CN214599032U - Experimental device for be used for nucleation to deposit in preparation of nanometer oxide powder - Google Patents
Experimental device for be used for nucleation to deposit in preparation of nanometer oxide powder Download PDFInfo
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- CN214599032U CN214599032U CN202120312610.0U CN202120312610U CN214599032U CN 214599032 U CN214599032 U CN 214599032U CN 202120312610 U CN202120312610 U CN 202120312610U CN 214599032 U CN214599032 U CN 214599032U
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Abstract
Experimental device for be used for nucleation sediment in nanometer oxide powder preparation includes: the device body comprises a reaction chamber and a shell forming the reaction chamber, wherein a heating part is arranged on the shell, and a heat-insulating layer is arranged outside the shell; the plurality of feed inlets are arranged on the shell at the upper part of the device body and are communicated with the reaction chamber; the raw material premixing assembly is arranged in the reaction chamber; the stirring component is arranged on the shell at the upper part of the device body; the plurality of test ports are arranged on the shell at the upper part of the device body, are communicated with the reaction chamber and are used for arranging test components; the discharge port is arranged on the shell at the lower part of the device body and is used for releasing products in the reaction chamber; an exhaust port provided on the housing at the upper part of the apparatus body for releasing the gas in the reaction chamber; the raw materials input from the plurality of feed inlets are premixed in the raw material premixing assembly, then output from the discharge hole of the raw material premixing assembly and enter the reaction chamber to participate in the nucleation and precipitation process.
Description
Technical Field
The application belongs to the technical field of preparation of target oxide powder, and particularly relates to an experimental device for nucleation precipitation in preparation of nano oxide powder.
Background
The target material is a sputtering source which forms various functional films on a substrate by sputtering through a magnetron sputtering system, multi-arc ion plating system or other types of film coating systems under proper process conditions. The target material is mainly applied to industries such as photovoltaic cells, flat panel displays, large-scale integrated circuits, microelectronic devices, decorative coatings and the like, is a functional material with high added value, and along with the rapid development of the electronic information industry in China, China becomes one of the countries with the greatest requirement on sputtering target materials in the world. Obtaining high-quality raw material powder is the first important process for preparing the high-performance oxide target material, and the basic requirements of the high-performance oxide target material on the powder are as follows: high purity, nano-grade primary particle size, narrow particle size distribution range, regular particle shape, good dispersibility and high activity.
The existing methods for preparing the nano oxide powder mainly comprise a liquid phase method and a gas phase method. The conventional methods include a sol-gel method, a chemical liquid deposition method, an alkoxide hydrolysis method, a microemulsion method, a hydrothermal method, a microwave synthesis method, a citric acid gel combustion method, a chemical vapor deposition method, a sputtering method, an evaporation method, and the like. The oxide powder synthesized by the liquid phase method has uniform components, narrow particle size distribution and controllable appearance, can be subjected to batch test, is suitable for industrial production, but has the problems of easy agglomeration of products, easy introduction of impurities, various used raw materials, complex steps and special treatment.
The powder preparation equipment used in factory production is large, is a device which is operated in a large scale under a determined process, has high operation cost, is not suitable for carrying out the innovative research of the powder for the target material rapidly, and is not suitable for developing new products of oxide powder. The laboratory usually utilizes containers such as glass and the like to prepare powder through a chemical reaction method, but the yield is less, generally 10-50 g, each procedure is manual operation, the accuracy and the specification of each experiment of an operator must be ensured to obtain a correct result, and the yield of the order of magnitude can only be used for carrying out basic characteristic research on the powder and is not suitable for innovative research or other applications of a target material; meanwhile, because the operation and the powder preparation process are open, impurities are easy to introduce; in addition, each link in the powder preparation process is manually operated, so that the precise control and repeatability of the process are low, and the stability and continuity of the preparation of the target powder cannot be realized.
SUMMERY OF THE UTILITY MODEL
In order to solve at least one of the above-mentioned technical problems of the prior art, the embodiments of the present application disclose an experimental apparatus for nucleation precipitation in the preparation of nano-oxide powder, the apparatus comprising:
the device body comprises a reaction chamber and a shell forming the reaction chamber, wherein a heating part for heating the shell is arranged on the shell, and a heat-insulating layer is arranged outside the shell;
the plurality of feed inlets are arranged on the shell at the upper part of the device body and are communicated with the reaction chamber;
the raw material premixing component is arranged in the reaction chamber, a feeding hole communicated with the feeding hole is formed above the raw material premixing component, and a discharging hole is formed below the raw material premixing component;
the stirring assembly is arranged on the shell at the upper part of the device body and is used for stirring the mixed liquid in the reaction chamber;
the plurality of test ports are arranged on the shell at the upper part of the device body, are communicated with the reaction chamber and are used for arranging test components;
the discharge port is arranged on the shell at the lower part of the device body and is used for releasing products in the reaction chamber;
an exhaust port provided on the housing at the upper part of the apparatus body for releasing the gas in the reaction chamber;
the raw materials input from the plurality of feed inlets are premixed in the raw material premixing assembly, then output from the discharge hole of the raw material premixing assembly in a shower mode, and enter the reaction chamber to participate in the nucleation and precipitation process.
Some examples disclose experimental apparatus for nucleation deposits in nanometer oxide powder preparation, the discharge gate of raw materials premixing subassembly sets up to a plurality ofly, and the interval evenly distributes in raw materials premixing subassembly's below.
Some examples disclose experimental apparatus for nucleation and precipitation in preparation of nano oxide powder, the feed hole of the raw material premixing component is provided with a mixing blade for promoting premixing of input raw materials.
Some examples disclose an experimental apparatus for nucleation and precipitation in the preparation of nano-oxide powder, wherein a plurality of feed inlets are respectively communicated with a plurality of raw material supply devices, and the flow rate of raw materials flowing from the raw material supply devices through the feed inlets is controlled by setting a flow rate pump.
Some examples disclose an experimental apparatus for nucleation precipitation in the preparation of nano-oxide powder, the test parts comprising:
the temperature testing component is used for testing the temperature of the mixed liquid in the reaction chamber and controlling the precipitation reaction temperature;
and the pH testing component is used for testing the pH value of the mixed liquid in the reaction chamber and controlling the degree of the precipitation reaction.
Some examples disclose experimental facilities for nucleation and precipitation in preparation of nano oxide powder, and the heating component is a jacket heat exchange component.
Some embodiments disclose an experimental apparatus for nucleation and precipitation in preparation of nano oxide powder, wherein the inner wall of the shell is provided with a high borosilicate glass layer or a polytetrafluoroethylene layer.
Some embodiments disclose an experimental apparatus for nucleation and precipitation in preparation of nano-oxide powder, the stirring assembly comprising:
the double-layer stirring blade is arranged in the reaction chamber;
the stirring rod is arranged on the shell at the upper part of the device body, and the bottom end of the stirring rod is fixedly connected with the stirring blade;
and the motor is connected with the stirring rod and used for driving the stirring rod to rotate.
Some examples disclose an experimental apparatus for nucleation and precipitation in preparation of nano oxide powder, and an exhaust port is connected with a tail gas treatment component.
The experimental device for nucleation precipitation in the preparation of nanometer oxide powder disclosed in the embodiment of the application can effectively premix multiple raw materials, and can the accurate control deposit reaction process, the addition and the rate of accurate control stoste and reaction liquid, the degree that deposit reaction rate and reaction go on, further obtain the oxide powder of excellent performance in nucleation precipitation process, and can realize continuous feeding, continuous production, production efficiency and production capacity have been improved, form confined reaction system among the experimental device, impurity has been avoided introducing in the operation process, the purity of powder has been improved, and have tail gas processing apparatus, do not have the environmental protection problem, there is good application prospect in target powder preparation field.
Drawings
FIG. 1 schematic diagram of experimental apparatus in embodiment 1
FIG. 2 schematic diagram of experimental apparatus in embodiment 2
FIG. 3 example 3 schematic of the premix feed assembly
FIG. 4 example 4 schematic view of a raw material premix assembly
Reference numerals
1 housing 2 heating element
3 insulating layer 4 feed inlet
5 raw material premixing assembly 6 water filling port
7 stirring assembly 8 test port
9 exhaust port 10 tail gas reflux tower
11 tail gas absorption box 12 discharge openings
41 first inlet 42 second inlet
50 premix assembly housing 51 first feed port
52 second feed hole 53 first mixing blade
54 second mixing blade 55 discharge hole
71 stirring motor 72 stirring blade
81 first test port 82 second test port
83 thermometer 84 pH meter
100 reaction chamber 101 first material tank
102 second feed tank 103 first flow pump
104 second flow pump
Detailed Description
The word "embodiment" as used herein, is not necessarily to be construed as preferred or advantageous over other embodiments, including any embodiment illustrated as "exemplary". Performance index tests in the examples of this application, unless otherwise indicated, were performed using routine experimentation in the art. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure.
Unless defined otherwise, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs; other test methods and techniques not specifically mentioned in the present application are those commonly employed by those of ordinary skill in the art.
The terms "substantially" and "about" are used herein to describe small fluctuations. For example, they may mean less than or equal to ± 5%, such as less than or equal to ± 2%, such as less than or equal to ± 1%, such as less than or equal to ± 0.5%, such as less than or equal to ± 0.2%, such as less than or equal to ± 0.1%, such as less than or equal to ± 0.05%. Numerical data represented or presented herein in a range format is used merely for convenience and brevity and thus should be interpreted flexibly to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. For example, a numerical range of "1 to 5%" should be interpreted to include not only the explicitly recited values of 1% to 5%, but also include individual values and sub-ranges within the indicated range. Thus, included in this numerical range are individual values, such as 2%, 3.5%, and 4%, and sub-ranges, such as 1% to 3%, 2% to 4%, and 3% to 5%, etc. This principle applies equally to ranges reciting only one numerical value. Moreover, such an interpretation applies regardless of the breadth of the range or the characteristics being described.
In this document, including the claims, all conjunctions such as "comprising," including, "" carrying, "" having, "" containing, "" involving, "" containing, "and the like are to be understood as being open-ended, i.e., to mean" including but not limited to. Only the conjunctions "consisting of … …" and "consisting of … …" are closed conjunctions.
In the following detailed description, numerous specific details are set forth in order to provide a better understanding of the present disclosure. It will be understood by those skilled in the art that the present application may be practiced without some of these specific details. In the examples, some methods, means, instruments, apparatuses, etc. known to those skilled in the art are not described in detail in order to highlight the subject matter of the present application.
On the premise of no conflict, the technical features disclosed in the embodiments of the present application may be combined arbitrarily, and the obtained technical solution belongs to the content disclosed in the embodiments of the present application.
In some embodiments, the experimental apparatus for nucleation precipitation in the preparation of nano-oxide powder comprises: the device body comprises a reaction chamber and a shell forming the reaction chamber, wherein a heating part for heating the shell is arranged on the shell, and a heat-insulating layer is arranged outside the shell; the plurality of feed inlets are arranged on the shell at the upper part of the device body and are communicated with the reaction chamber; the raw material premixing component is arranged in the reaction chamber, a feeding hole communicated with the feeding hole is formed above the raw material premixing component, and a discharging hole is formed below the raw material premixing component; the stirring assembly is arranged on the shell at the upper part of the device body and is used for stirring the liquid in the reaction chamber; the plurality of test ports are arranged on the shell at the upper part of the device body, are communicated with the reaction chamber and are used for arranging test components; the discharge port is arranged on the shell at the lower part of the device body and is used for releasing products in the reaction chamber; an exhaust port provided on the housing at the upper part of the apparatus body for releasing the gas in the reaction chamber; the raw materials input from the plurality of feed inlets are uniformly premixed in the raw material premixing assembly, then output from the discharge hole of the raw material premixing assembly and enter the reaction chamber to participate in the nucleation and precipitation process.
The experimental device disclosed herein is generally used for experimental research on the preparation of nano oxide powder, and the design, structure and specification of the experimental device are generally consistent with those of experimental sites and experimental scales. Generally, the plurality of feeding holes are those having a plurality of mutually independent feeding holes, so as to simultaneously input a plurality of different raw materials into the reaction chamber of the experimental device, for example, the number of the feeding holes may be two, three, four, etc.; the positions of the feeding holes need to be set according to the test requirements, for example, the feeding holes can be adjacently arranged so as to mix the raw materials input into the plurality of feeding holes with each other; the raw material premixing component is arranged in the reaction chamber, the raw material premixing component is provided with feeding holes with the number consistent with that of the feeding holes so as to be communicated with the feeding holes arranged on the shell in a one-to-one correspondence manner, the feeding holes on the shell and the feeding holes of the raw material premixing component are connected with each other through rigid connecting pipes, and the raw material premixing component is fixedly connected to the inner wall of the shell; generally, a cavity with a proper shape and size is formed in the raw material premixing component, a plurality of raw materials are preliminarily premixed in the cavity, and reaction liquid is contacted in advance to form premixed liquid with uniform components before entering a reaction cavity; the raw material premixing component is also provided with a lower surface with a certain shape and size, discharge holes similar to showers are distributed on the raw material premixing component, premixed liquid flows out of the discharge holes and enters a reaction chamber of the experimental device to form mixed liquid, and the mixed liquid participates in the nucleation and precipitation process. The premixed liquid flows out from a plurality of discharge holes at the lower part of the raw material premixing component and can be widely spread on the liquid level of the mixed liquid below, and the larger the contact area with the mixed liquid is, the more the improvement of nucleation uniformity is facilitated; the stirring assembly is generally used for stirring the mixed liquid in the reaction chamber, so that the mixed liquid is promoted to be kept in a uniform state in the reaction process, and the premixed liquid spread on the liquid level of the mixed liquid is rapidly dispersed in the mixed liquid, thereby being beneficial to uniform nucleation and uniform precipitation; the test port is usually used for setting test components and monitoring the inside of the experimental device, and the test port is usually set to be a plurality of so as to set up a plurality of test components, such as 2, 3, 4, etc., for example, a temperature sensor is set up to monitor and control the internal temperature, and a pH sensor is set up to monitor and control the hydrogen ion concentration of the mixed liquid inside the pH sensor.
As an alternative embodiment, a plurality of discharge holes of the raw material premixing assembly are arranged, and are uniformly distributed below the raw material premixing assembly at intervals, so that the premixed liquid is uniformly dispersed in the mixed liquid below.
As an alternative embodiment, the feed hole of the raw material premixing assembly is provided with a mixing blade for promoting the mixing of the input raw materials. The mixing blades can disturb the input raw materials, so that the input raw materials move and disperse in multiple directions, the raw materials are mixed with other raw materials, and the mixing speed is accelerated; the propeller blades can be selected as mixing blades, the flowing raw materials can rotate, the flowing raw materials can obtain certain movement, and the premixed liquid which is premixed can further move to promote further mixing.
As an alternative embodiment, a plurality of feed inlets are respectively arranged to communicate with a plurality of raw material supply devices, and the flow rate of the raw material flowing from the raw material supply devices through the feed inlets is controlled by arranging a flow rate pump. The flow pump can convey the raw materials to the feeding hole at a certain pressure and flow rate, the raw materials enter the raw material premixing assembly at a certain speed, the raw materials with a certain speed can control the contact degree of the reaction liquid according to the test requirement, and the efficiency and the premixing effect of the premixing process are improved. The raw material supply device generally comprises a storage tank for storing raw materials, the raw materials generally comprise a plurality of raw materials for preparing powder, such as metal salt solution, alkali solution, and the like, and a peristaltic pump and the like can be selected as a flow pump.
As an alternative embodiment, the test member comprises: a temperature testing part for testing the temperature of the mixed liquid in the reaction chamber, such as a thermometer, a temperature sensor, etc.; and a pH testing part for testing the pH value of the mixed solution in the reaction chamber, such as a pH meter and the like.
As an alternative embodiment, the heating member is a jacket heat exchange member. Usually, the heat exchange part of the jacket is arranged outside the shell and sleeved on the outer surface of the shell, a heat exchange medium, such as heat conduction oil or water, is arranged in the heat exchange part, and the temperature and the flow of the heat conduction oil or the water are controlled by a heating circulating pump to control the internal temperature of the experimental device.
As an alternative, the inner wall of the housing is provided with a layer of high borosilicate glass or a layer of polytetrafluoroethylene. The high borosilicate glass layer or the polytetrafluoroethylene layer which is usually arranged on the inner wall of the shell can adapt to the reaction process of the reaction liquid under the acidic and alkaline conditions.
As an alternative embodiment, the stirring assembly comprises: the stirring blade is arranged in the reaction chamber; the stirring rod is arranged on the shell at the upper part of the device body, and the bottom end of the stirring rod is fixedly connected with the stirring blade; and the motor is connected with the stirring rod and used for driving the stirring rod to rotate.
As an alternative embodiment, the exhaust port is connected with an exhaust gas treatment component. Generally, the tail gas treatment assembly can treat and recover gas generated in the reaction chamber, and prevent the gas from being discharged into air to cause environmental pollution.
The technical details are further illustrated in the following examples.
Example 1
FIG. 1 is a schematic view of an experimental apparatus in example 1.
The experimental device for nucleation and precipitation in the preparation of the nano oxide powder disclosed in the embodiment 1 comprises a device body, wherein the device body comprises a reaction chamber 100 and a shell 1 forming the reaction chamber, a heating part 2 for heating the shell 1 is arranged on the shell 1, and an insulating layer 3 is arranged outside the shell 1; a plurality of feed ports 4 are arranged on the shell at the upper part of the device body and communicated with the reaction chamber 100; the raw material premixing component 5 is arranged in the reaction chamber 100, a feeding hole communicated with the feeding hole 4 is arranged above the raw material premixing component, and a discharging hole is arranged below the raw material premixing component; the stirring assembly 7 is arranged on a shell arranged at the upper part of the device body and positioned at the center of the device body, and is used for stirring the liquid in the reaction chamber 100; a plurality of test ports 8 are provided on the housing at the upper part of the apparatus body, communicate with the reaction chamber 100, and are used for arranging test parts; a discharge port 12 is provided in the housing at the lower part of the apparatus body for discharging the product in the reaction chamber; an exhaust port 9 is arranged on the shell at the upper part of the device body and used for releasing gas in the reaction chamber; the exhaust port 9 is communicated with a tail gas reflux tower 10, a circulating cooling pipeline is arranged inside the tail gas reflux tower 10, the tail gas can be cooled and refluxed for recovery, an exhaust pressure reducing port is arranged on the tail gas reflux tower 10 so as to control the steam pressure in the reaction chamber, and the tail gas reflux tower 10 is communicated with a tail gas absorption box 11 so as to recover the tail gas which does not completely reflux; a pressure balancing port is formed in the tail gas absorption box 11 so as to balance the pressure inside and outside the tail gas absorption box 11 and avoid potential safety hazards caused by out-of-control internal pressure; the upper shell of the device body is also provided with a water filling port 6 for inputting water into the reaction chamber and adjusting the pH value of the mixed liquid.
In the using process, a plurality of raw materials are respectively input from a plurality of feed inlets and enter the raw material premixing assembly for premixing, and after uniform premixing, the raw materials are output from the discharge hole of the raw material premixing assembly to enter the reaction chamber and are spread in the reaction chamber to participate in the nucleation and precipitation process.
Example 2
FIG. 2 is a schematic view of the experimental apparatus of example 2.
The experimental device for nucleation and precipitation in the preparation of the nano oxide powder disclosed in the embodiment 2 comprises a device body, wherein the device body comprises a reaction chamber and a shell for forming the reaction chamber, a heating part for heating the shell is arranged on the shell, and a heat-insulating layer is arranged outside the shell; the first feed port 41 and the second feed port 42 are provided on the casing at the upper part of the apparatus body, communicating with the reaction chamber; the raw material premixing assembly 5 is arranged in the reaction chamber; the stirring component arranged on the shell arranged at the upper part of the device body and positioned at the center of the device body comprises a stirring blade 72, the stirring blade 72 is arranged in the reaction chamber, and the stirring motor 71 is arranged on the outer shell and is connected with the stirring blade 72 through a stirring rod; a first test port 81 and a second test port 82 which are independently provided in the housing at the upper part of the apparatus body and respectively communicate with the reaction chamber, wherein a thermometer 83 is provided in the first test port 81, and a pH meter 84 is provided in the second test port 82; the discharge port is arranged on the shell at the lower part of the device body and is used for releasing products in the reaction chamber; an exhaust port 9 is arranged on the shell at the upper part of the device body and used for releasing gas in the reaction chamber; the exhaust port 9 is communicated with a tail gas reflux tower 10, a condensation reflux pipe is arranged in the tail gas reflux tower 10 to carry out condensation reflux recovery on gas, and the upper end of the tail gas reflux tower 10 is communicated with a tail gas absorption box 11 to further recover tail gas which does not completely reflux; the first feed inlet 41 is communicated with a first raw material tank 101, and a first flow pump 103 is arranged and connected between the first feed inlet and the first raw material tank; the second feed port 42 is arranged to be communicated with a second raw material tank 102, and a second flow pump 104 is arranged and connected between the second feed port and the second raw material tank; the upper shell of the device body is also provided with a water filling port 6 for inputting water into the reaction chamber and adjusting the pH value of the mixed liquid.
In the using process, a first raw material arranged in a first raw material tank 101 enters the raw material premixing assembly 5 at a set flow rate under the control of a first flow pump 103, a second raw material arranged in a second raw material tank 102 enters the raw material premixing assembly 5 at a set flow rate under the control of a second flow pump 104, and the first raw material and the second raw material are fully premixed in the raw material premixing assembly 5 to form a premixed liquid with uniformly distributed components; the premixed liquid is output from a discharge hole of the raw material premixing component to enter a reaction chamber and is spread in the reaction chamber to form mixed liquid to participate in a nucleation precipitation process, the mixed liquid is heated to a set temperature in the reaction chamber and is subjected to a nucleation precipitation reaction under a set pH condition, the mixed liquid is stirred by the stirring component in the reaction process to be kept in a uniform mixing state and rapidly dispersed, the premixed liquid added subsequently is added, the thermometer 83 is arranged in the mixed liquid to test the temperature of the premixed liquid, and the pH meter 84 is arranged in the mixed liquid to test the hydrogen ion content of the premixed liquid.
Example 3
FIG. 3 is a schematic view of the raw material premix assembly of example 3.
The raw material premixing assembly comprises a premixing assembly shell 50, wherein a first feeding hole 51 and a second feeding hole 52 are formed in the upper part of the premixing assembly shell 50, the first feeding hole 51 is communicated with a first feeding hole 41 formed in the shell 1 of the experimental device through a rigid pipeline, the second feeding hole 52 is communicated with a second feeding hole 42 formed in the shell 1 of the experimental device through a rigid pipeline, and the raw material premixing assembly shell 50 is fixedly installed on the inner wall of the shell 1;
a first mixing blade 53 is arranged below the first feeding hole 51, and after entering the first feeding hole 51 from the first feeding hole 41, the first raw material is distributed to a plurality of directions around under the action of the first mixing blade 53; a second mixing blade 54 is arranged below the second feeding hole 52, and the second raw material enters the second feeding hole 52 from the second feeding hole 42 and then is distributed to a plurality of directions around under the action of the second mixing blade 54. The premixing process of the first raw material and the second raw material in the raw material premixing assembly is more effective, and the premixed liquid is more uniform.
Example 4
FIG. 4 is a schematic view of the raw material premix assembly of example 4.
The raw material premixing assembly comprises a premixing assembly shell 50, wherein a first feeding hole 51 and a second feeding hole 52 are formed in the upper part of the premixing assembly shell 50, the first feeding hole 51 is communicated with a first feeding hole 41 formed in the shell 1 of the experimental device through a rigid pipeline, the second feeding hole 52 is communicated with a second feeding hole 42 formed in the shell 1 of the experimental device through a rigid pipeline, and the raw material premixing assembly shell 50 is fixedly installed on the inner wall of the shell 1;
the first mixing blades 53 are fixedly connected to the inner wall of the bottom of the premixing component shell 50 and positioned below the first feeding hole 51, and after entering the first feeding hole 51 from the first feeding hole 41, the first raw material is distributed to a plurality of directions around under the action of the first mixing blades 53; the second mixing blades 54 are disposed on the inner wall of the bottom of the premix assembly housing 50 and located below the second feed openings 52, and the second feed materials entering the second feed openings 52 through the second feed ports 42 are distributed in a plurality of directions around the second mixing blades 54. The mixing of the first and second materials in the material premixing assembly is more efficient and uniform.
The experimental device for nucleation precipitation in the preparation of nanometer oxide powder disclosed in the embodiment of the application can effectively premix multiple raw materials, and can the accurate control deposit reaction process, the addition and the rate of accurate control stoste and reaction liquid, the degree that deposit reaction rate and reaction go on, further obtain the oxide powder of excellent performance in nucleation precipitation process, and can realize continuous feeding, continuous production, production efficiency and production capacity have been improved, form confined reaction system among the experimental device, impurity has been avoided introducing in the operation process, the purity of powder has been improved, and have tail gas processing apparatus, do not have the environmental protection problem, there is good application prospect in target powder preparation field.
The technical solutions and the technical details disclosed in the embodiments of the present application are only examples to illustrate the inventive concept of the present application, and do not constitute a limitation on the technical solutions of the present application, and all the inventive changes, substitutions or combinations that do not create any inventive idea of the technical details disclosed in the present application are the same as the present application and are within the protection scope of the claims of the present application.
Claims (9)
1. Experimental device for be used for nucleation sediment in nanometer oxide powder preparation, its characterized in that includes:
the device comprises a device body and a heating device, wherein the device body comprises a reaction chamber and a shell forming the reaction chamber, a heating part for heating the shell is arranged on the shell, and a heat insulation layer is arranged outside the shell;
the plurality of feed inlets are arranged on the shell at the upper part of the device body and are communicated with the reaction chamber;
the raw material premixing component is arranged in the reaction chamber, a feeding hole communicated with the feeding hole is formed in the upper part of the raw material premixing component, and a discharging hole is formed in the lower part of the raw material premixing component;
the stirring assembly is arranged on the shell at the upper part of the device body and is used for stirring the mixed liquid in the reaction chamber;
the plurality of test ports are arranged on the shell at the upper part of the device body, are communicated with the reaction chamber and are used for arranging test components;
the discharge port is arranged on the shell at the lower part of the device body and is used for releasing products in the reaction chamber;
the exhaust port is arranged on the shell at the upper part of the device body and used for releasing gas in the reaction chamber;
the raw materials input from the plurality of feed inlets are premixed in the raw material premixing assembly, and then output from the discharge hole of the raw material premixing assembly in a shower mode to enter the reaction chamber to participate in the nucleation and precipitation process.
2. The experimental device for nucleation and precipitation in the preparation of nano-oxide powder according to claim 1, wherein the raw material premixing assembly comprises a plurality of discharge ports, and the discharge ports are uniformly distributed below the raw material premixing assembly.
3. The experimental apparatus for nucleation and precipitation in the preparation of nano-oxide powder according to claim 1, wherein the feed hole of the raw material premixing assembly is provided with a mixing blade for promoting the premixing of the input raw materials.
4. The experimental apparatus for nucleation and precipitation in the preparation of nano-oxide powder according to claim 1, wherein a plurality of said feed inlets are respectively disposed to communicate with a plurality of raw material supply devices, and a flow rate of raw material flowing from said raw material supply devices through said feed inlets is controlled by a flow rate pump.
5. The experimental set-up for nucleation and precipitation in the preparation of nano-oxide powder according to claim 1, wherein said test unit comprises:
the temperature testing component is used for testing the temperature of the mixed liquid in the reaction chamber and controlling the precipitation reaction temperature;
and the pH testing component is used for testing the pH value of the mixed liquid in the reaction chamber and controlling the degree of the precipitation reaction.
6. The experimental device for nucleation and precipitation in the preparation of nano-oxide powder according to claim 1, wherein the heating component is a jacket heat exchange component.
7. The experimental device for nucleation and precipitation in the preparation of nano-oxide powder according to claim 1, wherein the inner wall of the housing is provided with a borosilicate glass layer or a polytetrafluoroethylene layer.
8. The experimental apparatus for nucleation and precipitation in the preparation of nano-oxide powder according to claim 1, wherein said bundle stirring assembly comprises:
the double-layer stirring blade is arranged in the reaction chamber;
the stirring rod is arranged on the shell at the upper part of the device body, and the bottom end of the stirring rod is fixedly connected with the stirring blade;
and the motor is arranged and connected with the stirring rod and used for driving the stirring rod to rotate.
9. The experimental apparatus for nucleation and precipitation in the preparation of nano-oxide powder according to claim 1, wherein the exhaust port is connected with a tail gas treatment component.
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