CN111761072A - Multi-section jet flow efficient mixing device and method for supercritical hydrothermal synthesis of nano metal powder - Google Patents

Multi-section jet flow efficient mixing device and method for supercritical hydrothermal synthesis of nano metal powder Download PDF

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CN111761072A
CN111761072A CN202010624323.3A CN202010624323A CN111761072A CN 111761072 A CN111761072 A CN 111761072A CN 202010624323 A CN202010624323 A CN 202010624323A CN 111761072 A CN111761072 A CN 111761072A
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laval
hydrothermal synthesis
metal powder
nano metal
supercritical
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CN111761072B (en
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王树众
王栋
孙盼盼
张宝权
刘璐
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Xian Jiaotong University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80Mixing plants; Combinations of mixers
    • B01F33/82Combinations of dissimilar mixers
    • B01F33/821Combinations of dissimilar mixers with consecutive receptacles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/71Feed mechanisms
    • B01F35/717Feed mechanisms characterised by the means for feeding the components to the mixer
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90Heating or cooling systems
    • B01F35/92Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90Heating or cooling systems
    • B01F2035/98Cooling

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

A multi-section jet flow high-efficiency mixing device for supercritical hydrothermal synthesis of nano metal powder comprises a sprayer, a Laval annular feeder and a static mixer which are sequentially communicated from top to bottom, wherein the top of the sprayer is a precursor material inlet, the bottom of the sprayer is a precursor material outlet, the top of the static mixer is an inlet, the bottom of the static mixer is an outlet, the interior of the Laval annular feeder is a vertical channel with two ends gradually reduced towards the middle, four reaction fluid inlet pipes used for feeding supercritical water, a modifier, a reducing agent and a pH regulator are communicated in the middle area of the Laval annular feeder, and the outlet of the supercritical water is arranged above the outlets of the modifier, the reducing agent and the pH regulator. The whole device realizes the rapid mixing and uniform mixing of the fluid through nozzle atomization, annular feeding acceleration and disturbance, adjusts the acidity and alkalinity of the mixed solution, and effectively ensures the quality of the nano metal particles.

Description

Multi-section jet flow efficient mixing device and method for supercritical hydrothermal synthesis of nano metal powder
Technical Field
The invention belongs to the technical field of chemical industry and environmental protection, and particularly relates to a multi-section jet flow efficient mixing device and method for supercritical hydrothermal synthesis of nano metal powder.
Background
As a leading-edge technology, the nanometer technology will bring great changes in the fields of chemical industry, medical treatment, communication, energy and the like, and the nanometer material is taken as the basis for developing the nanometer technology and becomes a hotspot for research in the field of material preparation at present. The nano material has special and excellent properties such as small size effect, surface effect, quantum tunneling effect and the like because the particle size is reduced to be less than 100 nm. The nano metal material not only has the special properties of the nano material, but also has the properties of the metal material, so that the nano metal material is widely applied to a plurality of fields. The traditional preparation method of the nano metal material comprises a physical method and a chemical method. The traditional preparation method has the defects of low production efficiency, large particle size, low product purity, easy surface pollution, complex equipment and difficult large-scale production; toxic reducing agents and a large amount of organic solvents are required to be added in the preparation process, and the production process is not environment-friendly; the prepared product has low crystallinity, needs subsequent heat treatment and has complex process. The problems faced by the traditional preparation method of the nano metal material seriously restrict the application of the nano material and the development of related industries.
The supercritical hydrothermal synthesis technology adopts supercritical water as a reaction medium, and utilizes the characteristic that the solubility of metal oxides in the supercritical water is extremely low to prepare nano metal and metal oxide powder thereof with small particle size. The nano-particles prepared by the supercritical hydrothermal synthesis technology have the characteristics of small particle size, uniform particle size distribution, high purity, controllable morphology, light agglomeration and the like. Meanwhile, the complex nano metal oxide powder can be prepared by multi-path feeding. Because supercritical water is adopted as a reaction medium, the supercritical hydrothermal synthesis technology has the following advantages: the reaction speed is high, the nucleation rate is high, the production process is efficient and environment-friendly, and the method has the potential of industrial production.
However, the supercritical hydrothermal synthesis technology has the following problems in the application process: the reaction temperature of the supercritical hydrothermal synthesis reaction is about 400 ℃, meanwhile, the supercritical hydrothermal synthesis reaction rate is high, too low heating rate can cause the metal salt solution to react when the reaction temperature is not reached, the particle size of the prepared product is large and uneven in distribution, the heating method adopted at present is to mix cold materials with high-temperature supercritical water with large flow and then quickly heat up to the reaction temperature, and therefore the key for preparing the nano material with good performance is to ensure that the cold materials and the supercritical water are quickly and effectively mixed; when the nano metal material is prepared, a reducing agent is required to be added to reduce nano metal oxide generated by supercritical hydrothermal synthesis into nano metal, a modifier is required to be added to perform surface modification on nano particles to prevent particle agglomeration, a pH regulator is required to be added to adjust the appearance and particle size of acid-base control particles of a reaction system, the reaction rate of the supercritical hydrothermal synthesis process is very high, the particle size is increased and the agglomeration phenomenon is serious due to the fact that the reaction time is prolonged, the performance of the nano material is seriously influenced, and therefore how to realize the quick and uniform mixing of multiple strands of fluid in a short time is very critical to the performance influence of the nano material. The existing mixing mode mostly adopts a T-shaped or Y-shaped mixer for mixing, and because the difference between cold materials and supercritical water fluid in the aspects of flow rate, density and the like is overlarge, the mixing method can cause the nonuniformity of a concentration field, a temperature field and a speed field during mixing, a large amount of particles are agglomerated together, and meanwhile, the particle size of a product is large and is unevenly distributed, so that the performance of the product is seriously influenced. Meanwhile, a simple T-shaped or Y-shaped mixer cannot realize uniform and rapid mixing of various materials, so that the morphology and the particle size of nano particles cannot be adjusted, the prepared product has large particle size and uneven particle size distribution, and the agglomeration phenomenon is obvious.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a multi-section jet flow high-efficiency mixing device and a multi-section jet flow high-efficiency mixing method for supercritical hydrothermal synthesis of nano metal powder.
In order to achieve the purpose, the invention adopts the technical scheme that:
a multi-section jet flow high-efficiency mixing device for supercritical hydrothermal synthesis of nano metal powder comprises a sprayer 1, a Laval annular feeder 2 and a static mixer 3 which are sequentially communicated from top to bottom, wherein the top of the sprayer 1 is a precursor material inlet, the bottom of the sprayer is a precursor material outlet, the top of the static mixer 3 is an inlet, the bottom of the static mixer is an outlet, the interior of the Laval annular feeder 2 is a vertical channel with two ends gradually reduced and narrowed towards the middle, and four reaction fluid inlet pipes 2-3 for feeding supercritical water, a modifier, a reducing agent and a pH regulator are communicated in the middle area of the Laval annular feeder, wherein the outlet of the supercritical water is arranged above the outlets of the modifier, the reducing agent and the pH regulator.
The sprayer 1 comprises a material inlet pipe 1-1, a water-cooling sleeve 1-2 wrapped outside the material inlet pipe 1-1 and a nozzle 1-3 installed and connected to the bottom end of the material inlet pipe 1-1.
The nozzles 1-3 are atomizing nozzles.
The cold water inlet and outlet of the water-cooling sleeve 1-2 are centrosymmetric, the cold water inlet is arranged below the water-cooling sleeve 1-2, and the outlet is arranged above the water-cooling sleeve 1-2.
The Laval annular feeder 2 comprises a cylinder body 2-7, a Laval boss 2-1 is arranged on the inner wall of the cylinder body 2-7, a vertical channel with two ends narrowing towards the middle in a smooth shrinkage mode is formed in the cylinder, a throat opening 2-6 is formed in the middle shrinkage area, and a precursor material outlet of the sprayer 1 is connected above the throat opening 2-6.
Four annular grooves 2-2 are arranged in the Laval boss 2-1, one end of each annular groove 2-2 is connected with a reaction fluid inlet pipe 2-3, and the other end of each annular groove 2-2 is communicated with the upper part of the narrowest position of the throat 2-6.
The other end of each annular groove 2-2 is communicated with an opening 2-5 on the inner wall of the Laval boss 2-1 through a drainage tube 2-4.
The static mixer 3 is SV type, SX type, SI type, SH type or SK type.
The invention also provides a mixing method based on the multistage jet flow efficient mixing device for supercritical hydrothermal synthesis of nano metal powder, which comprises the following steps:
1) the cold material enters a precursor material inlet of the sprayer 1, flows downwards and is sent out in a spraying mode;
2) supercritical water enters a Laval annular feeder 2 through a reaction fluid inlet pipe 2-3 and is fully mixed with atomized cold materials;
3) the reducing agent, the modifying agent and the pH regulating agent respectively enter a Laval annular feeder 2 through a reaction fluid inlet pipe 2-3 and are fully mixed with a mixed fluid of supercritical water and cold-state materials;
4) the mixed fluid passes through the middle contraction area of the Laval annular feeder 2, and the fluid is accelerated to improve the mixing degree;
5) the mixed fluid enters the static mixer 3, and is disturbed and swirled in the static mixer 3 to be sufficiently and uniformly mixed.
Compared with the prior art, the invention has the beneficial effects that:
1. through using the nozzle that has the atomizing function, spout precursor metal salt solution after atomizing into the annular feeder, improved the mixing degree of material and supercritical water for the abundant homogeneous mixing of material, and strengthen the heat transfer, make metal salt solution can rapid heating up to reaction temperature, do benefit to the good nanoparticle of preparation performance. The cooling water jacket arranged outside the precursor feeder pipe can effectively prevent the precursor from reacting before being mixed with supercritical water, and the property of the product is improved.
2. This device is through using annular feeder with supercritical water, reductant, modifier and pH regulator input blender, through set up the even feed inlet of a plurality of position distributions at annular feeder inner wall, can make above-mentioned stranded fluid evenly get into in the blender. Through set up the convergent throat behind the annular feeder, can make the fluid after the mixture in throat department with higher speed, strengthen the torrent degree of fluid after the mixture, strengthen mass transfer heat transfer process, reach rapid heating up, the effect of homogeneous mixing, guaranteed that supercritical hydrothermal synthesis reaction's high efficiency goes on. The mixed fluid is ensured to reach the temperature of the reaction condition by matching the flow of each fluid with the preheating temperature of the supercritical water. The purity, the morphology and the particle size of the nano-particles are regulated and controlled by controlling the flow of the reducing agent, the modifying agent and the pH regulator, so that the nano-metal particles with different morphologies and particle sizes are prepared.
3. Through set up static mixer behind the annular feeder, strengthen the disturbance degree of fluid after mixing, strengthened the inside heat and mass transfer of mixed fluid, improved the even degree of concentration field and temperature field in the mixer, avoid appearing local material concentration too high and lead to the condition that the granule particle diameter is great and distribute inhomogeneous even pipeline blocking, effectively guaranteed the quality of reaction product, improved the stability of mixer simultaneously.
Drawings
FIG. 1 is a schematic structural diagram of a multi-stage jet high-efficiency mixing device for supercritical hydrothermal synthesis of nano metal powder according to the present invention. Wherein 1 is a sprayer, 1-1 is a material inlet pipe, 1-2 is a water-cooling sleeve, and 1-3 is a nozzle; 2 is a Laval annular feeder, 2-1 is a Laval boss, 2-2 is an annular groove, 2-3 is a fluid inlet pipe, 2-4 is a drainage pipe, 2-5 is an opening, 2-6 is a throat, and 2-7 is a cylinder; and 3 is a static mixer.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It is to be understood that in the description and claims of the present invention, unless otherwise specified, "a plurality" means two or more. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
as shown in figure 1, the multi-section jet flow high-efficiency mixing device for supercritical hydrothermal synthesis of nano metal powder comprises a sprayer 1, a Laval annular feeder 2 and a static mixer 3 which are sequentially communicated from top to bottom. The top of the sprayer 1 is a precursor material inlet, the bottom of the sprayer is a precursor material outlet, the top of the static mixer 3 is an inlet, the bottom of the sprayer is an outlet, the inside of the Laval annular feeder 2 is a vertical channel with two ends gradually reduced and narrowed towards the middle, and four reaction fluid inlet pipes 2-3 for feeding supercritical water, a modifier, a reducing agent and a pH regulator are communicated in the middle area of the Laval annular feeder, wherein the outlet of the supercritical water is arranged above the outlets of the modifier, the reducing agent and the pH regulator.
The atomizer 1 comprises a material inlet pipe 1-1, a water-cooling sleeve 1-2 wrapped outside the material inlet pipe 1-1 and a nozzle 1-3 installed and connected to the bottom end of the material inlet pipe 1-1, wherein the nozzle 1-3 is a nozzle with an atomizing function and can be connected with the material inlet pipe 1-1 through a screw. The water-cooling sleeve 1-2 is connected with the material inlet pipe 1-1 in a welding mode, the cold water inlet and the cold water outlet of the water-cooling sleeve are centrosymmetric, the cold water inlet is arranged below the water-cooling sleeve 1-2, and the cold water outlet is arranged above the water-cooling sleeve 1-2.
The Laval annular feeder 2 comprises a cylinder body 2-7, the top of the cylinder body 2-7 is welded with the bottom of a material inlet pipe 1-1, a Laval boss 2-1 is arranged on the inner wall of the cylinder body 2-7 and connected with the cylinder body in a sealing mode, a vertical channel with two ends smoothly contracted and narrowed towards the middle is formed in the cylinder, a throat opening 2-6 is formed in the middle contraction area, and a precursor material outlet of a sprayer 1 is connected above the throat opening 2-6. Specifically, four annular grooves 2-2 are arranged in a Laval boss 2-1 to form annular cavities respectively, one end of each annular cavity is connected with a reaction fluid inlet pipe 2-3, the other end of each annular cavity is communicated with the position above the narrowest position of a throat 2-6, the other end of each annular groove 2-2 is communicated with an opening 2-5 on the inner wall of the Laval boss 2-1 through a drainage pipe 2-4, the opening 2-5 is used as a jet opening of a feeder, supercritical water, a modifier, a reducing agent and a pH regulator respectively enter the annular cavities through the reaction fluid inlet pipes 2-3 and then circularly flow into the inner cavity of the Laval annular feeder 2 through the drainage pipes 2-4 and the openings 2-5.
The static mixer 3 is a mixing device having a turbulent action to increase turbulence of a fluid, including but not limited to SV type, SX type, SI type, SH type, and SK type. Fig. 1 shows a static mixer of the SK type.
On the basis, the mixing method comprises the following steps:
1) the cold material enters a precursor material inlet of the sprayer 1, flows downwards and is sent out in a spraying mode, and uniform jet flow of the cold material solution is realized. Specifically, the cold material can be precursor metal salt solution, and the metal salt solution enters the Laval annular feeder 2 after being atomized by the atomizing nozzles 1-3. The water cooling sleeve 1-2 can prevent the metal salt solution from reacting before mixing with the supercritical water.
2) Supercritical water enters a Laval annular feeder 2 through a reaction fluid inlet pipe 2-3 and is fully mixed with atomized cold materials firstly. Specifically, supercritical water firstly enters an annular groove 2-2 and then enters the inner space of the Laval annular feeder 2 through a plurality of openings 2-5 on the inner wall, and the mixed fluid flows downwards towards a throat 2-6.
3) The reducing agent, the modifying agent and the pH regulator respectively enter a Laval annular feeder 2 through a reaction fluid inlet pipe 2-3 in the same way as the supercritical water, and are fully mixed with the mixed fluid of the supercritical water and the cold-state materials.
4) The mixed fluid passes through the intermediate constricted region of the laval ring feeder 2. Specifically, the throats 2-6 are a tapered nozzle structure, whereby the flow is accelerated therein, increasing the degree of mixing.
5) The mixed fluid enters the static mixer 3, is disturbed and swirled in the static mixer 3 to be fully and uniformly mixed, and the outlet of the static mixer is connected with a subsequent system.
In conclusion, the atomizing nozzle is designed to atomize and uniformly jet the metal salt solution, so that the mixing degree is improved, and the heat transfer and mass transfer of the mixed fluid are enhanced. Supercritical water, a reducing agent, a modifying agent and a pH regulator are uniformly injected into a metal salt solution by arranging a Laval annular feeder, rapid and uniform mixing is realized by utilizing the accelerating effect of a throat pipe, the mixing degree of multiple strands of fluids is improved, the heat transfer and mass transfer of the mixed fluid are enhanced, and the control on the type, purity, morphology and particle size of nanoparticles is realized by controlling the flow and the type of the fluid. The static mixer is arranged to improve the disturbance degree of the mixed fluid, enhance the fluid mixing degree and promote the reaction. The whole device realizes the rapid mixing and uniform mixing of the fluid through nozzle atomization, annular feeding acceleration and disturbance, adjusts the acidity and alkalinity of the mixed solution, and effectively ensures the quality of the nano metal particles.
It will be appreciated by those skilled in the art that the above-described embodiments are exemplary and can be modified by those skilled in the art, and that the structures described in the various embodiments can be freely combined without conflict in structure or principle, thereby solving the technical problem of the present invention.
Having described the embodiments of the present invention in detail, it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the scope and spirit of the appended claims, and the invention is not limited to the exemplary embodiments set forth in the specification. The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims (9)

1. The utility model provides a high-efficient mixing arrangement of multistage efflux for supercritical hydrothermal synthesis nanometer metal powder, its characterized in that includes atomizer (1), Laval annular feeder (2) and static mixer (3) that top-down communicates in proper order, and wherein the top of atomizer (1) is precursor material entry, and the bottom is precursor material export, and the top of static mixer (3) is the entry, and the bottom is the export, the inside of Laval annular feeder (2) is the vertical passageway that both ends narrow down to the centre convergent, and in its middle zone intercommunication have four reaction fluid import pipes (2-3) that are used for sending into supercritical water, modifier, reductant and pH regulator, wherein the export of supercritical water is in the top of modifier, reductant and pH regulator export.
2. The multi-stage jet flow high-efficiency mixing device for supercritical hydrothermal synthesis of nano metal powder as claimed in claim 1, wherein the sprayer (1) comprises a material inlet pipe (1-1), a water-cooling sleeve (1-2) wrapped outside the material inlet pipe (1-1) and a nozzle (1-3) installed and connected to the bottom end of the material inlet pipe (1-1).
3. The multi-stage jet flow high-efficiency mixing device for supercritical hydrothermal synthesis of nano metal powder according to claim 2, wherein the nozzles (1-3) are atomizing nozzles.
4. The multi-stage jet flow high-efficiency mixing device for supercritical hydrothermal synthesis of nano metal powder according to claim 2, wherein the cold water inlets and outlets of the water-cooling sleeves (1-2) are centrosymmetric, the cold water inlets are arranged below the water-cooling sleeves (1-2), and the outlets are arranged above the water-cooling sleeves (1-2).
5. The multi-section jet flow high-efficiency mixing device for supercritical hydrothermal synthesis of nano metal powder as claimed in claim 1, wherein the laval annular feeder (2) comprises a cylinder (2-7), the inner wall of the cylinder (2-7) is provided with laval bosses (2-1), a vertical channel with two ends narrowing towards the middle in a smooth shrinkage mode is formed in the cylinder, the middle shrinkage area is a throat (2-6), and a precursor material outlet of the sprayer (1) is connected above the throat (2-6).
6. The multistage jet flow efficient mixing device for supercritical hydrothermal synthesis of nano metal powder according to claim 5, wherein four annular grooves (2-2) are arranged in the Laval boss (2-1), one end of each annular groove (2-2) is connected with one reaction fluid inlet pipe (2-3), and the other end is communicated with the upper part of the narrowest position of the throat (2-6).
7. The multi-stage jet flow high-efficiency mixing device for supercritical hydrothermal synthesis of nano metal powder according to claim 6, wherein the other end of each annular groove (2-2) is communicated with an opening (2-5) on the inner wall of the Laval boss (2-1) through a drainage tube (2-4).
8. The multistage jet flow high-efficiency mixing device for supercritical hydrothermal synthesis of nano metal powder according to claim 6, wherein the static mixer (3) is SV type, SX type, SI type, SH type or SK type.
9. The mixing method of the multistage jet flow high-efficiency mixing device for supercritical hydrothermal synthesis of nano metal powder, based on claim 1, is characterized by comprising the following steps:
1) the cold material enters a precursor material inlet of the sprayer (1), flows downwards and is sent out in a spraying mode;
2) supercritical water enters a Laval annular feeder (2) through a reaction fluid inlet pipe (2-3) and is fully mixed with atomized cold materials;
3) the reducing agent, the modifying agent and the pH regulating agent respectively enter a Laval annular feeder (2) through a reaction fluid inlet pipe (2-3) and are fully mixed with a mixed fluid of supercritical water and cold materials;
4) the mixed fluid passes through the middle contraction area of the Laval annular feeder (2), and the fluid is accelerated to improve the mixing degree;
5) the mixed fluid enters the static mixer (3) and is disturbed and swirled in the static mixer (3) to be fully and uniformly mixed.
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