CN111774019A - High-temperature high-pressure visual hydrothermal device - Google Patents
High-temperature high-pressure visual hydrothermal device Download PDFInfo
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- CN111774019A CN111774019A CN202010639586.1A CN202010639586A CN111774019A CN 111774019 A CN111774019 A CN 111774019A CN 202010639586 A CN202010639586 A CN 202010639586A CN 111774019 A CN111774019 A CN 111774019A
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/12—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of critical point; of other phase change
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/14—Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation
- G01N25/145—Accessories, e.g. cooling devices
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/14—Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation
- G01N25/147—Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation by cristallisation
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Abstract
The utility model provides a visual hydrothermal device of high temperature high pressure, includes the heating furnace, and vertical quartz tube reactor sets up in the heating furnace through the test-tube rack, and the heating furnace lower part is provided with window and the light inlet of wait for the same height, is provided with the light source before the light inlet, is provided with camera or analytical instrument before the window, and the visual angle direction of window is perpendicular with the light inlet direction of light inlet. The invention can observe the phase equilibrium rule and the crystallization characteristic of the salt solution under high temperature and high pressure on line, solves the problems of difficult capture of inorganic salt behavior phenomenon, difficult sampling and testing of crystal particles and the like under the supercritical condition of high temperature and high pressure, realizes the on-line observation of the phase behavior and the crystal evolution process of the inorganic salt under the supercritical water condition, can intuitively master the behavior rule of the inorganic salt, obtains the structural property and the phase equilibrium behavior of the crystal particles of the inorganic salt, finally solves the problems of inorganic salt deposition and blockage of the SCWO/SCWG technology, realizes the safe, long-term and stable operation of the system, and improves the economical efficiency and the safety of the system.
Description
Technical Field
The invention belongs to the technical field of energy, environment and chemical industry, and particularly relates to a high-temperature high-pressure visual hydrothermal device.
Background
Supercritical Water (SCW) is Water in a special state with temperature and pressure greater than its critical point (T: 374.15 ℃, P: 22.12 MPa). In this state, only a small amount of hydrogen bonds exist in water, the dielectric constant is similar to that of an organic solvent, and the water has a low viscosity and a high diffusion coefficient. Organic matter and oxygen can be mutually dissolved with supercritical water according to any proportion, so that heterogeneous reaction is changed into homogeneous reaction, and mass transfer and heat transfer resistance among substances is greatly reduced.
Supercritical Water Oxidation (SCWO) utilizes the special properties of Water in a Supercritical state to enable organic matters and an oxidant to rapidly generate an Oxidation reaction in Supercritical Water to thoroughly decompose the organic matters. The supercritical water oxidation technology has wide application range, can treat various industrial organic wastewater and wastes, municipal sewage, excessive activated sludge of sewage treatment plants and human metabolic sewage, eliminates toxicants of chemical weapons and the like, and has good environmental protection benefit, social benefit and economic benefit. Meanwhile, the method has the advantages of extremely high reaction speed, high removal rate, no secondary pollution, low energy consumption, easy separation and recovery of products and the like. The technology is carried out in an environment with high temperature, high pressure and high oxygen concentration, and the harsh conditions are easy to cause corrosion to equipment and form salt precipitates in the equipment. The corrosion not only reduces the service life of the equipment, but also causes the reaction products to contain certain metal ions (such as chromium and the like) to influence the treatment effect of the supercritical water oxidation technology. Deposited solid salts form agglomerates to cover the surface of equipment, so that the heat exchange rate is reduced, the system pressure is increased, the blockage of a reactor and a system pipeline can be caused in serious conditions, the supercritical water oxidation system cannot normally operate, and in addition, the wall surface covered by the agglomerates is often seriously corroded. Thus, in order to make this process economically practical, the bottleneck problems of corrosion and salt deposition must be solved.
Supercritical Water Gasification (SCWG) is a series of complex thermochemical reactions, such as pyrolysis, oxidation and reduction, to convert biomass into hydrogen by directly using Supercritical Water as a reaction medium and utilizing the special properties (small dielectric constant, small viscosity, large diffusion coefficient, strong solubility and the like) of Supercritical Water under the condition that the temperature and pressure are higher than critical values of Water. The main process comprises steam reforming reaction, water-gas shift reaction and methanation reaction. Compared with the traditional gasification method, the supercritical water gasification can directly treat wet materials, thereby reducing the production cost, and simultaneously has the characteristics of high reaction efficiency, high thermal efficiency and high hydrogen content. Inorganic salts, such as sodium sulfate, sodium chloride, are generally present in the reaction feed. In addition, a certain amount of inorganic salts is also produced during the gasification reaction or oxidation reaction of the heteroatom-containing organic substance. The inorganic salt not only affects the performance of the catalyst, but also when the temperature exceeds the critical value of water, the solubility of various inorganic salts in water is sharply reduced, the inorganic salts are easy to precipitate and crystallize in supercritical water and deposit on the surfaces of equipment and pipelines, the pressure drop of the system is increased, the heat transfer is deteriorated, the blockage of the equipment and the pipelines is caused, finally, the shutdown and the cleaning of the device are forced, and the continuous and stable operation of the device and the economical efficiency of the system are seriously affected. However, under severe high-temperature and high-pressure supercritical conditions, the phase behavior and the crystal evolution process of the inorganic salt in supercritical water are difficult to explore, and the behavior law cannot be predicted, so that an effective inorganic salt deposition prevention and control technology is developed.
Disclosure of Invention
In order to overcome the defects of the prior art and solve the problem that inorganic salt is easy to precipitate crystals in supercritical water and deposit on the surfaces of equipment and pipelines, the invention aims to provide a high-temperature high-pressure visual hydrothermal device which can observe the phase equilibrium rule and the crystallization characteristic of a salt solution under high temperature and high pressure on line, solve the problems of difficult capture of inorganic salt behavior phenomenon, difficult sampling and testing of crystal particles and the like under a high-temperature high-pressure supercritical condition, realize the on-line observation of the phase behavior and the crystal evolution process of the inorganic salt under the supercritical water condition, so that the behavior rule of the inorganic salt can be intuitively mastered, the structural property and the phase equilibrium behavior of inorganic salt crystal particles can be obtained, the development of a targeted prevention and control technology is carried out, the problems of inorganic salt deposition and blockage of the SCWO/SCWG technology are finally solved, and the safe, long-term and stable operation of a system is realized, the economy and the safety of the system are improved.
In order to achieve the purpose, the invention adopts the technical scheme that:
the utility model provides a visual hydrothermal device of high temperature high pressure, includes heating furnace 9, and vertical quartz tube reactor 2 sets up in heating furnace 9 through test-tube rack 6, its characterized in that, heating furnace 9 lower part is provided with equal high window 5 and advances light mouth 11, be provided with light source 12 before advancing light mouth 11, be provided with camera or analytical instrument before window 5, the visual angle direction of window 5 is perpendicular with the light direction that advances of light mouth 11.
The bottom end of the test tube rack 6 is a test tube rack support 10, the top end of the test tube rack is connected with a holder 8 outside a heating furnace 9, and the bottom of the quartz tube reactor 2 is positioned on the test tube rack support 10 and fixed on the test tube rack 6 through a test tube rack ring 4.
The holder 8 is fixedly connected with the test tube rack 6, and the test tube rack 6 is positioned in the center of the heating furnace 9.
The side surface of the quartz tube reactor 2 is tightly wrapped by thermal insulation cotton 3 to form a thermocouple I1.
The heat insulation cotton 3 is made of asbestos, aluminosilicate or aerogel, and the design thickness of the heat insulation cotton is determined by actual operation temperature calculation.
And a second thermocouple 7 is arranged in the heating furnace 9, and the probe of the second thermocouple 7 is equal to the bottom end of the quartz tube reactor 2 in height.
The window 5 and the light inlet 11 are both rectangular, and the lower ends of the window 5 and the light inlet 11 are both located 5-10 mm below the bottom end of the quartz tube reactor 2.
The window 5 and the light inlet 11 are sealed by embedding a large-size quartz plate with strong light transmittance into the heating furnace 9.
In the phase transition and crystal evolution process of the inorganic salt, light enters the light inlet 11 through the light source 12 and irradiates the quartz tube reactor 2, and an optical signal transmitted by the window 5 is recorded by a camera or a diffraction wave is emitted by an analysis instrument through the window 5 so as to carry out online analysis on the structure of the crystal particles.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention discloses a high-temperature high-pressure visual hydrothermal device which can observe the phase equilibrium rule and the crystallization characteristic of a salt solution under high temperature and high pressure on line, solves the problems of difficult capture of inorganic salt behavior phenomenon, difficult sampling and testing of crystallization particles and the like under a high-temperature high-pressure supercritical condition, realizes the on-line observation of the phase behavior and the crystallization evolution process of the inorganic salt under the supercritical water condition, can intuitively master the behavior rule of the inorganic salt, obtains the structural property and the phase equilibrium behavior of inorganic salt crystallization particles, develops a targeted prevention and control technology, finally solves the problems of inorganic salt deposition and blockage of an SCWO/SCWG technology, realizes the safe, long-term and stable operation of a system, and improves the economical efficiency and the safety of the system.
(2) Compared with the existing high-temperature high-pressure sapphire window reaction kettle, the device of the invention has greatly improved economy and safety.
Drawings
Fig. 1 is a schematic front view of a high-temperature high-pressure visual hydrothermal device of the invention.
Fig. 2 is a left side view schematic diagram of the high-temperature high-pressure visual hydrothermal device of the invention.
Fig. 3 is a schematic top view of a high-temperature high-pressure visual hydrothermal device of the present invention.
Wherein: 1 is a thermocouple I; 2 is a quartz tube reactor; 3 is heat preservation cotton; 4 is a test tube rack ring; 5 is a window; 6 is a test tube rack; 7 is a second thermocouple; 8 is a holder; 9 is a heating furnace; the 10 is the bottom of the test tube rack; 11 is a light inlet; and 12 is a light source.
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 should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. 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 fig. 1, 2 and 3, the invention is a high-temperature high-pressure visual hydrothermal device, which mainly comprises a heating furnace 9, a quartz tube reactor 2 and a test tube rack 6.
Wherein, the test tube rack 6 is positioned at the center in the heating furnace 9, the bottom end of the test tube rack is provided with a support bottom 10, and the top end of the test tube rack is fixedly connected with the holder 8 outside the heating furnace 9. The quartz tube reactor 2 is vertically arranged, the bottom of the quartz tube reactor is positioned on the support bottom 10 of the test tube rack, and the quartz tube reactor is fixed on the test tube rack 6 through the test tube rack circular ring 4.
The thermocouple I1 is tightly wrapped on the side face of the quartz tube reactor 2 through heat insulation cotton 3, the heat insulation cotton 3 is made of asbestos, aluminosilicate or aerogel, and the design thickness of the thermocouple I is determined by actual operation temperature calculation.
A second thermocouple 7 is arranged in the heating furnace 9, and the probe of the second thermocouple 7 is equal to the bottom end of the quartz tube reactor 2 in height.
The lower part of the heating furnace 9 is provided with a window 5 and a light inlet 11 which are equal in height, a light source 12 is arranged in front of the light inlet 11, a camera or an analysis instrument is arranged in front of the window 5, and the visual angle direction of the window 5 is vertical to the light inlet direction of the light inlet 11.
In this embodiment, the window 5 and the light inlet 11 are both rectangular, and the lower ends thereof are both located 5-10 mm below the bottom end of the quartz tube reactor 2. The window 5 and the light inlet 11 are sealed by embedding a large quartz plate into the heating furnace 9, and the quartz plate with strong light transmittance is selected.
In the phase transition and crystal evolution process of the inorganic salt, light enters the light inlet 11 through the light source 12 and irradiates the quartz tube reactor 2, and an optical signal transmitted by the window 5 is recorded by a camera or a diffraction wave is emitted by an analysis instrument through the window 5 so as to carry out online analysis on the structure of the crystal particles.
According to the structure, the use mode of the invention is as follows:
the method comprises the steps of adding a salt solution into a quartz tube reactor 2, heating the open end of the quartz tube reactor 2 by using high-temperature flame, sealing the opening after melting, fixing the quartz tube reactor 2 on a test tube rack 6 through a test tube rack circular ring 4 and a test tube rack support bottom 10, heating a furnace 9 for heating the salt solution inside the quartz tube reactor 2, gradually increasing the temperature of the salt solution inside the quartz tube reactor 2, and generating bubbles, reducing the liquid level, disappearing the liquid phase, salting out crystals, depositing the crystals on the wall surface of the quartz tube reactor 2 and other phase change phenomena on the salt solution. During the operation of the device, the first thermocouple 1 and the second thermocouple 7 positioned in the heating furnace 9 respectively measure the temperature in the quartz tube reactor 2 and the temperature in the heating furnace 9 in real time, and are used for accurately reacting the temperature of the salt solution and the temperature of the heating furnace; in the phase change and crystal evolution process of the inorganic salt, a light source 12 is turned on to be aligned to the quartz tube reactor 2, a video recorder is turned on to record the whole process, and the whole process is transmitted to a computer; or starting an analytical instrument and the like to perform online test of salt solution crystallization phase change.
In the invention, under the high-temperature and high-pressure condition of sub/supercritical water, the salt solution is sealed in the quartz tube reactor, the quartz tube is arranged in the heating furnace, the heating furnace is started to continuously raise the temperature of the salt solution in the quartz tube, and the temperature of the inner pressure of the quartz tube is raised along with the temperature rise because the quartz tube reactor is sealed to have equal volume, so that the target temperature and pressure condition is finally reached.
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 visual hydrothermal device of high temperature high pressure, includes heating furnace (9), and vertical quartz tube reactor (2) sets up in heating furnace (9) through test-tube rack (6), its characterized in that, heating furnace (9) lower part is provided with window (5) and light inlet (11) of constant height, be provided with light source (12) before light inlet (11), be provided with camera or analytical instrument before window (5), the visual angle direction of window (5) is perpendicular with the light inlet direction of light inlet (11).
2. The high-temperature high-pressure visual hydrothermal device according to claim 1, wherein the bottom end of the test tube rack (6) is a rack support (10), the top end of the test tube rack is connected with a holder (8) outside the heating furnace (9), the bottom of the quartz tube reactor (2) is positioned on the rack support (10), and the quartz tube reactor is fixed on the test tube rack (6) through a rack ring (4).
3. The hydrothermal device for visualization at high temperature and high pressure according to claim 2, wherein the holder (8) is fixedly connected with a test tube rack (6), and the test tube rack (6) is centrally located in the heating furnace (9).
4. The high-temperature high-pressure visual hydrothermal device according to claim 1, wherein the side of the quartz tube reactor (2) is tightly wrapped by thermal insulation cotton (3) to form a thermocouple I (1).
5. The high-temperature high-pressure visualization hydrothermal device according to claim 4, characterized in that the thermal insulation cotton (3) is made of asbestos, aluminosilicate or aerogel, and the design thickness is determined by actual operation temperature calculation.
6. A high-temperature high-pressure visual hydrothermal device according to claim 1, 4 or 5, characterized in that a second thermocouple (7) is arranged in the heating furnace (9), and the probe of the second thermocouple (7) is as high as the bottom end of the quartz tube reactor (2).
7. The high-temperature high-pressure visual hydrothermal device according to claim 1, wherein the window (5) and the light inlet (11) are both rectangular, and the lower ends of the window (5) and the light inlet (11) are both located 5-10 mm below the bottom end of the quartz tube reactor (2).
8. The hydrothermal device for visualization at high temperature and high pressure as defined in claim 1 or 7, wherein the window (5) and the light inlet (11) are sealed by a large-sized quartz plate with high light transmittance embedded in the heating furnace (9).
9. A high-temperature high-pressure visual hydrothermal device according to claim 1, characterized in that during the phase transition and crystal evolution of inorganic salts, light enters the light inlet (11) through the light source (12) and irradiates on the quartz tube reactor (2), and the optical signal transmitted through the window (5) is recorded by a camera, or the diffraction wave is emitted through the window (5) by an analytical instrument to perform on-line analysis of the crystal grain structure.
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| CN202010639586.1A CN111774019B (en) | 2020-07-06 | 2020-07-06 | High-temperature high-pressure visual hydrothermal device |
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| CN202010639586.1A CN111774019B (en) | 2020-07-06 | 2020-07-06 | High-temperature high-pressure visual hydrothermal device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115824895A (en) * | 2022-11-07 | 2023-03-21 | 中国核动力研究设计院 | Visual test device and method for dynamic bubble adhesion measurement and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115824895A (en) * | 2022-11-07 | 2023-03-21 | 中国核动力研究设计院 | Visual test device and method for dynamic bubble adhesion measurement and application |
| CN115824895B (en) * | 2022-11-07 | 2024-01-30 | 中国核动力研究设计院 | Visual test device and method for measuring dynamic bubble adhesion force and application |
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