CN115432735A - Preparation process and application of gas-phase-method nano-zirconia - Google Patents
Preparation process and application of gas-phase-method nano-zirconia Download PDFInfo
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- CN115432735A CN115432735A CN202210893087.4A CN202210893087A CN115432735A CN 115432735 A CN115432735 A CN 115432735A CN 202210893087 A CN202210893087 A CN 202210893087A CN 115432735 A CN115432735 A CN 115432735A
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Abstract
The invention relates to the field of C01G9/03, in particular to a preparation process and application of gas-phase nano-zirconia, which solve the defects of the traditional precipitation process, have simple production process, form nano-powder in one step, do not need powder post-treatment procedures such as precipitation solid-liquid separation, drying, grinding and the like, and can control the generated ZrO by controlling the mixed gas ejection speed, the temperature in a gas-phase reactor and the proportion of raw materials in the preparation process 2 The crystal form and the surface performance of the product can continuously produce the nano zirconia powder with various specifications, and the prepared nano powder product has small particles, high purity, easy dispersion and good filling property, and can be widely applied to various fields.
Description
Technical Field
The invention relates to the field of C01G9/03, in particular to a preparation process and application of gas-phase-method nano zirconium oxide.
Background
The nanometer material is one of the main development directions of the current material technology, and after the material is subjected to nanocrystallization, the mechanical property, the chemical property, the interface property, the photoelectric property, the catalytic property, the quantum characteristic and the like of the material are substantially leaped. The improvement of the performance widens the application field of the material, and makes a large number of technical targets which cannot be realized in the past possible. In addition, the improvement of the material performance greatly reduces the material usage amount, reduces energy exploitation and plays a great role in promoting the environmental improvement.
The existing methods for preparing nano zirconium oxide powder mainly comprise a liquid phase synthesis method, a fused salt evaporation and calcination method, a mechanical crushing method, an alkoxide hydrolysis method, an aluminum sulfate ammonia decomposition method and a chemical vapor phase method. The mature preparation process in China is mostly finished in a liquid phase, and Chinese patent CN107915255B discloses a preparation method of nano zirconia and the nano zirconia prepared by the preparation method, although the specific surface area of the nano zirconia is improved to a certain extent, the process steps are complicated, and a large amount of waste water and waste residues are generated in the powder post-treatment process. The traditional precipitation method process has the following defects: (1) The powder is easy to form gel in a liquid medium, and solid-liquid separation is difficult; (2) The components of the synthetic raw materials cannot be instantly and uniformly mixed, so that the nucleation and growth processes of the powder are different, and the particle size distribution is wide; (3) the energy consumption is high in the filter cake dehydration process; (4) Capillary action exists among the powder in the dehydration process, so that powder agglomeration is caused, and subsequent application is seriously influenced; (5) The mechanical crushing post-treatment process has the problem that the particle size distribution of nano/micron powder is difficult to control.
Therefore, aiming at the problems, the invention provides a preparation process and application of gas-phase nano-zirconia, the production process is simple, the nano-powder is formed at one time, powder post-treatment procedures such as precipitation solid-liquid separation, drying, grinding and the like are not needed, large-scale industrial production can be realized, and the prepared nano-powder product has small particles, high purity, easy dispersion and good filling property, and can be widely applied to various fields.
Disclosure of Invention
The invention provides a preparation process of gas-phase nano zirconium oxide, which at least comprises the following steps:
(1) ZrCl is put in a zirconium oxide evaporator in an inert environment 4 The solid is vaporized;
(2) Controlling the internal temperature of the evaporator and the amount of inert gas, and adjusting the ZrCl gas entering the gas phase reactor 4 Concentration of vapor to vaporized ZrCl 4 Mixing the steam with inert gas;
(3) Then the mixed gas is sprayed out at a certain flow rate and mixed with the heated superheated steam to obtain the steam-steam mixed gas.
As a preferable technical scheme, the preparation process of the gas-phase nano zirconia specifically comprises the following steps:
s1, adding a certain amount of zirconium tetrachloride solid into a bin, and performing gas replacement in the system for more than 5 times by using inert gas;
s2, after gas replacement is finished, heating the interior of the evaporator, continuously adding zirconium tetrachloride solid into the evaporator through a zirconium tetrachloride continuous feeding device after the temperature of the interior of the evaporator is more than or equal to 450 ℃, simultaneously introducing inert gas, further increasing the temperature of the interior of the evaporator after the evaporator is started for feeding for the first time to enable the temperature of the mixed gas of zirconium tetrachloride steam and the inert gas at the outlet of the evaporator to reach a specified temperature, and maintaining the temperature value of the mixed gas at the outlet of the evaporator;
s3, mixing the water vapor and the oxidizing gas, heating to a specified temperature, and introducing into a gas phase reactor;
s4, controlling the spraying speed of the zirconium tetrachloride mixed gas to be more than or equal to 50m/S, spraying the zirconium tetrachloride mixed gas through a nozzle, immediately contacting the sprayed zirconium tetrachloride mixed gas with the steam mixed gas, and carrying out chemical reaction in a gas phase reactor to obtain the nano-zirconia.
As a preferable technical scheme, the zirconium tetrachloride solid is anhydrous zirconium tetrachloride. Based on the preparation process provided by the invention, the raw material zirconium tetrachloride is controlled to be anhydrous zirconium tetrachloride, so that the problem that water contained in the raw material is changed into vapor after being evaporated at high temperature, and the stability of subsequent reaction and the purity and yield of a nano zirconium oxide product are influenced is avoided.
As a preferable technical solution, the inert gas is at least one of nitrogen, helium and argon. Preferably, the inert gas is nitrogen.
As a preferred technical solution, the oxidizing gas is air and/or oxygen; preferably, the oxidizing gas is air.
As a preferable technical solution, the volume ratio of the zirconium tetrachloride vapor to the inert gas in the step S2 is 1: (0.05-1); preferably, the volume ratio of the zirconium tetrachloride vapor to the inert gas in the step S2 is 1: (0.2-0.5).
As a preferable technical scheme, the temperature of the mixed gas of zirconium tetrachloride steam and inert gas at the outlet of the evaporator in the step S2 is 550-950 ℃, preferably 700-850 ℃.
As a preferable technical solution, the volume ratio of the oxidizing gas to the water vapor in the step S3 is (0.01-0.2): 1; preferably, the volume ratio of the oxidizing gas to the water vapor in step S3 is (0.05-0.1): 1.
as a preferable technical scheme, the spraying speed of the zirconium tetrachloride mixed gas in the step S4 is 50-200m/S; preferably, the spraying speed of the zirconium tetrachloride mixed gas in the step S4 is 80-120m/S.
As a preferable technical solution, the molar ratio of the zirconium tetrachloride mixed gas to the water vapor mixed gas in the step S4 is 1: (2-10); preferably, the molar ratio of the zirconium tetrachloride mixed gas to the water vapor mixed gas in the step S4 is 1: (7-9).
As a preferred technical scheme, the internal temperature of the gas phase reactor is controlled to be 500-900 ℃; preferably, the internal temperature of the gas phase reactor is controlled to 800 to 850 ℃.
The vapor phase method nanometer zirconium oxide preparation process based on the system can control the generated ZrO by controlling the mixed gas ejection speed, the temperature in the vapor phase reactor and the raw material proportion 2 The crystal form and the surface performance of the product can continuously produce the nano zirconia powder with various specifications.
The invention realizes the production of the nano zirconia powder by the gas phase process, solves the defects of the traditional precipitation process, has one-step molding of the powder in the production process, small and uniform particle size of nano particles, and simultaneously, the powder particles are agglomerated in a flocculent form, so that the powder is easier to disperse and the particle size distribution range is narrow after dispersion. In addition, the nano zirconia powder prepared by the process has small density and good filling performance, is matched with a filling agent in the fields of casting materials, silicon rubber, special ceramics and the like to ensure that the material has better compactness, has large surface activity, and expands the application of the nano zirconia powder in the fields of catalysts, photocatalysts and the like.
The invention also provides application of the preparation process of the gas-phase-method nano-zirconia, which is applied to the preparation of the nano-zirconia powder.
Advantageous effects
1. The invention provides a preparation process of gas-phase nano-zirconia and application thereof, the production process is simple, the nano-powder is formed at one time, powder post-treatment procedures such as precipitation method solid-liquid separation, drying, grinding and the like are not needed, large-scale industrial production can be realized, and the prepared nano-powder product has small particles, high purity, easy dispersion and good filling property, and is widely applied to various fields.
2. Based on the preparation process provided by the invention, the raw material zirconium tetrachloride is controlled to be anhydrous zirconium tetrachloride, so that the problem that water contained in the raw material is changed into vapor after being evaporated at high temperature, and the stability of subsequent reaction and the purity and yield of a nano zirconium oxide product are influenced is avoided.
3. The vapor phase method nanometer zirconium oxide preparation process based on the system can control the generated ZrO by controlling the mixed gas ejection speed, the temperature in the vapor phase reactor and the raw material proportion 2 The crystal form and the surface performance of the product can continuously produce the nano zirconia powder with various specifications.
4. The invention realizes the production of the nano zirconia powder by the gas phase process, solves the defects of the traditional precipitation process, has one-step molding of the powder in the production process, small and uniform particle size of nano particles, and simultaneously, the powder particles are agglomerated in a flocculent form, so that the powder is easier to disperse and the particle size distribution range is narrow after dispersion.
5. The nano zirconia powder prepared by the process has small density and good filling performance, is matched with a filling agent in the fields of casting materials, silicon rubber, special ceramics and the like to ensure that the material has better compactness, has large surface activity, and expands the application of the nano zirconia powder in the fields of catalysts, photocatalysts and the like.
Detailed Description
Example 1
The embodiment 1 of the invention provides a preparation process of gas-phase nano zirconium oxide, which specifically comprises the following steps:
s1, adding a certain amount of zirconium tetrachloride solid into a storage bin, and performing gas replacement in a system for 6 times by using inert gas;
s2, after gas replacement is finished, heating the interior of the evaporator, continuously adding zirconium tetrachloride solid into the evaporator at the speed of 0.4kg/h through a zirconium tetrachloride continuous feeding device after the interior temperature of the evaporator is 500 ℃, simultaneously introducing inert gas at the speed of 8L/h, further increasing the interior temperature of the evaporator after the evaporator is started for the first time and fed, enabling the temperature of mixed gas of zirconium tetrachloride steam and the inert gas at the outlet of the evaporator to reach a specified temperature, and maintaining the temperature value of the mixed gas at the outlet of the evaporator;
s3, preheating 30L/h of air to 550 ℃ through a first stage, introducing the air into a secondary heater, simultaneously controlling the amount of water vapor to be introduced into the secondary heater at the speed of 0.25kg/h, mixing the air with the air, and controlling the temperature of a water vapor mixed gas outlet to be 750 ℃;
s4, controlling the spraying speed of the zirconium tetrachloride mixed gas, spraying the zirconium tetrachloride mixed gas through a nozzle, immediately contacting the sprayed zirconium tetrachloride mixed gas with the steam mixed gas to perform chemical reaction in the gas phase reactor, continuously producing for 48 hours, collecting about 10.54kg of nano zirconium oxide powder in the gas-solid separator, and discharging HCl in the acidic tail gas after the acidic tail gas is collected by an absorption device.
The zirconium tetrachloride solid is anhydrous zirconium tetrachloride.
The inert gas is nitrogen.
The oxidizing gas is air.
The volume ratio of the zirconium tetrachloride steam to the inert gas in the step S2 is 1:0.2.
and in the step S2, the temperature of the mixed gas of zirconium tetrachloride steam and inert gas at the outlet of the evaporator is 700 ℃.
The volume ratio of air to water vapor in the step S3 is 0.1:1.
in the step S4, the spraying speed of the zirconium tetrachloride mixed gas is 100m/S.
In the step S4, the molar ratio of the zirconium tetrachloride mixed gas to the water vapor mixed gas is 1:8.
the internal temperature of the gas phase reactor was controlled to 680 ℃.
Example 2
The embodiment 2 of the invention provides a preparation process of gas-phase nano zirconium oxide, which specifically comprises the following steps:
s1, adding a certain amount of zirconium tetrachloride solid into a stock bin, and performing gas replacement in a system for 6 times by using inert gas;
s2, after gas replacement is finished, heating the interior of the evaporator, continuously adding zirconium tetrachloride solid into the evaporator at the speed of 0.4kg/h through a zirconium tetrachloride continuous feeding device after the interior temperature of the evaporator is 500 ℃, simultaneously introducing inert gas at the speed of 8L/h, further increasing the interior temperature of the evaporator after the evaporator is started for the first time and fed, enabling the temperature of mixed gas of zirconium tetrachloride steam and the inert gas at the outlet of the evaporator to reach a specified temperature, and maintaining the temperature value of the mixed gas at the outlet of the evaporator;
s3, preheating 30L/h of air to 550 ℃ through the primary heating, introducing the air into a secondary heater, simultaneously controlling the amount of water vapor to be introduced into the secondary heater at the speed of 0.25kg/h to be mixed with the air, and controlling the temperature of a water vapor mixed gas outlet to be controlled at 600 ℃;
s4, controlling the spraying speed of the zirconium tetrachloride mixed gas, spraying the zirconium tetrachloride mixed gas through a nozzle, immediately contacting the sprayed zirconium tetrachloride mixed gas with the steam mixed gas to perform chemical reaction in the gas phase reactor, continuously producing for 2.5 hours, collecting about 31.2g of nano-zirconia powder in a gas-solid separator because the zirconium tetrachloride mixed gas nozzle is frequently blocked, and discharging the acidic tail gas after collecting HCl in the acidic tail gas through an absorption device.
The zirconium tetrachloride solid is anhydrous zirconium tetrachloride.
The inert gas is nitrogen.
The oxidizing gas is air.
The volume ratio of the zirconium tetrachloride steam to the inert gas in the step S2 is 1:0.2.
and in the step S2, the temperature of the mixed gas of zirconium tetrachloride steam and inert gas at the outlet of the evaporator is 400 ℃.
The volume ratio of air to water vapor in the step S3 is 0.1:1.
the spraying speed of the zirconium tetrachloride mixed gas in the step S4 is 100m/S.
In the step S4, the molar ratio of the zirconium tetrachloride mixed gas to the water vapor mixed gas is 1:8.
the internal temperature of the gas phase reactor was controlled to 430 ℃.
Example 3
Embodiment 3 of the present invention provides a process for preparing a gas-phase nano zirconia, which specifically comprises the following steps:
s1, adding a certain amount of zirconium tetrachloride solid into a storage bin, and performing gas replacement in a system for 6 times by using inert gas;
s2, after gas replacement is finished, heating the interior of the evaporator, continuously adding zirconium tetrachloride solid into the evaporator at the speed of 0.5kg/h through a zirconium tetrachloride continuous feeding device after the interior temperature of the evaporator is 500 ℃, simultaneously introducing inert gas at the speed of 6L/h, further increasing the interior temperature of the evaporator after the evaporator is started for the first time and fed, enabling the temperature of the mixed gas of zirconium tetrachloride steam and the inert gas at the outlet of the evaporator to reach a specified temperature, and maintaining the temperature value of the mixed gas at the outlet of the evaporator;
s3, preheating 25L/h of air to 550 ℃ through the primary heating, introducing the air into a secondary heater, simultaneously controlling the amount of water vapor to be introduced into the secondary heater at the speed of 0.35kg/h to be mixed with the air, and controlling the temperature of a water vapor mixed gas outlet to be 750 ℃;
s4, controlling the spraying speed of the zirconium tetrachloride mixed gas, spraying the zirconium tetrachloride mixed gas through a nozzle, immediately contacting the sprayed zirconium tetrachloride mixed gas with the steam mixed gas to perform chemical reaction in the gas phase reactor, continuously producing for 48 hours, collecting about 13.19kg of nano-zirconia powder in the gas-solid separator, and discharging HCl in the acidic tail gas after the acidic tail gas passes through an absorption device and is collected.
The zirconium tetrachloride solid is anhydrous zirconium tetrachloride.
The inert gas is nitrogen.
The oxidizing gas is air.
The volume ratio of the zirconium tetrachloride steam to the inert gas in the step S2 is 1:0.1.
in the step S2, the temperature of the mixed gas of zirconium tetrachloride steam and inert gas at the outlet of the evaporator is 750 ℃.
The volume ratio of air to water vapor in the step S3 is 0.06:1.
in the step S4, the spraying speed of the zirconium tetrachloride mixed gas is 100m/S.
In the step S4, the molar ratio of the zirconium tetrachloride mixed gas to the water vapor mixed gas is 1:9.
the internal temperature of the gas phase reactor was controlled to 710 ℃.
Example 4
Embodiment 4 of the present invention provides a process for preparing a gas-phase nano zirconia, which specifically comprises the following steps:
s1, adding a certain amount of zirconium tetrachloride solid into a storage bin, and performing gas replacement in a system for 6 times by using inert gas;
s2, after gas replacement is finished, heating the interior of the evaporator, continuously adding zirconium tetrachloride solid into the evaporator at the speed of 0.2kg/h through a zirconium tetrachloride continuous feeding device after the interior temperature of the evaporator is 500 ℃, simultaneously introducing inert gas at the speed of 8L/h, further increasing the interior temperature of the evaporator after the evaporator is started for the first time and fed, enabling the temperature of mixed gas of zirconium tetrachloride steam and the inert gas at the outlet of the evaporator to reach a specified temperature, and maintaining the temperature value of the mixed gas at the outlet of the evaporator;
s3, preheating 30L/h of air to 550 ℃ through the primary heating, introducing the air into a secondary heater, simultaneously controlling the amount of water vapor to be introduced into the secondary heater at the speed of 0.15kg/h to be mixed with the air, and controlling the temperature of a water vapor mixed gas outlet to be 750 ℃;
s4, controlling the spraying speed of the zirconium tetrachloride mixed gas, spraying the zirconium tetrachloride mixed gas through a nozzle, immediately contacting the sprayed zirconium tetrachloride mixed gas with the steam mixed gas to perform chemical reaction in the gas phase reactor, continuously producing for 48 hours, collecting about 4.98kg of nano zirconium oxide powder in the gas-solid separator, and discharging HCl in the acidic tail gas after the acidic tail gas passes through an absorption device and is collected.
The zirconium tetrachloride solid is anhydrous zirconium tetrachloride.
The inert gas is nitrogen.
The oxidizing gas is air.
The volume ratio of the zirconium tetrachloride steam to the inert gas in the step S2 is 1:0.4.
and in the step S2, the temperature of the mixed gas of zirconium tetrachloride steam and inert gas at the outlet of the evaporator is 750 ℃.
The volume ratio of air to water vapor in the step S3 is 0.2:1.
and the spraying speed of the zirconium tetrachloride mixed gas in the step S4 is 75m/S.
In the step S4, the molar ratio of the zirconium tetrachloride mixed gas to the water vapor mixed gas is 1:10.
the internal temperature of the gas phase reactor was controlled to 670 ℃.
Performance test method
The appearance, specific surface area, aggregate particle size, primary particle average particle size, suspension pH, bulk density, volatiles, loss on ignition, and zirconia content of the nano zirconia powder prepared in the examples were measured, and the results are shown in table 1.
TABLE 1,
Claims (10)
1. A preparation process of gas-phase nano zirconia is characterized by at least comprising the following steps:
(1) ZrCl is put in a zirconium oxide evaporator in an inert environment 4 The solid is vaporized;
(2) Controlling the internal temperature of the evaporator and the amount of inert gas, and adjusting the temperature of the inert gas to enter the gas phase reactor ZrCl 4 Concentration of vapor to vaporized ZrCl 4 Mixing the steam with inert gas;
(3) And then spraying the mixed gas at a certain flow rate, and mixing the gas with the heated superheated steam to obtain the high-temperature-resistant superheated steam.
2. The preparation process of the gas-phase nano-zirconia according to claim 1, which is characterized by comprising the following steps:
s1, adding a certain amount of zirconium tetrachloride solid into a bin, and performing gas replacement in the system for more than 5 times by using inert gas;
s2, after gas replacement is finished, heating the interior of the evaporator, continuously adding zirconium tetrachloride solid into the evaporator through a zirconium tetrachloride continuous feeding device after the temperature of the interior of the evaporator is more than or equal to 450 ℃, simultaneously introducing inert gas, further increasing the temperature of the interior of the evaporator after the evaporator is started for feeding for the first time to enable the temperature of mixed gas of zirconium tetrachloride steam and the inert gas at the outlet of the evaporator to reach a specified temperature, and maintaining the temperature value of the mixed gas at the outlet of the evaporator;
s3, mixing water vapor and oxidizing gas, heating to a specified temperature, and introducing into a gas phase reactor;
s4, controlling the spraying speed of the zirconium tetrachloride mixed gas to be more than or equal to 50m/S, spraying the zirconium tetrachloride mixed gas through a nozzle, immediately contacting the sprayed zirconium tetrachloride mixed gas with the steam mixed gas, and carrying out chemical reaction in a gas phase reactor to obtain the nano-zirconia.
3. The process for preparing nano zirconia by a vapor phase method according to claim 1 or 2, wherein the inert gas is at least one of nitrogen, helium and argon.
4. The process for preparing nano zirconium oxide by gas phase method according to claim 3, wherein the volume ratio of zirconium tetrachloride steam to inert gas in the step S2 is 1: (0.05-1).
5. The process according to claim 4, wherein the temperature of the mixed gas of zirconium tetrachloride vapor and inert gas at the outlet of the evaporator in the step S2 is 550-950 ℃.
6. The process for preparing nano zirconia by a vapor phase method according to claim 5, wherein the volume ratio of the oxidizing gas to the water vapor in the step S3 is (0.01-0.2): 1.
7. the process according to claim 6, wherein the spraying speed of the mixed gas of zirconium tetrachloride in step S4 is 50-200m/S.
8. The process for preparing nano zirconium oxide by vapor phase method according to claim 7, wherein the molar ratio of the zirconium tetrachloride mixed gas to the water vapor mixed gas in the step S4 is 1: (2-10).
9. The process for preparing nano zirconia by a gas phase method according to claim 8, wherein the temperature inside the gas phase reactor is controlled to be 500-900 ℃.
10. The application of the preparation process of the gas-phase nano-zirconia according to claim 9 is characterized by being applied to the preparation of nano-zirconia powder.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1259488A (en) * | 1999-01-04 | 2000-07-12 | 北京大学 | Prepn. method of surface doped and weakly agglomerated nanometer zirconium oxide powder |
| CA2481152A1 (en) * | 2003-09-11 | 2005-03-11 | E.I. Du Pont De Nemours And Company | Plasma synthesis of metal oxide nanoparticles |
| CN111847507A (en) * | 2020-07-06 | 2020-10-30 | 南通江山农药化工股份有限公司 | Preparation process of nano titanium dioxide by gas phase method |
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- 2022-07-27 CN CN202210893087.4A patent/CN115432735A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1259488A (en) * | 1999-01-04 | 2000-07-12 | 北京大学 | Prepn. method of surface doped and weakly agglomerated nanometer zirconium oxide powder |
| CA2481152A1 (en) * | 2003-09-11 | 2005-03-11 | E.I. Du Pont De Nemours And Company | Plasma synthesis of metal oxide nanoparticles |
| CN111847507A (en) * | 2020-07-06 | 2020-10-30 | 南通江山农药化工股份有限公司 | Preparation process of nano titanium dioxide by gas phase method |
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