CN111774581B - Heat circulation system and method for supercritical hydrothermal synthesis of nano powder - Google Patents
Heat circulation system and method for supercritical hydrothermal synthesis of nano powder Download PDFInfo
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- CN111774581B CN111774581B CN202010639730.1A CN202010639730A CN111774581B CN 111774581 B CN111774581 B CN 111774581B CN 202010639730 A CN202010639730 A CN 202010639730A CN 111774581 B CN111774581 B CN 111774581B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24V—COLLECTION, PRODUCTION OR USE OF HEAT NOT OTHERWISE PROVIDED FOR
- F24V30/00—Apparatus or devices using heat produced by exothermal chemical reactions other than combustion
Abstract
A heat cycle system for supercritical hydrothermal synthesis of nanopowder comprises: the invention also provides a thermal cycle method based on the system, which can fully thermally cycle high-temperature and high-pressure fluid flowing out of a reactor, provide heat for unreacted fluid and dry nanoparticles through three-stage heat exchange, realize the recovery and gradient utilization of heat, realize energy level matching as far as possible in the utilization process of heat energy, furthest utilize low-grade heat energy, reduce the energy consumption and the operation cost of the system, improve the economy and the stability of the system, and realize the harmless and resource treatment of the system.
Description
Technical Field
The invention belongs to the technical fields of energy chemical industry, synthetic materials, environmental protection and the like, and particularly relates to a heat circulation system and a method for supercritical hydrothermal synthesis of nano powder.
Background
The nano material has unique electrical, thermal, magnetic, optical and mechanical properties, and is applied to the fields of electronic information, high-end manufacturing, new energy, green chemical industry, life medicine, military science and technology and the like, so that the revolutionary technical breakthrough in the field is caused, and the nano material has extremely bright application prospect.
The preparation of the nano material is the basis and core of the nano technology, and the existing synthesis methods of the nano material, such as a coprecipitation method, an alcohol hydrolysis precipitation method, a sol-gel method, a solvent evaporation method, a hydrothermal method and the like, have the problems of insufficient purity, complex process, high cost, long reaction time and the like, so that an efficient, thorough, environment-friendly and economic synthesis technology is urgently needed.
Supercritical Water (SCW) is a form of Water that exists in a specific manner above the critical state (T: 374.15 ℃, P: 22.12 MPa). In this form, the density of water becomes lower, the viscosity decreases, the diffusivity becomes higher, the ionic product increases by several orders of magnitude, and the number of hydrogen bonds increases greatly, which becomes a good reaction medium. Supercritical Hydrothermal Synthesis (SCHS) can hydrolyze and dehydrate a series of physical and chemical reactions by taking metal compounds as raw materials at the second level or millisecond level to precipitate nanoparticles with small particle size (5-10 nm), high purity and good dispersibility, has the advantages of greenness, high efficiency, low cost and the like, and is an ideal technology for preparing nano materials.
The technological process of continuous supercritical hydrothermal synthesis consists of 3 parts, including material feeding/preheating system, mixing/reaction system and cooling/material recovering system. In the charging/preheating system, the water-containing material is heated and pressurized to be above the critical point of water and then enters the mixing/reaction system, the material is fully reacted, and in the cooling/material recovery system, the outlet product after the reaction is finished can be discharged out of the system only by cooling and depressurizing, which relates to the problems of energy recovery and thermal cycle.
In the existing heat cycle system of the supercritical hydrothermal synthesis system, heat is generally directly transferred to materials or intermediate heat exchange substances by a high-temperature and high-pressure product of the materials after reaction in a reactor through a simple heat exchanger, so that the heat is utilized. Although the mode is also cyclic utilization, only one-stage heat exchange is generally carried out, the standard of energy cascade utilization is not met, the energy utilization rate is low, and the economical efficiency and the stability of the system are poor.
Therefore, a heat cycle system and a method for realizing energy gradient utilization in the field of supercritical hydrothermal synthesis of nano powder are needed, energy level matching is achieved as far as possible in the utilization process of heat energy, low-grade heat energy is utilized to the maximum extent, the heat efficiency of the system is improved, and energy is saved.
Disclosure of Invention
In order to overcome the defects of the prior art, reasonably utilize the heat energy of the system and optimize the heat circulation scheme, the invention aims to provide a heat circulation system and a method for supercritical hydrothermal synthesis of nano-powder, which can ensure that high-temperature and high-pressure fluid flowing out of a reactor is fully subjected to heat circulation, provide heat for unreacted fluid and dry nano-particles through three-stage heat exchange, realize the recovery and cascade utilization of heat, achieve energy level matching as far as possible in the utilization process of the heat energy, furthest utilize low-grade heat energy, reduce the energy consumption and the operation cost of the system, improve the economy and the stability of the system, and realize the harmless and recycling treatment of the system as well as the environment-friendly, economic and efficient because the waste gas is circularly combusted until the emission reaches the standard. The design of the whole system provides a certain condition for large-scale batch production of the nano materials, and accelerates the industrialization process of the supercritical hydrothermal synthesis technology.
In order to achieve the purpose, the invention adopts the technical scheme that:
a heat cycle system for supercritical hydrothermal synthesis of nanopowder comprises:
the material conveying unit comprises a material conveying line with a material storage tank 1 and a high-pressure pump I2 and a reducing agent conveying line with a reducing agent storage tank 3 and a high-pressure pump II 4, and an outlet of the high-pressure pump II 4 is divided into two branches;
the heat recycling unit comprises a mixer 5, wherein a first inlet of the mixer 5 is connected with an outlet of a first high-pressure pump 2, a second inlet of the mixer 5 is connected with an outlet of a heater 14, an outlet of the mixer is connected with an inlet at the top of a reactor 6, an outlet of the reactor 6 is connected with a hot side inlet of a preheater 7, a hot side outlet of the preheater 7 is connected with a hot side inlet of a heat regenerator 8, a cold side inlet of the preheater 7 is connected with one branch of a second high-pressure pump 4, a cold side outlet of the preheater 14 is connected with an inlet of the heater 14, the other branch of the second high-pressure pump 4 is connected with a material coil inlet of a gas furnace, and a material coil;
and the reaction post-processing unit comprises a pressure reduction unit 9, a product separation unit 10, an antioxidant processing unit 15 and a vacuum drier which are sequentially connected in a front-back manner, wherein an inlet of the pressure reduction unit 9 is connected with a hot side outlet of the heat regenerator 8.
And a cold side inlet of the heat regenerator 8 is connected with a heat source outlet of the vacuum dryer, and a cold side outlet is connected with a heat source inlet of the vacuum dryer.
The outlet of the product separation unit 10 is divided into three paths, the first path is a gas phase outlet and is connected with a gas inlet at the bottom of the gas furnace, and the second path is a liquid phase outlet and is connected with a waste liquid treatment unit 11; the third path is a solid-phase product outlet which is connected with an inlet of the anti-oxidation processing unit 15.
The gas outlet of the gas furnace is connected with a waste gas treatment unit 13.
And a material inlet of the vacuum drier is connected with an outlet of the antioxidant treatment unit 15, and a material outlet is connected with the product storage tank 17.
The first high-pressure pump 2 and the second high-pressure pump 4 are diaphragm type or piston type high-pressure pumps.
The mixer 5 is a T-shaped three-way mixer, a sleeve-type countercurrent mixer or a cross-shaped jet mixer; the reactor 6 is a tubular reactor or a kettle type reactor; the heater 14 is an electromagnetic heater, an infrared heater or a resistance heater; the preheater 7 and the regenerator 8 adopt a double-pipe high-pressure heat exchanger.
The invention also provides a thermal cycle method based on the thermal cycle system for supercritical hydrothermal synthesis of nano powder, which comprises the following steps:
and 5, separating the solid-liquid-gas three-phase mixture treated in the step 4 into three branches after the solid-liquid-gas three-phase separation is carried out in the product separation unit 10, enabling the gas to release heat for the reducing agent or the organic additive fluid in the step 2 after the gas enters the gas furnace for combustion, then enabling the gas to enter the waste gas treatment unit 13 for treatment, enabling the liquid phase to enter the waste liquid treatment unit 11 for treatment, enabling the water-containing solid-phase product to enter the anti-oxidation treatment unit 15 and the vacuum dryer to be changed into a solid-phase nanocrystal finished product, and then enabling the solid-phase nanocrystal finished.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention discloses a heat cycle system and a method for supercritical hydrothermal synthesis of nano powder, which comprises a material conveying unit, a heat cycle utilization unit and a reaction post-treatment unit; the material conveying unit conveys the metal precursor solution in the material storage tank and the reducing agent or the organic solvent in the reducing agent storage tank to the heat recycling unit after passing through the high-pressure pump; the low-temperature reducing agent or organic solvent in the heat recycling unit is subjected to heat exchange temperature rise through a preheater or a heating furnace, then passes through a heater, a mixer and a reactor, and is fully mixed with the metal precursor solution for rapid reaction; the reacted fluid sequentially passes through a preheater and a heat regenerator and exchanges heat with the cold fluid before reaction and the fluid in the dryer after reaction, so that the recovery and the gradient utilization of energy are realized; and finally, the reaction product enters a post-treatment unit for gas-liquid-solid three-phase post-treatment, so that the quality of the product, the resource and utilization of waste and the harmlessness and stabilization of a system are finally realized.
(2) The invention discloses a heat circulation system and a method for supercritical hydrothermal synthesis of nano powder, wherein the forms of a high-pressure pump, a preheater, a mixer, a reactor, a heater and the like are diversified, and when any part has a problem, workers can select more and are easy to replace.
(3) The invention discloses a heat cycle system and a method for supercritical hydrothermal synthesis of nano powder.A post-reaction treatment unit is used for carrying out stabilization and harmless landfill on separated liquid residues; the separated gas is circularly combusted until the gas reaches the standard and is discharged, so that the environment is protected; and carrying out anti-oxidation treatment and drying treatment on the separated solid particles to obtain high-quality nano crystal particles with small particle size, high purity and good dispersity.
(4) The heat circulation system and the method for supercritical hydrothermal synthesis of nano powder, disclosed by the invention, integrate multiple functions, improve the economy and stability of the system, realize system optimization, effectively solve the problems of rapid temperature rise and waste heat utilization of SCHS (small scale high speed high temperature synthesis) technology, provide a certain condition for large-scale batch production of nano materials, and accelerate the industrial process of the supercritical hydrothermal synthesis technology to a certain extent by the supercritical hydrothermal synthesis system with multi-stage utilization of energy.
Drawings
Fig. 1 is a schematic structural diagram of a supercritical hydrothermal synthesis nano-powder heat cycle system of the present invention.
Wherein: 1 is a material storage tank; 2 is a high-pressure pump 1; 3 is a reducing agent storage tank; 4 is a high-pressure pump II; 5 is a mixer; 6 is a reactor; 7 is a preheater; 8 is a heat regenerator; 9 is a voltage reduction unit; 10 is a product separation unit; 11 is a waste liquid treatment unit; 13 is an exhaust gas treatment unit; 14 is a heater; 15 is an anti-oxidation unit and 17 is a product storage tank.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention. The invention is described in further detail below with reference to the accompanying drawings:
referring to fig. 1, the heat cycle system and method for supercritical hydrothermal synthesis of nano-powder of the present invention comprises a material conveying unit, a heat cycle utilization unit, and a post-reaction treatment unit, wherein:
the material conveying unit comprises a material storage tank 1, a first high-pressure pump 2, a reducing agent storage tank 3 and a second high-pressure pump 4, an outlet of the material storage tank 1 is connected with an inlet of the first high-pressure pump 2 through a pipeline, an outlet of the reducing agent storage tank 3 is connected with an inlet of the second high-pressure pump 4 through a pipeline, and in the embodiment, an outlet of the second high-pressure pump 4 is divided into two branches.
The heat recycling unit includes a mixer 5, a reactor 6, a preheater 7, a regenerator 8, a gas furnace, a heater 14, and the like. The mixer 5 has two inlets, one inlet connected to the outlet of the first high pressure pump 2, the second inlet connected to the outlet of the heater 14, and the outlet connected to the top inlet of the reactor 6. The outlet of the reactor 6 is connected with the hot side inlet of the preheater 7, the hot side outlet of the preheater 7 is connected with the hot side inlet of the regenerator 8, the cold side inlet of the preheater 7 is connected with one branch of the second high-pressure pump 4, the cold side outlet is connected with the inlet of the heater 14, the other branch of the second high-pressure pump 4 is connected with the material coil inlet of the gas furnace, and the material coil outlet of the gas furnace is connected with the inlet of the heater 14.
The post-reaction treatment unit comprises a pressure reduction unit 9, a product separation unit 10, a waste liquid treatment unit 11, a waste gas treatment unit 13, an anti-oxidation treatment unit 15, a vacuum drier and a product storage tank 17. Wherein, the pressure reduction unit 9, the product separation unit 10, the antioxidant processing unit 15, the vacuum drier and the product storage tank 17 are sequentially connected in front and back, and the inlet of the pressure reduction unit 9 is connected with the hot side outlet of the heat regenerator 8. The waste liquid treatment unit 11 and the waste gas treatment unit 13 are positioned on a branch of the reaction post-treatment unit, and the waste gas treatment unit 13 is connected with a gas outlet of the gas furnace. The outlet of the product separation unit 10 is divided into three paths, the first path is a gas phase outlet and is connected with a gas inlet at the bottom of the gas furnace, and the second path is a liquid phase outlet and is connected with a waste liquid treatment unit 11; the third path is a solid-phase product outlet which is connected with an inlet of the anti-oxidation processing unit 15. The vacuum dryer is provided with 2 inlets and 2 outlets, wherein the material inlet is connected with the outlet of the anti-oxidation treatment unit 15, and the material outlet is connected with the product storage tank 17; the heat source inlet is connected to the cold side outlet of regenerator 8, which is connected to the cold side inlet of regenerator 8.
In the invention, the first high-pressure pump and the second high-pressure pump 4 can be selected from a diaphragm type or a piston type high-pressure pump, and the mixer 5 can be a T-shaped three-way mixer, a sleeve type counter-flow mixer and a cross jet type mixer; the reactor 6 may be a tubular reactor or a tank reactor; the heater 14 may be an electromagnetic heater, an infrared heater, or a resistance heater; the preheater 7 and the regenerator 8 adopt a double-pipe high-pressure heat exchanger.
The invention relates to a thermal cycle method for supercritical hydrothermal synthesis of nano powder, which is based on the thermal cycle system and comprises the following steps:
And 4, sequentially feeding the solid-liquid-gas three-phase mixture subjected to further temperature reduction into a pressure reduction unit 9 and a product separation unit 10, and performing solid-liquid-gas three-phase separation in the product separation unit. Wherein the gas phase enters the gas furnace to burn and then releases heat to the reducing agent or organic additive fluid in the step 2), and the circulation is startedThe waste gas generated by the system is concentrated in the waste gas treatment unit 13 for treatment, so that the harmful gas is changed into CO2、N2And H2And releasing clean gases such as O and the like, allowing a liquid phase to enter a waste liquid treatment unit 11 for harmless treatment, allowing a water-containing solid-phase product to enter an antioxidant treatment unit 15 for preventing oxidation and agglomeration of particles to generate impurities, allowing the impurities to enter a vacuum drier to become a solid-phase nanocrystal finished product, and conveying the solid-phase nanocrystal finished product into a product storage tank 17, wherein the product in the product storage tank 17 is generally nanocrystal with small particle size, good dispersity and high purity. The reaction post-treatment unit completely meets the standard emission standard of waste gas and waste liquid, and is green, environment-friendly and efficient.
The invention relates to a heat cycle system for supercritical hydrothermal synthesis of nano powder by energy gradient utilization, which comprises the following steps:
can let the abundant thermal cycle of the high temperature high pressure fluid that flows out in the reactor, provide the heat for unreacted fluid and dry nanoparticle through tertiary heat transfer, realize thermal recovery and cascade utilization, accomplish the energy level matching as far as possible in the utilization process of heat energy, and utilize low-grade heat energy to furthest, reduce system energy consumption and running cost, improve system economy and stability, in addition, because waste gas circulation burning is up to discharge to reach standard, realize system innocent treatment and resourceful treatment, green economy and high efficiency. The design of the whole system provides a certain condition for large-scale batch production of the nano materials, and accelerates the industrialization process of the supercritical hydrothermal synthesis technology.
Of course, the anti-oxidation treatment unit 15 of the present invention is not limited to be connected between the product separation unit 10 and the vacuum dryer, and the gas furnace is not limited to be connected between the high-pressure pump two 4 and the product separation unit 10, that is, the process sequence is not limited to the above, and particularly, reasonable and efficient cascade utilization is performed according to the quality of the waste heat.
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 (7)
1. A thermal cycle method for supercritical hydrothermal synthesis of nano powder is realized based on a thermal cycle system, and the thermal cycle system comprises:
the material conveying unit comprises a material conveying line with a material storage tank (1) and a high-pressure pump I (2) and a reducing agent conveying line with a reducing agent storage tank (3) and a high-pressure pump II (4), and an outlet of the high-pressure pump II (4) is divided into two branches;
the heat recycling unit comprises a mixer (5), wherein a first inlet of the mixer (5) is connected with an outlet of a first high-pressure pump (2), a second inlet of the mixer (5) is connected with an outlet of a heater (14), an outlet of the mixer is connected with a top inlet of a reactor (6), an outlet of the reactor (6) is connected with a hot side inlet of a preheater (7), a hot side outlet of the preheater (7) is connected with a hot side inlet of a heat regenerator (8), a cold side inlet of the preheater (7) is connected with one branch of a second high-pressure pump (4), a cold side outlet of the preheater is connected with an inlet of the heater (14), the other branch of the second high-pressure pump (4) is connected with a material coil inlet of a gas furnace, and a material coil outlet of the gas furnace is connected with an inlet;
the reaction post-processing unit comprises a pressure reduction unit (9), a product separation unit (10), an antioxidant processing unit (15) and a vacuum drier which are sequentially connected in front and back, wherein an inlet of the pressure reduction unit (9) is connected with a hot side outlet of the heat regenerator (8);
the thermal cycle method is characterized by comprising the following steps:
step 1), a metal salt solution, namely a precursor solution, enters a material storage tank (1) for storage, the pressure of the metal salt solution is increased by a high-pressure pump I (2) to reach the critical pressure value of supercritical hydrothermal synthesis, and the increased pressure material is pumped into a mixer (5);
step 2), the reducing agent or the organic additive is boosted and conveyed from a reducing agent storage tank (3) by a second high-pressure pump (4) to be divided into two branches, one branch is pumped into a preheater (7) to carry out heat exchange with high-temperature fluid flowing out of a reactor (6) so as to heat, the other branch enters a gas furnace to carry out heat absorption and temperature rise, the two heated reducing agent or organic additive flows are converged and enter a heater (14) to complete second-stage preheating and temperature rise, and then are quickly, uniformly and efficiently mixed with the material in the step 1) in a mixer (5);
step 3), the fluid fully mixed in the step 2) enters a reactor (6) through a pipeline to carry out rapid and uniform hydrolysis reaction, dehydration reaction and reduction reaction, then flows into a preheater (7) to carry out heat exchange with unreacted low-temperature fluid, and then is quenched and cooled, so that heat circulation is realized, and a solid-liquid-gas three-phase mixture containing nanocrystals is formed;
step 4), the solid-liquid-gas three-phase mixture subjected to heat exchange and temperature reduction in the step 3) enters a heat regenerator (8), heat is circularly exchanged with heat source fluid in the vacuum dryer by using waste heat, and the mixture enters a pressure reduction unit (9) and a product separation unit (10) after being further cooled;
and 5) separating the solid-liquid-gas three-phase mixture treated in the step 4) into three branches after solid-liquid-gas three-phase separation in a product separation unit (10), enabling the gas to release heat for the reducing agent or the organic additive fluid in the step 2) after entering a gas furnace for combustion, then entering a waste gas treatment unit (13) for treatment, enabling a liquid phase to enter a waste liquid treatment unit (11) for treatment, enabling a solid-phase product containing water to enter an anti-oxidation treatment unit (15) and a vacuum dryer to be changed into a solid-phase nanocrystal finished product, and then sending the solid-phase nanocrystal finished product into a product storage tank (17).
2. The thermal cycle method for supercritical hydrothermal synthesis of nanopowder according to claim 1, wherein the cold side inlet of the regenerator (8) is connected with the heat source outlet of the vacuum drier, and the cold side outlet is connected with the heat source inlet of the vacuum drier.
3. The thermal cycle method for supercritical hydrothermal synthesis of nanopowder as defined in claim 1, wherein the outlet of the product separation unit (10) is divided into three paths, the first path is a gas phase outlet connected to the gas inlet at the bottom of the gas furnace, and the second path is a liquid phase outlet connected to the waste liquid treatment unit (11); the third path is a solid-phase product outlet which is connected with an inlet of an anti-oxidation processing unit (15).
4. The thermal cycle method for supercritical hydrothermal synthesis of nanopowder as claimed in claim 1, wherein the gas outlet of the gas furnace is connected to an exhaust gas treatment unit (13).
5. The thermal cycle method for supercritical hydrothermal synthesis of nanopowder as defined in claim 1, wherein the material inlet of the vacuum drier is connected with the outlet of the anti-oxidation treatment unit (15), and the material outlet is connected with the product storage tank (17).
6. The thermal cycle method for supercritical hydrothermal synthesis of nanopowders according to claim 1, wherein the first high pressure pump (2) and the second high pressure pump (4) are diaphragm type or piston type high pressure pumps.
7. The thermal cycle method for supercritical hydrothermal synthesis of nanopowder according to claim 1, wherein the mixer (5) is a T-shaped three-way mixer, a sleeve-type counter-flow mixer or a cross-type jet mixer; the reactor (6) is a tubular reactor or a kettle type reactor; the heater (14) is an electromagnetic heater, an infrared heater or a resistance heater; the preheater (7) and the regenerator (8) adopt a double-pipe high-pressure heat exchanger.
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| CN103935962A (en) * | 2014-04-02 | 2014-07-23 | 西安交通大学 | Supercritical hydrothermal synthesis preparation system of nano-metal oxide |
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| CN103935962A (en) * | 2014-04-02 | 2014-07-23 | 西安交通大学 | Supercritical hydrothermal synthesis preparation system of nano-metal oxide |
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