-11-15 | 2022-02-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Titanium dioxide oxidation reaction device by chlorination process |
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