CN111003727B - Rapid preparation of lambda-Ti3O5Powder device and method - Google Patents
Rapid preparation of lambda-Ti3O5Powder device and method Download PDFInfo
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- CN111003727B CN111003727B CN202010024394.XA CN202010024394A CN111003727B CN 111003727 B CN111003727 B CN 111003727B CN 202010024394 A CN202010024394 A CN 202010024394A CN 111003727 B CN111003727 B CN 111003727B
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- C01G23/043—Titanium sub-oxides
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses a method for quickly preparing lambda-Ti3O5The device comprises a hydrogen storage tank, a material tank, a vibrator, a linear motor, a reaction furnace, a gas-solid separator, a material collecting tank and a tail gas purification device; commercial P25 or pigment-grade titanium dioxide is used as a raw material, hydrogen is used as carrier gas and reducing gas, the gas flow and the reaction temperature are controlled, and lambda-Ti is obtained in a material collecting region after the reaction is finished3O5Powder; the method can rapidly prepare the lambda-Ti3O5Powder with micron-sized particle diameter and Ti3O5Phase stabilization, realizing lambda-Ti3O5And (3) rapidly preparing the powder.
Description
Technical Field
The invention provides a method for quickly preparing lambda-Ti3O5A device and a method for powder belong to the field of powder material preparation.
Background
Since the 70 s of the 20 th century, solar technology has gained rapid development due to its attractive application prospects. The inexhaustible too much energy is utilized to solve the problem of energy shortage, and the pollution-free degradable environmental-friendly energy-saving system has no pollution and is a perfect choice for human beings.
In the application of energy environment, the titanium content in the earth crust is high, the synthesis process of the main oxide is various, and the titanium oxide has stable physicochemical properties, moderate band gap, good oxygen sensitivity, optical storage and photocatalytic performance, low price and easy obtainment, thereby becoming the research hotspot of the current titanium nano semiconductor material. Among the titanium oxide nanomaterials, Ti3O5Is a relatively stable titanium suboxide, often colloquially referred to as titanium black along with other titanium suboxides, and is often used as an industrial pigment. Due to Ti3O5Has better conductivity and acid and alkali corrosion resistance, and can replace noble metal to be used as an electrode material. In addition, Ti3O5Is also an ideal evaporation material for the oxidation evaporation plating of TiO2The solid phase component of the membrane is stable and unchanged when the membrane is used as a raw material. Ti3O5The oxygen-sensitive material is a non-stoichiometric compound, wherein the atomic ratio of O to Ti is between 1.66 and 1.70, a large number of oxygen vacancies are contained in the oxygen-sensitive material, the oxygen-sensitive material has higher quasi-free electron concentration, and the resistance is changed along with the change of atmosphere, so that the oxygen-sensitive material becomes a potential oxygen-sensitive material.
Ti3O5Has a plurality of crystal forms, and different crystal forms have different properties. Since the study, Ti was separately added3O5Are designated as alpha, beta, gamma, delta, lambda, etc., where lambda-Ti3O5Ti discovered only in 20103O5And (4) phase(s). At room temperature, when irradiating λ -Ti with laser having a wavelength of 532nm3O5A λ to β transition occurs, which is reversed when the β phase is irradiated with a laser having a wavelength of 410nm, and both structures are stable at room temperature. Because the two phase structures have different conductivity, reflectivity, permeability and the like, the functional requirements of a data storage switch are met, and the high-density storage of the optical disk can be realized by controlling the particle size, the grain size and the laser irradiation parameters of the material. In addition, the current readable and writable blue-ray disc and DVD disc materials are mainly rare metal substances of germanium-antimony-tellurium alloy, such as Ti3O5The cost can be greatly reduced as a storage medium, and the storage medium is safe and environment-friendly. Therefore, the material has good application prospect in the field of optical storage and has potential to become the next generation optical storage material.
CN 105887182A discloses a process for preparing a titanium pentoxide crystal, which comprises mixing titanium powder and titanium dioxide uniformly, granulating, oven drying to obtain a sintered block, and vacuumizing the furnace body to 10 deg.C3~104Pa, a method of heating and sintering by stages is adopted: the normal temperature of the first stage is raised to 1200 ℃; in the second stage, the temperature is increased to 1500 ℃ and inert gas is filled when the temperature reaches 1400 ℃; in the third stage, the temperature is increased to 1750-1850 ℃ from 1500 ℃, the method effectively avoids the generation of a large number of air holes, the purity and the quality of the prepared titanium pentoxide are high, the reaction process time is long, the light heat preservation time reaches 13-30 hours, and the process is complex.
CN 103806099A discloses a method for preparing a trititanium pentoxide crystal, which also adopts a staged sintering method to prepare a flaky trititanium pentoxide crystal, shortens premelting time or saves premelting time, directly evaporates and plates for a short time.
Disclosure of Invention
The invention provides a method for quickly preparing lambda-Ti3O5The device and the method of the powder can obtain the high-purity lambda-Ti in a very short time3O5The powder is very simple in operation process.
Rapid preparation of lambda-Ti3O5The powder device comprises a hydrogen storage tank 1, a material tank 2, a reaction furnace 3, a gas-solid separator 4, a material collecting tank 5, a tail gas purifying device 6, a vibrator 7 and a linear motor 8; the hydrogen storage tank 1 is connected with 2 entry of material jar, and 2 bottoms of material jar are equipped with vibrator 7, and 7 bottoms of vibrator are connected with linear electric motor 8's output, and 2 exports of material jar are connected with 3 one end of reacting furnace, and the 3 other end of reacting furnace is connected with gas-solid separator 4, and 4 bottoms of gas-solid separator are connected with material collecting vessel 5, and 4 tops of gas-solid separator are connected with tail gas cleanup unit 6.
The inside vertical track that is equipped with of material jar 2, material tank cover is last to be fluted, and the recess and vertical track cooperation, material tank cover reciprocate along the inside vertical track of material jar 2.
The length of the high-temperature heating section in the reaction furnace 3 is 0.8-1.2 m.
(1) Repeatedly replacing air in the device with hydrogen to keep hydrogen atmosphere in the device;
(2) drying titanium dioxide powder, then loading the dried titanium dioxide powder into a material tank 2, starting a vibrator 7 and a linear motor 8, driving the material tank 2 and the titanium dioxide powder inside to vibrate by the vibrator 7, and driving the vibrator 7, the material tank 2 and the titanium dioxide powder inside the material tank 2 to move towards a material tank cover by the linear motor 8;
(3) opening a valve of a hydrogen storage tank 1, after hydrogen enters a material tank 2, the hydrogen brings the titanium dioxide powder out of the material tank 2 and enters a reaction furnace 3 to perform high-temperature reaction in the reaction furnace 3 due to vibration of the material tank 2 and the titanium dioxide powder inside;
(4) the reaction product enters a gas-solid separator 4 after coming out from the other end of the reaction furnace 3 along with the gas, and the solid separated by the gas-solid separator is lambda-Ti3O5The powder enters a material collecting tank 5, and the gas enters a tail gas purifying device 6.
The titanium dioxide powder in step (2) may be commercial P25 powder, pigment grade titanium dioxide powder, or the like.
And (3) the running speed of the output end of the linear motor 8 in the step (2) is 5-10 mm/min.
The hydrogen flow rate in the step (3) is 2-4L/min.
In the step (3), the high-temperature reaction of the reaction furnace 3 is carried out by heating to 1450-1550 ℃ at a heating rate of 3-10 ℃/min.
And (4) the tail gas purification device 6 is filled with aqueous solution.
The invention has the beneficial effects that:
(1) the invention can realize Ti3O5The powder is prepared quickly and continuously, the preparation period is extremely short, the operation process is simple, and the industrial operation can be realized;
(2) the powder lambda-Ti prepared by the invention3O5Phase stability, and filling up the preparation of the lambda-Ti by removing the titanium dioxide3O5Blank of powder method.
Drawings
FIG. 1 is a schematic view of the structure of an apparatus according to example 1;
FIG. 2 shows the λ -Ti obtained in example 23O5Powder XRD pattern;
FIG. 3 shows the λ -Ti obtained in example 23O5SEM image of microstructure of the powder;
FIG. 4 is a powder XRD pattern of the powder obtained in comparative example 1;
FIG. 5 is a powder XRD pattern of the powder obtained in comparative example 2;
in the figure, 1-a hydrogen storage tank, 2-a material tank, 3-a reaction furnace, 4-a gas-solid separator, 5-a material collecting tank, 6-a tail gas purifying device, 7-a vibrator and 8-a linear motor.
Detailed Description
The invention is described in more detail below with reference to the figures and examples, but the scope of the invention is not limited to the description.
Example 1
Rapid preparation of lambda-Ti3O5The powder device, as shown in fig. 1, comprises a hydrogen storage tank 1, a material tank 2, a reaction furnace 3, a gas-solid separator 4, a material collecting tank 5, a tail gas purifying device 6, a vibrator 7 and a straight line 8; the hydrogen storage tank 1 is connected with the inlet of the material tank 2, the vibrator 7 is arranged at the bottom of the material tank 2, the linear motor 8 is arranged at the bottom of the vibrator 7, and the outlet of the material tank 2 is connected with the outlet of the material tank 2One end of a reaction furnace 3 is connected, the other end of the reaction furnace 3 is connected with a gas-solid separator 4, the bottom of the gas-solid separator 4 is connected with a material collecting tank 5, the top of the gas-solid separator 4 is connected with a tail gas purifying device 6, a vertical rail is arranged inside a material tank 2, a groove is formed in a material tank cover and matched with the vertical rail, and a material tank cover moves up and down along the vertical rail inside the material tank 2; the length of the high-temperature heating section in the reaction furnace 3 is 0.8-1.2 m.
Example 2
Using the apparatus of example 1, λ -Ti was rapidly prepared3O5The method for preparing the powder comprises the following specific steps:
(1) firstly, repeatedly replacing air in a reaction device with hydrogen for many times to keep hydrogen atmosphere in a furnace device; the length of the high-temperature heating section in the reaction furnace 3 is 0.8 m;
(2) drying commercial P25 powder, then filling the dried powder into a material tank 2, starting a vibrator 7 and a linear motor 8, wherein the vibration frequency of the vibrator 7 is 55Hz, the running speed of the output end of the linear motor 8 is 8mm/min, the vibrator 7 drives the material tank 2 and the titanium dioxide powder inside the material tank to vibrate, and the linear motor 8 drives the vibrator 7, the material tank 2 and the titanium dioxide powder inside the material tank 2 to move towards the direction of a material tank cover, so that the titanium dioxide powder is close to a hydrogen pipe;
(3) opening a valve of a hydrogen storage tank 1, wherein the hydrogen flow is 3L/min, after hydrogen enters a material tank 2, the hydrogen can bring titanium dioxide powder out of the material tank 2 due to vibration of the material tank 2 and the titanium dioxide powder inside, and then the hydrogen enters a reaction furnace, wherein the temperature of the high-temperature reaction of the reaction furnace 3 is increased to 1500 ℃ at the temperature increasing rate of 5 ℃/min, and the material conveying speed is 7 mg/min;
(4) the reaction product enters a gas-solid separator 4 after coming out from the other end of the reaction furnace 3 along with the gas, and the solid separated by the gas-solid separator is lambda-Ti3O5The powder enters a material collecting tank 5, and the gas enters a tail gas purifying device 6 filled with water for purification treatment and then is emptied.
FIG. 2 shows the λ -Ti obtained in example 23O5Comparing the powder XRD pattern with a standard card, the phase is pure Ti3O5Phase, 2 theta characteristic peak appearanceAt 17.89 °, 25.16 °, 26.69 °, 31.17 °, 32.20 °, 48.03 °, etc.
FIG. 3 shows the λ -Ti obtained in example 23O5The SEM image of the microstructure of the powder shows that the sample size is in the order of micron, about 5 μm.
The lattice parameters of the sample are shown in Table 1, and it can be seen from Table 1 that the sample is a lambda type Ti3O5。
TABLE 1
Example 3
Using the apparatus of example 1, λ -Ti was rapidly prepared3O5The method for preparing the powder comprises the following specific steps:
(1) firstly, repeatedly replacing air in a reaction device with hydrogen for many times to keep hydrogen atmosphere in a furnace device; the length of the high-temperature heating section in the reaction furnace 3 is 1.2 meters;
(2) drying commercial P25 powder, then filling the dried powder into a material tank 2, starting a vibrator 7 and a linear motor 8, wherein the vibration frequency of the vibrator 7 is 60Hz, the running speed of the output end of the linear motor 8 is 10mm/min, the vibrator 7 drives the material tank 2 and the titanium dioxide powder inside the material tank to vibrate, and the linear motor 8 drives the vibrator 7, the material tank 2 and the titanium dioxide powder inside the material tank 2 to move towards the direction of a material tank cover, so that the titanium dioxide powder is close to a hydrogen pipe;
(3) opening a valve of a hydrogen storage tank 1, wherein the hydrogen flow is 4L/min, after hydrogen enters a material tank 2, the hydrogen can bring titanium dioxide powder out of the material tank 2 due to vibration of the material tank 2 and the titanium dioxide powder inside, and then the hydrogen enters a reaction furnace, the high-temperature reaction of the reaction furnace 3 is carried out, the temperature is increased to 1550 ℃ at the heating rate of 10 ℃/min, and the material conveying speed is 10 mg/min;
(4) the reaction product enters a gas-solid separator 4 after coming out from the other end of the reaction furnace 3 along with the gas, and the solid separated by the gas-solid separator is lambda-Ti3O5The powder enters a material collecting tank 5, and the gas enters a tail gas purifying device 6 filled with water for purification treatment and then is emptied。
Example 4
Using the apparatus of example 1, λ -Ti was rapidly prepared3O5The method for preparing the powder comprises the following specific steps:
(1) firstly, repeatedly replacing air in a reaction device with hydrogen for many times to keep hydrogen atmosphere in a furnace device; the length of the high-temperature heating section in the reaction furnace 3 is 1 meter;
(2) drying commercial P25 powder, then filling the dried powder into a material tank 2, starting a vibrator 7 and a linear motor 8, wherein the vibration frequency of the vibrator 7 is 50Hz, the running speed of the output end of the linear motor 8 is 5mm/min, the vibrator 7 drives the material tank 2 and the titanium dioxide powder inside the material tank to vibrate, and the linear motor 8 drives the vibrator 7, the material tank 2 and the titanium dioxide powder inside the material tank 2 to move towards the direction of a material tank cover, so that the titanium dioxide powder is close to a hydrogen pipe;
(3) opening a valve of a hydrogen storage tank 1, wherein the hydrogen flow is 2L/min, after hydrogen enters a material tank 2, the hydrogen can take titanium dioxide powder out of the material tank 2 due to vibration of the material tank 2 and the titanium dioxide powder inside, and then the hydrogen enters a reaction furnace, the high-temperature reaction of the reaction furnace 3 is carried out, the temperature is increased to 1450 ℃ at the heating rate of 3 ℃/min, and the material conveying speed is 5 mg/min;
(4) the reaction product enters a gas-solid separator 4 after coming out from the other end of the reaction furnace 3 along with the gas, and the solid separated by the gas-solid separator is lambda-Ti3O5The powder enters a material collecting tank 5, and the gas enters a tail gas purifying device 6 filled with water for purification treatment and then is emptied.
Comparative example 1
XRD detection of the powder prepared in example 3 was carried out while the temperature of the reaction furnace 3 in step (3) of example 3 was set to 1300 ℃ in the same manner as in example 3, and it was found from the powder XRD pattern of the powder prepared in FIG. 4 that Ti began to appear in the phase of the product obtained in this example3O5But the host phase is Ti4O7Mainly comprises the following steps.
Comparative example 2
The temperature of the reaction furnace 3 in the step (3) of example 3 was set to 1285 ℃, and the prepared powder was subjected to XRD examination in the same manner as in example 3 except thatIn the powder XRD pattern of the powder obtained in FIG. 5, the phase of the product obtained in this example was Ti4O7And Ti5O9And the target phase was not found.
Claims (2)
1. Rapid preparation of lambda-Ti3O5The powder preparation method is characterized by comprising the following steps:
(1) repeatedly replacing air in the device with hydrogen to keep hydrogen atmosphere in the device;
(2) drying titanium dioxide powder, then loading the dried titanium dioxide powder into a material tank (2), starting a vibrator (7) and a linear motor (8), driving the material tank (2) and the titanium dioxide powder inside to vibrate by the vibrator (7), and driving the vibrator (7), the material tank (2) and the titanium dioxide powder inside the material tank (2) to move towards the material tank cover by the linear motor (8); the titanium dioxide powder is commercial P25 powder or pigment grade titanium dioxide powder; the running speed of the output end of the linear motor (8) is 5-10 mm/min;
(3) opening a valve of a hydrogen storage tank (1), allowing hydrogen to enter a material tank (2), and allowing the hydrogen to take titanium dioxide powder out of the material tank (2) and enter a reaction furnace (3) for high-temperature reaction in the reaction furnace (3); the high-temperature reaction of the reaction furnace (3) is carried out, wherein the temperature is increased to 1450-1550 ℃ at the temperature increase rate of 3-10 ℃/min; the hydrogen flow is 2-4L/min;
(4) the reaction product enters a gas-solid separator (4) after coming out from the other end of the reaction furnace (3) along with the gas, and the solid separated by the gas-solid separator (4) is lambda-Ti3O5The powder enters a material collecting tank (5), and the gas enters a tail gas purifying device (6);
the device used by the method comprises a hydrogen storage tank (1), a material tank (2), a reaction furnace (3), a gas-solid separator (4), a material collecting tank (5), a tail gas purification device (6), a vibrator (7) and a linear motor (8); the hydrogen storage tank (1) is connected with an inlet of the material tank (2), a vibrator (7) is arranged at the bottom of the material tank (2), the bottom of the vibrator (7) is connected with an output end of a linear motor (8), an outlet of the material tank (2) is connected with one end of a reaction furnace (3), the other end of the reaction furnace (3) is connected with a gas-solid separator (4), the bottom of the gas-solid separator (4) is connected with a material collecting tank (5), and the top of the gas-solid separator (4) is connected with a tail gas purification device (6); a vertical rail is arranged inside the material tank (2), a groove is formed in the material tank cover and matched with the vertical rail, and the material tank cover moves up and down along the vertical rail inside the material tank (2);
the length of the high-temperature heating section in the reaction furnace (3) is 0.8-1.2 m.
2. Rapid preparation of lambda-Ti according to claim 13O5The powder body preparation method is characterized in that the tail gas purification device (6) in the step (4) is filled with aqueous solution.
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