CN111111584B - Supercritical hydrothermal synthesis reaction device coupled with online ultrasonic crushing technology and hydrothermal synthesis method thereof - Google Patents
Supercritical hydrothermal synthesis reaction device coupled with online ultrasonic crushing technology and hydrothermal synthesis method thereof Download PDFInfo
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- CN111111584B CN111111584B CN201911358447.5A CN201911358447A CN111111584B CN 111111584 B CN111111584 B CN 111111584B CN 201911358447 A CN201911358447 A CN 201911358447A CN 111111584 B CN111111584 B CN 111111584B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
Abstract
The invention discloses a supercritical hydrothermal synthesis reaction device coupled with an online ultrasonic crushing technology and a hydrothermal synthesis method thereof, belonging to the technical field of chemical industry. The ultrasonic high-pressure kettle with mature and reliable products on the market is adopted, the pipeline of the supercritical hydrothermal synthesis reactor is placed in the high-pressure kettle, ultrasonic strengthening particles are broken and dispersed in the supercritical hydrothermal synthesis reaction process, and therefore products with low particle size and high value are obtained, the supercritical water in the high-pressure kettle can be used as a heat preservation medium, and the problem that the product quality is influenced by heat dissipation of materials in the reactor in the reaction process is solved. Meanwhile, the invention realizes the parallel connection of a plurality of pipelines by arranging the flow divider and controls the reaction time by controlling the total through-flow time. The invention effectively solves the problem that the traditional ultrasonic transducer can not be attached to the outer surface of the high-temperature and superfine pipeline of the supercritical hydrothermal synthesis tubular reactor, and effectively improves the product quality of preparing the nano metal powder by adopting the supercritical hydrothermal synthesis technology.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a supercritical hydrothermal synthesis reaction device coupled with an online ultrasonic crushing technology and a hydrothermal synthesis method thereof.
Background
The supercritical hydrothermal synthesis technology is a green synthesis technology for preparing nano metal powder. The basic principle of the supercritical hydrothermal synthesis technology is that supercritical water is adopted as a reaction medium in a closed high-pressure container to form nano metal or metal oxide powder with extremely small particle size. The particles prepared in the supercritical hydrothermal synthesis process have the advantages of uniform particle size distribution, complete crystal grain development, high purity, light particle agglomeration, applicability to cheap raw materials, low operation cost compared with the traditional preparation method, and the technical advantages of preparing the nano metal particles by supercritical hydrothermal synthesis mainly comprise the following aspects:
1. the nucleation rate is extremely high, which is beneficial to the formation of ultrafine particles (10nm-30 nm);
2. the reaction rate is extremely fast and is improved by several orders of magnitude compared with the conventional method;
3. the reaction space is closed, no secondary pollution is caused, and the environment is friendly.
For the nano material, the lower the particle size, the greater the product value. At present, scientific researchers and enterprise technical research personnel at home and abroad control the particle size by various methods, and the methods mainly comprise intensified mixing of a mixer section, intensified particle crushing by applying an ultrasonic vibration external field effect in the reaction process, accurate control of reaction time and the like. Wherein, ultrasonic crushing is to generate cavitation through alternate compression and expansion, realize crushing effect on the nano particles in the reaction process and inhibit the agglomeration of the nano particles.
Currently, the loading of ultrasonic waves is generally realized by directly welding an ultrasonic transducer on a pipeline. Supercritical hydrothermal synthesis reactors generally adopt a tubular reactor form, namely materials flow in a pipeline and react, and the reaction time is controlled by controlling the retention time of the materials in the pipeline of the reactor. This group of technologies has been introduced in the patent "an apparatus and method for producing nano metal powder based on supercritical hydrothermal synthesis technology" (application No. 2019101011364). The reaction time of the supercritical hydrothermal synthesis reaction needs to be accurately controlled in the second level, so that a pipeline with a small inner diameter (generally lower than 20mm) is generally adopted as a pipeline of the reactor in order to accurately control the reaction time. Moreover, the supercritical hydrothermal synthesis reaction is an endothermic reaction, and in order to maintain the reaction temperature, an insulating layer or an external heating device is generally arranged on the outer surface of the reactor pipeline, and the temperature of the outer surface of the pipeline can generally reach 400-500 ℃. Thus, it is difficult to mount the ultrasonic wave generator on the pipe for the following reasons:
1) the reactor tube is undersized, and the diameter of the wafer (i.e., the element where the ultrasonic transducer is directly welded to the outer wall of the tube) of the transducer of the more reliable ultrasonic generator currently on the market is generally higher than 20mm, so that the transducer is difficult to load.
2.) the highest temperature resistance of the wafer of the transducer of the more reliable ultrasonic generating device sold in the market at present is generally lower than 200 ℃, while the temperature of the outer wall surface of the supercritical hydrothermal synthesis reactor is far higher than 200 ℃, and the transducer can be damaged soon after being welded on the wall surface of the pipeline. And the arrangement of the energy converter can damage the heat insulation layer of the reactor, which is unacceptable for the supercritical hydrothermal synthesis reaction.
Disclosure of Invention
In order to overcome the technical problems, the invention discloses a supercritical hydrothermal synthesis reaction device coupled with an online ultrasonic crushing technology and a hydrothermal synthesis method thereof, which can solve the problem that the traditional ultrasonic transducer cannot be attached to the outer surface of a high-temperature and superfine pipeline of a supercritical hydrothermal synthesis tubular reactor.
The invention is realized by the following technical scheme:
the invention discloses a supercritical hydrothermal synthesis reaction device coupled with an online ultrasonic crushing technology, which comprises an ultrasonic transducer, a high-pressure kettle and a tubular reactor, wherein the ultrasonic transducer is arranged in the high-pressure kettle;
the tubular reactor is arranged in the autoclave body, the ultrasonic transducer is fixedly connected to the top cover of the autoclave, and the heating sleeve is arranged outside the autoclave body;
the top cover is provided with an inlet of the tubular reactor and a plurality of pipeline outlets of the tubular reactor, and the bottom of the kettle body is provided with an autoclave outlet;
the inlet pipeline of the tubular reactor extending into the kettle body is provided with a flow divider, the inlet pipeline is branched into a plurality of parallel pipelines through the flow divider, the fluid entering the kettle body can be averagely divided into a plurality of strands of parallel fluid, and the tail ends of the parallel pipelines are connected to the outlet of the pipeline.
Preferably, the plurality of parallel pipelines have the same size, and the pipelines immersed in the kettle body have the same length.
Preferably, a high-temperature high-pressure stop valve is arranged on a pipeline externally connected with each pipeline outlet of the tubular reactor.
Preferably, the heating jacket adopts a silicon-molybdenum rod or an electric furnace wire.
Preferably, the heating jacket is externally provided with an insulating layer.
Preferably, the bottom of the heat-insulating layer is provided with a bottom outlet, the autoclave outlet is externally connected with a guide pipe which can extend out of the bottom outlet, and the guide pipe is provided with a valve.
Preferably, an interface shared by the ultrasonic transducer and the tubular reactor is further formed in the top cover, and the ultrasonic transducer is connected to the top cover through the interface in a welding or bolt mode.
Preferably, a thermowell inlet for inserting a thermocouple and a pressure gauge lead interface for inserting a pressure gauge are further provided on the top cover.
The invention also discloses a method for carrying out supercritical hydrothermal synthesis reaction by adopting the supercritical hydrothermal synthesis reaction device coupled with the on-line ultrasonic crushing technology, which comprises the following steps:
1) obtaining the feeding amount of reactants in the high-pressure autoclave through theoretical calculation and Aspen plus simulation according to physical properties;
2) opening the top cover, feeding according to the feeding amount obtained in the step, then reinstalling the top cover, setting the required heating temperature, and starting the heating sleeve to heat;
3) keeping the autoclave outlet at the bottom of the autoclave body closed, keeping part of the outlets of the plurality of pipelines of the tubular reactor open, and keeping the rest closed;
4) the mixed supercritical water and reaction materials enter a tubular reactor in a high-pressure kettle, and the materials which are shunted by a shunt move in parallel pipelines to generate supercritical hydrothermal synthesis reaction;
5) and after the reaction is finished, the reaction materials flow out of the plurality of parallel pipes and are collected into a main pipeline, and then the supercritical hydrothermal synthesis reaction is finished through temperature reduction treatment.
Preferably, a high-temperature high-pressure stop valve is arranged on a pipeline externally connected with an outlet of each pipeline of the tubular reactor, and the reaction time is adjusted by controlling the opening and closing of the high-temperature high-pressure stop valves; if the reaction time needs to be increased, the high-temperature and high-pressure stop valves in the open state are closed one by one, and if the reaction time needs to be reduced, the high-temperature and high-pressure stop valves in the closed state are opened one by one.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention discloses a supercritical hydrothermal synthesis reaction device coupled with an online ultrasonic crushing technology, which is characterized in that an ultrasonic transducer is fixed on a top cover of a high-pressure kettle, and a tubular reactor capable of generating supercritical hydrothermal synthesis reaction is effectively assembled in the kettle body of the high-pressure kettle, so that the combined assembly of the ultrasonic generator and the supercritical hydrothermal synthesis tubular reactor is realized, on one hand, ultrasonic reinforced particles can be crushed and dispersed in the supercritical hydrothermal synthesis reaction process to obtain a product with low particle size and high value, on the other hand, supercritical water in the high-pressure kettle can be simultaneously used as a heat preservation medium, the influence of heat dissipation of materials in the reactor on the product quality in the reaction process is prevented, and the product quality of preparing nano metal powder by adopting the supercritical hydrothermal synthesis technology is effectively improved. More importantly, because the reactor pipeline is arranged in the autoclave body, valves are difficult to be arranged at different length positions of the reactor pipeline to control the reaction time, and the adjustment of the flow of the main material can cause the change of the parameters of the whole system, and the product quality can not be ensured. Therefore, the invention effectively solves the problem that the traditional ultrasonic transducer can not be used on the outer surface of the high-temperature and superfine pipeline of the supercritical hydrothermal synthesis tubular reactor in a fitting way.
Furthermore, a high-temperature and high-pressure valve is arranged on an outlet pipeline of the parallel pipeline of the tubular reactor, and the total through-flow time is controlled by controlling the opening and closing of the high-temperature and high-pressure valve, so that the reaction time is controlled.
Furthermore, the heat preservation layer outside the heating jacket can reduce the heat loss of the reaction system and improve the effect of the environment temperature of the supercritical reaction.
Furthermore, the connection mode of the ultrasonic transducer and the autoclave top cover is flexible, and the ultrasonic transducer and the autoclave top cover can be effectively connected in a welding or bolt mode.
The method for carrying out the hydrothermal synthesis reaction based on the supercritical hydrothermal synthesis reaction device disclosed by the invention is simple to operate, easy to control the process, convenient to use and capable of controlling the total flow-through time by controlling the opening and closing of the valve, so that the reaction time is controlled, the reaction process is controllable, and the product quality is fully ensured.
Drawings
FIG. 1 is a supercritical hydrothermal synthesis reaction apparatus coupled with an on-line ultrasonic crushing technology according to the present invention;
wherein: 1-an ultrasonic transducer; 2-a top cover; 3-kettle body; 4-heating a jacket; 5-insulating layer; 6-a flow divider; 7-a tubular reactor; 8-autoclave outlet;
FIG. 2 is a schematic view of the opening of the autoclave head;
wherein, 21-thermowell entry; 22-a conduit outlet; 23-an interface; 24-a fastening bolt; 25-a pressure gauge lead pipe interface;
FIG. 3 is a flow chart illustrating a method of controlling reaction time.
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.
Referring to fig. 1, a supercritical hydrothermal synthesis reaction apparatus coupled with an online ultrasonic crushing technology comprises an ultrasonic transducer 1, an autoclave and a tubular reactor 7;
the tubular reactor 7 is arranged in the autoclave body 3, the ultrasonic transducer 1 is fixedly connected to the top cover 2 of the autoclave, and the heating sleeve 4 is arranged outside the autoclave body 3;
an inlet of the tubular reactor 7 and a plurality of pipeline outlets of the tubular reactor 7 are arranged on the top cover 2, and an autoclave outlet 8 is arranged at the bottom of the autoclave body 3;
the inlet pipeline of the tubular reactor 7 extending into the kettle body 3 is provided with a flow divider 6, and the inlet pipeline is branched into a plurality of parallel pipelines through the flow divider 6, so that the fluid entering into the kettle body 3 can be averagely divided into a plurality of strands of parallel fluid.
Preferably, the plurality of parallel pipelines have the same size, and the pipelines immersed in the kettle body 3 have the same length, so that the uniform distribution of the materials is ensured. The pipeline externally connected with the outlet of each pipeline of the tubular reactor 7 is provided with a high-temperature high-pressure stop valve, such as V1, V2, V3, V4, V5 and V6 in figure 3. Therefore, the circulation condition of the reaction materials in a specific certain parallel pipeline in the kettle body 3 can be controlled by controlling the opening and closing of the high-temperature high-pressure stop valve, so that the overall material through flow is controlled to adjust the reaction time.
An ultrasonic transducer interface is further arranged on the top cover 2, and the ultrasonic transducer 1 is welded or bolted to the top cover 2 through the ultrasonic transducer interface.
The heating jacket 4 adopts a silicon-molybdenum rod heating or electric furnace wire heating mode.
And a heat-insulating layer 5 is arranged on the outer side surface of the heating sleeve 4.
The bottom of the kettle body 3 is provided with a high-pressure kettle outlet 8, a guide pipe is welded outside the high-pressure kettle outlet 8, the guide pipe extends out of the heat preservation layer 5, and a valve is arranged on the guide pipe.
Referring to fig. 2, the autoclave top cover is provided with a thermowell inlet 21, a tubular reactor branch pipeline outlet 22, an ultrasonic transducer interface 23, a fastening bolt 24 and a pressure gauge lead pipe interface 25.
The number of the branch pipe outlets 22 of the tubular reactor is determined according to the parallel pipes branched by the tubular reactor 7, and the specific number is determined according to actual requirements.
The fastening bolts 24 are used for fixing the autoclave body 3 and the top cover 2, and the number of the fastening bolts is not particularly required, so that the fastening bolts are used for fastening the autoclave body 3 and the top cover 2.
The following describes a method for performing supercritical hydrothermal synthesis reaction by using a supercritical hydrothermal synthesis reaction apparatus based on the coupled online ultrasonic fragmentation technology of the present invention by using specific application examples. The reaction temperature and pressure parameters of the supercritical hydrothermal synthesis reaction are assumed to be 400 ℃ and 28MPa, the normal mixed fluid flow of the system is 30L/h, and the rated reaction time is 20 s. The effective volume of the autoclave was 2L. The reaction comprises the following steps:
1) theoretical calculation and Aspen plus simulation are carried out according to physical properties, the charging amount of the reaction kettle is 519mL, and the environmental pressure of 28MPa can be reached when the temperature of supercritical water in the high-pressure kettle (the supercritical water is added into the high-pressure kettle in advance) is 400 ℃. The autoclave was opened, charged, resealed, set to a target temperature of 400 ℃ and heat was initiated.
2) The vent at the bottom end of the autoclave was kept closed. And opening valves V1-V4 after parallel pipelines of the reactor, and keeping V5 and V6 in a closed state.
3) After materials and supercritical water are mixed in a mixer, the mixture enters the high-pressure kettle, and fluid is uniformly distributed in the flow divider.
4) The material flow after being divided moves in the parallel pipelines of the tubular reactor to generate hydrothermal synthesis reaction.
5) The reaction time is adjusted by opening and closing a valve after the parallel pipelines of the reactor:
a) the reaction time is increased: v5 is opened.
b) The reaction time continues to increase: v5 and V6 are opened.
c) The reaction time is reduced: v4, V5 and V6 are closed.
d) The reaction time continues to decrease: v3, V4, V5, V6 are closed.
6) The reacted materials flow to a uniform collecting pipe and then enter a cooler for cooling, thereby finishing the hydrothermal synthesis reaction.
Claims (9)
1. A supercritical hydrothermal synthesis reaction device coupled with an online ultrasonic crushing technology is characterized by comprising an ultrasonic transducer (1), a high-pressure kettle and a tubular reactor (7);
the tubular reactor (7) is arranged in the autoclave body (3), the ultrasonic transducer (1) is fixedly connected on the top cover (2) of the autoclave, and the heating sleeve (4) is arranged outside the autoclave body (3);
an inlet of the tubular reactor (7) and a plurality of pipeline outlets (22) of the tubular reactor (7) are arranged on the top cover (2), and an autoclave outlet (8) is arranged at the bottom of the autoclave body (3); a high-temperature high-pressure stop valve is arranged on a pipeline externally connected with each pipeline outlet (22) of the tubular reactor (7);
the inlet pipeline of the tubular reactor (7) extending into the kettle body (3) is provided with a flow divider (6), the inlet pipeline is branched into a plurality of parallel pipelines through the flow divider (6), the fluid entering into the kettle body (3) can be averagely divided into a plurality of strands of parallel fluid, and the tail ends of the parallel pipelines are connected to a pipeline outlet (22).
2. The supercritical hydrothermal synthesis reaction apparatus coupled with an online ultrasonic crushing technology as recited in claim 1, wherein the plurality of parallel pipes have the same size, and the pipes immersed in the tank (3) have the same length.
3. The supercritical hydrothermal synthesis reaction device coupled with the online ultrasonic crushing technology according to claim 1, wherein the heating jacket (4) adopts a silicon-molybdenum rod or an electric furnace wire.
4. The supercritical hydrothermal synthesis reaction device coupled with the online ultrasonic crushing technology according to claim 1, characterized in that an insulating layer (5) is arranged outside the heating jacket (4).
5. The supercritical hydrothermal synthesis reaction device coupled with the online ultrasonic crushing technology according to claim 4, wherein a bottom outlet (26) is formed at the bottom of the heat-insulating layer (5), a guide pipe capable of extending out of the bottom outlet (26) is externally connected to the autoclave outlet (8), and a valve is arranged on the guide pipe.
6. The supercritical hydrothermal synthesis reaction apparatus coupled with an online ultrasonic crushing technology according to any one of claims 1 to 5, characterized in that an interface (23) shared by the ultrasonic transducer (1) and the tubular reactor (7) is further provided on the top cover (2), and the ultrasonic transducer (1) is welded or bolted to the top cover (2) through the interface (23).
7. The supercritical hydrothermal synthesis reaction apparatus coupled with online ultrasonic crushing technology according to claim 1, characterized in that a thermowell inlet (21) for inserting a thermocouple and a pressure gauge lead pipe interface (25) for inserting a pressure gauge are further provided on the top cover (2).
8. The supercritical hydrothermal synthesis reaction method by using the supercritical hydrothermal synthesis reaction apparatus coupled with the on-line ultrasonic crushing technology in claim 1 is characterized by comprising the following steps:
1) obtaining the feeding amount of reactants in the autoclave through theoretical calculation and Aspenplus simulation according to physical properties;
2) opening the top cover (2), feeding according to the feeding amount obtained in the step (1), then reinstalling the top cover (2), setting the required heating temperature, and starting the heating sleeve (4) for heating;
3) keeping a high-pressure kettle outlet (8) at the bottom of the kettle body (3) closed, keeping part of a plurality of pipeline outlets of the tubular reactor (7) open, and keeping the rest closed;
4) the mixed supercritical water and reaction materials enter a tubular reactor (7) in a high-pressure kettle, and the materials which are divided by a flow divider (6) move in parallel pipelines to generate supercritical hydrothermal synthesis reaction;
5) and after the reaction is finished, the reaction materials flow out of the plurality of parallel pipes and are collected into a main pipeline, and then the supercritical hydrothermal synthesis reaction is finished through temperature reduction treatment.
9. The supercritical hydrothermal synthesis reaction method according to claim 8, wherein the reaction time is adjusted by controlling the opening and closing of the high-temperature high-pressure stop valve; if the reaction time needs to be increased, the high-temperature and high-pressure stop valves in the open state are closed one by one, and if the reaction time needs to be reduced, the high-temperature and high-pressure stop valves in the closed state are opened one by one.
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| CN111514832A (en) * | 2020-05-30 | 2020-08-11 | 侯梦斌 | Hydrothermal carbonization equipment and process for intervening in micro-interface strengthening reaction |
| CN113769677B (en) * | 2021-10-22 | 2022-10-28 | 西安交通大学 | Integrated micro-channel supercritical hydrothermal synthesis reactor capable of realizing accurate control of reaction time |
| CN113813898B (en) * | 2021-10-22 | 2022-10-28 | 西安交通大学 | Combined supercritical hydrothermal synthesis microchannel reactor |
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