CN111781108A - System and method for testing crystallization-deposition of inorganic salt in subcritical/supercritical water - Google Patents
System and method for testing crystallization-deposition of inorganic salt in subcritical/supercritical water Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N15/04—Investigating sedimentation of particle suspensions
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/02—Devices for withdrawing samples
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Abstract
An inorganic salt crystallization-deposition test system in subcritical/supercritical water, comprising: the preheating unit is used for respectively preheating water and the salt solution; the testing unit comprises a high-pressure reaction kettle with a built-in coil, preheated water is connected with an inlet of the coil, a preheated salt solution is connected with the inlet of the high-pressure reaction kettle, the inlet of the high-pressure reaction kettle is arranged on a kettle cover, a sample block is arranged at the tail end of the inlet in the high-pressure reaction kettle, a stirrer and a thermometer sleeve are further arranged in the high-pressure reaction kettle, and an outlet and a pressure gauge interface of the high-pressure reaction kettle are further arranged on the kettle cover; and the post-reaction treatment unit comprises a salt solution filtering, cooling and pressure-reducing sampling pipeline connected with the outlet of the high-pressure reaction kettle and a water cooling and pressure-reducing pipeline connected with the outlet of the coil pipe. The invention also provides a testing method based on the system, which can collect salt crystallized particle samples on line and test inorganic salt crystallization deposition rules under different wall surface temperatures and different turbulence degrees, so as to master the behavior rules and solve the problem of salt deposition in subcritical/supercritical water oxidation.
Description
Technical Field
The invention belongs to the technical field of energy, chemical industry and environmental protection, and particularly relates to a crystallization-deposition test system and method for inorganic salt in subcritical/supercritical water.
Background
The supercritical water oxidation treatment range is wide, and waste almost containing organic matters can be treated by adopting the technology. The technology has mature and excellent technical effects in the aspects of phenolic compounds, polychlorinated biphenyl organic matters, pesticides, fuel intermediate aniline, sludge treatment, supercritical water oxidation treatment of pollutants such as human metabolites and the like. From the perspective of sustainable development of the environment and industrial development, the supercritical water oxidation technology is a new green and environment-friendly technology with a great prospect.
The supercritical water oxidation treatment technology has the following unique advantages:
1. the reaction speed is very fast, and the removal rate is high. In the supercritical water oxidation process, organic matters and air (or oxygen) can be mutually dissolved in the supercritical water, interphase interfaces disappear, the diffusion coefficient is 10-100 times that of common liquid water, and the heat and mass transfer rate is high, so that the reaction rate is very high, and the removal rate of most of the organic matters can reach more than 99.99 percent within short retention time (from a few seconds to a few minutes).
2. No secondary pollution. The hydrocarbons may eventually be oxidized to CO2And H2O, nitrogen in organic waste is oxidized into N2And N2O and the like; hetero atoms such as sulfur, chlorine, phosphorus and the like are respectively converted into corresponding inorganic acids (such as sulfate radicals, hydrochloric acid radicals and phosphate radicals) and are neutralized with alkali liquor to form corresponding inorganic salts; the cation forms an oxide or combines with acid radical ions to generate inorganic salt. Does not generate any pollution gas, thoroughly degrades and removes toxic wastes and pathogens to meet the requirement of harmless treatment. Several researchers have investigated the possibility of oxidative degradation of a range of toxic substances including dioxins, polychlorinated biphenyls, cyanides, phenols, etc. in supercritical water.
3. The energy consumption is low. When the mass fraction of the organic matters in the wastewater is more than 2-5%, the heat balance required by the reaction can be maintained by means of the reaction heat released in the reaction process, and an external heat source or fuel is not needed; when the content of organic matters in the wastewater is higher, heat can be supplied to the outside of the system.
4. The product is easy to separate and recover. Inorganic salts and metal oxides have low solubility in supercritical water, and when organic wastes are treated by supercritical water oxidation, the inorganic salts and metal oxides are often precipitated in the form of crystals, are easily separated in the form of solids, and can be recycled. After the reaction product is cooled and depressurized, CO can be directly recovered2And sale, low cost CO2Certain economic benefit is obtained while trapping.
However, the technology is carried out in an environment with high temperature, high pressure and high oxygen concentration, and the harsh conditions are easy to form salt precipitates in equipment. 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. Therefore, in order to make the process economical, the technical problem of salt deposition is to be solved.
At present, the basic method for solving the problem of reactor blockage caused by salt deposition is to adopt a special operation technology and a special reactor structure, and specifically comprises the steps of adopting a mechanical brush, a rotary scraper, filtering, an additive, high flow rate, homogeneous deposition, extreme high pressure, a counter-current kettle type reactor, an evaporation wall type reactor, a counter-current kettle type evaporation wall reactor, a counter-current tube type reactor, a cold wall reactor, a centrifugal reactor and the like. However, the existing methods for solving the salt deposition all have respective disadvantages, and no structural design or operation technology has obvious advantages. The main reason is that under the severe condition of high-temperature and high-pressure supercritical water, the crystallization and deposition characteristics of inorganic salt are difficult to probe, so that the behavior rule can not be mastered, and the medicine can not be applied according to the symptoms.
Disclosure of Invention
In order to overcome the defects of the prior art and explore the crystallization and deposition characteristics of inorganic salts, the invention aims to provide a crystallization and deposition test system and a crystallization and deposition test method for inorganic salts in subcritical/supercritical water, which can test the crystallization and deposition rules of the inorganic salts at different wall temperatures and different turbulence degrees and further master the behavior rules, thereby solving the problem of salt deposition in subcritical/supercritical water oxidation.
In order to achieve the purpose, the invention adopts the technical scheme that:
an inorganic salt crystallization-deposition test system in subcritical/supercritical water, comprising:
the preheating unit is used for respectively preheating water and the salt solution;
the testing unit comprises a high-pressure reaction kettle 7 with a built-in coil 73, preheated water is connected with an inlet of the coil 73, a preheated salt solution is connected with an inlet 71 of the high-pressure reaction kettle, the inlet 71 of the high-pressure reaction kettle is opened on a kettle cover of the high-pressure reaction kettle 7, a sample block 72 is arranged at the tail end of the inlet 71 of the high-pressure reaction kettle 7, a stirrer 77 and a thermometer sleeve 74 for installing a thermometer are also arranged in the high-pressure reaction kettle 7, and a high-pressure reaction kettle outlet 76 and a pressure gauge interface 75 for installing a pressure gauge are also arranged on the kettle cover;
and the post-reaction treatment unit comprises a salt solution filtering, cooling and pressure reduction sampling pipeline connected with the outlet 76 of the high-pressure reaction kettle and a water cooling and pressure reduction pipeline connected with the outlet of the coil 73.
The preheating unit comprises a water storage tank 1, a water pump 2, a first preheater 3, a salt solution tank 4, a salt solution pump 5 and a second preheater 6, wherein an outlet of the water storage tank 1 is connected with an inlet of the water pump 2, an outlet of the water pump 2 is connected with an inlet of the first preheater 3, an outlet of the salt solution tank 4 is connected with an inlet of the salt solution pump 5, and an outlet of the salt solution pump 5 is connected with an inlet of the second preheater 6;
in the flow direction, a filter 8, a second cooler 11, a second back pressure valve V6, a collection tank 12 and a sampling bottle 13 which are connected in parallel are sequentially arranged on the saline solution filtering, cooling and depressurizing sampling pipeline; and a first cooler 9, a first back pressure valve V5 and a waste liquid tank 10 are sequentially arranged on the water cooling pressure reducing pipeline.
A second stop valve V2 is arranged between the second preheater 6 and the high-pressure reaction kettle inlet 71, and a fourth stop valve V4 is arranged between the filter 8 and the second cooler 11.
A bypass is arranged between the second cooler 11 and the preheated salt solution, the inlet of the bypass is positioned in front of the second stop valve V2, the outlet of the bypass is positioned behind the fourth stop valve V4, a first stop valve V1 and a third stop valve V3 are arranged on the bypass, the first stop valve V1 is close to the second preheater 6, and the third stop valve V3 is close to the second cooler 11.
A stop valve five V7 is arranged between the back pressure valve two V6 and the collecting tank 12, a branch is arranged in front of the stop valve five V7, and a stop valve six V8 and the sampling tank 13 are sequentially arranged on the branch.
The high-pressure reaction kettle inlet 71 is positioned at the top of the kettle cover, the tail end of the high-pressure reaction kettle inlet is positioned at the bottom of the kettle cover, the high-pressure reaction kettle outlet 76 is positioned at the bottom of the high-pressure reaction kettle, a thermometer is arranged in the thermometer sleeve 74, the pressure gauge connector 75 is connected with a pressure gauge, and the stirrer 77 is positioned at the axis of the kettle body and penetrates through the whole kettle body.
The coil 73 is arranged on a kettle cover of the high-pressure reaction kettle 7, the axis of the coil is coaxial with the high-pressure reaction kettle 7, and the inlet and the outlet of the coil penetrate through the kettle cover and are respectively connected with the first preheater 3 and the first cooler 9.
The first preheater 3 and the second preheater 6 are tubular electric heating devices, the first cooler 9 and the second cooler 11 are spiral coil type or tube type heat exchangers, and the water pump 2 and the saline solution pump 5 are high-pressure metering pumps.
The invention also provides a test method based on the crystallization-deposition test system of the inorganic salt in the sub-supercritical water, which comprises the following steps:
step 1, boosting the saline solution in a saline solution tank 4 through a saline solution pump 5, pumping the saline solution into a second preheater 6 for preheating, and then flowing into a high-pressure reaction kettle 7 through a high-pressure reaction kettle inlet 71;
step 4, allowing the salt solution obtained in the step 3 to flow out of the high-pressure reaction kettle 7, filtering by a filter 8, cooling in a second cooler 11, reducing the pressure in a second backpressure valve V6, and then allowing the salt solution to enter a sampling bottle 13 for sampling test or flowing into a collection tank 12;
step 5, water in the coil 73 in the step 2 flows into a cooler I9 for cooling, enters a backpressure valve I V5 for pressure reduction, and then enters a waste liquid tank 10;
and 6, after the experiment is finished, temporarily closing the salt solution pump 5, the first preheater 3 and the second preheater 6, closing the second stop valve V2, gradually and slowly screwing the second back pressure valve V6, performing pressure relief operation on the high-pressure reaction kettle 7, closing the fourth stop valve V4 after all the salt solution flows out of the high-pressure reaction kettle 7 in the step 4, opening the first stop valve V1 and the third stop valve V3, restarting the salt solution pump 5, continuously pumping a cold salt solution cooling pipeline into the pipeline, and stopping when the temperature is reduced to below 80 ℃.
Compared with the prior art, the invention has the beneficial effects that:
(1) the sample block is arranged to allow the solution to be sprayed on the surface to form crystal deposition particles and to facilitate the collection of samples for subsequent test analysis.
(2) The arrangement of the coil pipe controls the temperature of the cold/hot wall surface of the coil pipe by adjusting the temperature of water, can be used for testing the crystallization and deposition characteristics of inorganic salt under different wall surface temperature conditions, and collects samples for subsequent test and analysis.
(3) The setting of agitator can test inorganic salt crystallization deposit law under the different degree of turbulence.
(4) The setting of sampling bottle is used for collecting the solution sample on line, and the setting of bypass is used for after the experiment the reation kettle pressure release in order to collect salt crystallization in the cauldron, deposit sample (if not the direct normal cooling of pressure release, salt deposit granule can be redissolved in water) and cool down the system, can guarantee the safe operation of system.
Drawings
FIG. 1 is a schematic structural diagram of a crystallization-deposition test system for inorganic salts in sub-supercritical water according to the present invention.
Wherein, 1 is a water storage tank; 2 is a water pump; 3 is a preheater I; 4 is a salt solution tank; 5 is a salt solution pump; 6 is a second preheater; 7 is a high-pressure reaction kettle; 71 is an inlet of the high-pressure reaction kettle; 72 is a sample block; 73 is a coil pipe; 74 is a thermo-well tube; 75 is a pressure tap; 76 is an outlet of the high-pressure reaction kettle; 77 is a stirrer; 8 is a filter; 9 is a cooler I; 10 is a waste liquid tank; a second cooler 11; 12 is a collecting tank; 13 is a sampling bottle; v1 is a first stop valve; v2 is a stop valve II; v3 is a stop valve III; v4 is stop valve IV; v5 is a first backpressure valve; v6 is back pressure valve II; v7 is stop valve V; v8 is stop valve six.
Detailed Description
The embodiments of the present invention will be described in detail below with reference to the drawings and examples.
The present invention is further described in detail below with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Referring to fig. 1, the whole system of the crystallization-deposition test system of inorganic salts in sub-supercritical water of the present invention comprises a preheating unit, a test unit, and a post-reaction treatment unit, wherein:
the preheating unit is mainly used for respectively preheating water and saline solution and can realize pressurization. In this embodiment, it includes two 6 of water storage tank 1, water pump 2, preheater 3, salt solution jar 4, salt solution pump 5 and preheater, and 1 export of water storage tank links to each other with 2 entrances of water pump, and 2 exports of water pump link to each other with 3 entrances of preheater, and 4 exports of salt solution jar link to each other with 5 entrances of salt solution pump, and 5 exports of salt solution pump and two 6 entrances of preheater link to each other.
The test unit is used for completing reaction tests. In this embodiment, the apparatus mainly includes a high-pressure reaction kettle 7, a sample block 72, a coil 73, a thermo-well tube 74, a pressure interface 75 and a stirrer 77, wherein the pressure interface 75 is located on the kettle cover and connected to a pressure gauge. The thermometer sleeve 74, the coil 73 and the stirrer 77 are all positioned in the high-pressure reaction kettle 7, a thermometer is arranged in the thermometer sleeve 74, the stirrer 77 is positioned at the axis position of the kettle body and penetrates through the whole kettle body, the initial end of the high-pressure reaction kettle inlet 71 is positioned at the top of the kettle cover, the tail end of the high-pressure reaction kettle inlet 71 is positioned at the bottom of the kettle cover, the outlet of the second preheater 6 is connected with the initial end of the high-pressure reaction kettle inlet 71, a second stop valve V2 is arranged between the outlet of the second preheater 6 and the initial end of the high-pressure reaction kettle inlet 71, the sample block 72 is arranged at the. The coil pipe 73 is arranged on the kettle cover, the axis of the coil pipe is coaxial with the high-pressure reaction kettle 7, and the inlet and the outlet of the coil pipe penetrate through the kettle cover and are respectively connected with the first preheater 3 and the first cooler 9.
The post-reaction treatment unit is used for finishing the treatment and sampling of the reacted materials and mainly comprises a salt solution filtering, cooling and pressure-reducing sampling pipeline connected with the outlet 76 of the high-pressure reaction kettle and a water cooling and pressure-reducing pipeline connected with the outlet of the coil 73. In the embodiment, a salt solution filtering, cooling and depressurizing sampling pipeline is sequentially provided with a filter 8, a second cooler 11, a second back pressure valve V6, a collecting tank 12 and a sampling bottle 13 which are connected in parallel; a first cooler 9, a first backpressure valve V5 and a waste liquid tank 10 are sequentially arranged on the water cooling pressure reducing pipeline, an outlet of a coil 73 is connected with a first cooler 9 inlet, a first cooler 9 outlet is connected with a first backpressure valve V5 inlet, a first backpressure valve V5 outlet is connected with a waste liquid tank 10 inlet, an outlet 76 of the high-pressure reaction kettle is connected with an inlet of a filter 8, an outlet of the filter 8 is connected with a second cooler 11 inlet, a four-V4 stop valve is arranged between the outlet of the filter 8 and the second cooler 11 inlet, a second cooler 11 outlet is connected with a second backpressure valve V6 inlet, and a second backpressure valve V6 outlet is connected with a collection tank 12 or a sampling bottle 13 inlet. More specifically, a stop valve five V7 is arranged between the back pressure valve two V6 and the collecting tank 12, a branch is arranged in front of the stop valve five V7, and a stop valve six V8 and the sampling tank 13 are arranged on the branch in sequence
In this embodiment, a bypass is provided between the second preheater 6 and the second cooler 11, an inlet of the bypass is located before the second stop valve V2, an outlet of the bypass is located after the fourth stop valve V4, the bypass is provided with the first stop valve V1 and the third stop valve V3, the first stop valve V1 is close to the second preheater 6, and the third stop valve V3 is close to the second cooler 11.
In this embodiment, the first preheater 3 and the second preheater 6 may be tube-type electric heating, the first cooler 9 and the second cooler 11 may be shell-and-tube-type heat exchangers such as a spiral coil tube type or a tube array type, and the water pump 2 and the salt solution pump 5 may be high-pressure metering pumps, and may be plunger-type metering pumps or diaphragm-type metering pumps.
Based on the crystallization-deposition test system for the inorganic salt in the sub-supercritical water, the crystallization-deposition test method for the inorganic salt in the sub-supercritical water comprises the following steps:
step 1), boosting the saline solution in a saline solution tank 4 through a saline solution pump 5, pumping the saline solution into a second preheater 6 for preheating, and then flowing into a high-pressure reaction kettle 7 through a high-pressure reaction kettle inlet 71;
step 2), boosting water in the water storage tank 1 through a water pump 2, pumping the water into a preheater I3 for preheating, and then flowing the water into a coil 73 to form a cold wall or a hot wall with controllable temperature for the salt solution in the step 1);
step 3), the salt solution after pressurization and temperature rise in the step 1) reaches a subcritical or supercritical state, and flows out from an inlet 71 of the high-pressure reaction kettle and is sprayed on a sample block 72 for crystallization or deposition; the salt solution in the high-pressure reaction kettle 7 simultaneously generates different inorganic salt crystallization and deposition processes on the surface of the coil 73 under the influence of the cold wall or the hot wall, and forms crystallization and deposition particles; during this process, the agitator 77 may also be activated to create turbulent turbulence to the saline solution;
step 4), the salt solution obtained in the step 3) flows out of the high-pressure reaction kettle 7, is filtered by a filter 8 and then enters a second cooler 11 for cooling, then enters a second backpressure valve V6 for pressure reduction, and then enters a sampling bottle 13 for sampling test or flows into a collecting tank 12;
step 5) and step 2), the water in the coil 73 flows into a cooler I9 for cooling, enters a backpressure valve I V5 for pressure reduction, and then enters a waste liquid tank 10;
step 6), after the experiment, temporarily closing the salt solution pump 5, the first preheater 3 and the second preheater 6, closing the second stop valve V2, gradually and slowly screwing the second back pressure valve V6, performing pressure relief operation on the high-pressure reaction kettle 7, closing the fourth stop valve V4 after all the salt solution in the step 4) flows out of the high-pressure reaction kettle 7, opening the first stop valve V1 and the third stop valve V3, restarting the salt solution pump 5, continuously pumping a cold salt solution cooling pipeline into the pipeline, and stopping when the temperature is reduced to below 80 ℃.
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 (10)
1. An inorganic salt crystallization-deposition test system in subcritical/supercritical water, comprising:
the preheating unit is used for respectively preheating water and the salt solution;
the testing unit comprises a high-pressure reaction kettle (7) with a built-in coil (73), preheated water is connected with an inlet of the coil (73), preheated salt solution is connected with an inlet (71) of the high-pressure reaction kettle, the inlet (71) of the high-pressure reaction kettle (7) is arranged on a kettle cover of the high-pressure reaction kettle (7), a sample block (72) is arranged at the tail end of the inlet (71) of the high-pressure reaction kettle (7) positioned in the high-pressure reaction kettle, a stirrer (77) and a thermometer sleeve (74) for installing a thermometer are further arranged in the high-pressure reaction kettle (7), and a high-pressure reaction kettle outlet (76) and a pressure gauge interface (75) for installing a pressure gauge are further arranged on the;
and the reaction post-treatment unit comprises a salt solution filtering, cooling and pressure reduction sampling pipeline connected with the outlet (76) of the high-pressure reaction kettle and a water cooling and pressure reduction pipeline connected with the outlet of the coil (73).
2. The crystallization-deposition test system for inorganic salt in subcritical/supercritical water according to claim 1, wherein the preheating unit comprises a water storage tank (1), a water pump (2), a first preheater (3), a salt solution tank (4), a salt solution pump (5) and a second preheater (6), wherein an outlet of the water storage tank (1) is connected with an inlet of the water pump (2), an outlet of the water pump (2) is connected with an inlet of the first preheater (3), an outlet of the salt solution tank (4) is connected with an inlet of the salt solution pump (5), and an outlet of the salt solution pump (5) is connected with an inlet of the second preheater (6).
3. The crystallization-deposition test system for inorganic salts in subcritical/supercritical water according to claim 1, characterized in that a filter (8), a second cooler (11), a second backpressure valve (V6), a collection tank (12) and a sampling bottle (13) which are connected in parallel are sequentially arranged on the saline solution filtering, cooling and depressurizing sampling pipeline along the flow direction; and a cooler I (9), a backpressure valve I (V5) and a waste liquid tank (10) are sequentially arranged on the water cooling pressure reducing pipeline.
4. The crystallization-deposition test system for inorganic salts in subcritical/supercritical water according to claim 3, characterized in that a second stop valve (V2) is arranged between the second preheater (6) and the high-pressure reaction kettle inlet (71), and a fourth stop valve (V4) is arranged between the filter (8) and the second cooler (11).
5. The crystallization-deposition test system for inorganic salts in subcritical/supercritical water as claimed in claim 4, characterized in that a bypass is provided between the second cooler (11) and the preheated salt solution, the inlet of the bypass is located before the second cut-off valve (V2), the outlet of the bypass is located after the fourth cut-off valve (V4), and the bypass is provided with the first cut-off valve (V1) and the third cut-off valve (V3), the first cut-off valve (V1) is close to the second preheater (6), and the third cut-off valve (V3) is close to the second cooler (11).
6. The crystallization-deposition test system for inorganic salts in subcritical/supercritical water according to claim 4, characterized in that a stop valve five (V7) is arranged between the back pressure valve II (V6) and the collection tank (12), a branch is arranged in front of the stop valve five (V7), and a stop valve six (V8) and a sampling tank (13) are sequentially arranged on the branch.
7. The crystallization-deposition test system for inorganic salts in subcritical/supercritical water as claimed in claim 1, wherein the high-pressure reaction kettle inlet (71) is located at the top position of the kettle cover, the tail end is located at the bottom position of the kettle cover, the high-pressure reaction kettle outlet (76) is located at the bottom position of the high-pressure reaction kettle, a thermometer is arranged in the thermometer sleeve (74), the pressure gauge interface (75) is connected with a pressure gauge, and the stirrer (77) is located at the axial position of the kettle body and penetrates through the whole kettle body.
8. The crystallization-deposition test system for inorganic salts in subcritical/supercritical water according to claim 1, wherein the coil pipe (73) is installed on a kettle cover of the high-pressure reaction kettle (7), the axis of the coil pipe is coaxial with the high-pressure reaction kettle (7), and the inlet and the outlet of the coil pipe penetrate through the kettle cover and are respectively connected with the first preheater (3) and the first cooler (9).
9. The crystallization-deposition test system for inorganic salts in subcritical/supercritical water according to claim 1, characterized in that the first preheater (3) and the second preheater (6) are tubular electric heaters, the first cooler (9) and the second cooler (11) are spiral coil type or tubular heat exchangers, and the water pump (2) and the salt solution pump (5) are high-pressure metering pumps.
10. A test method based on the crystallization-deposition test system of inorganic salt in sub-supercritical water according to any one of claims 1 to 9, characterized by comprising the following steps:
step 1), boosting the salt solution in a salt solution tank (4) through a salt solution pump (5), pumping the salt solution into a second preheater (6) for preheating, and then flowing into a high-pressure reaction kettle (7) through a high-pressure reaction kettle inlet (71);
step 2), boosting water in the water storage tank (1) through a water pump (2), pumping the water into a first preheater (3) for preheating, and then flowing into a coil (73) to form a cold wall or a hot wall with controllable temperature for the salt solution in the step 1);
step 3), the salt solution after pressurization and temperature rise in the step 1) reaches a subcritical or supercritical state, and flows out from an inlet (71) of the high-pressure reaction kettle and is sprayed on a sample block (72) for crystallization or deposition; the salt solution in the high-pressure reaction kettle (7) simultaneously generates different inorganic salt crystallization and deposition processes on the surface of the coil pipe (73) under the influence of a cold wall or a hot wall, and forms crystallization and deposition particles; during the process, the stirrer (77) can also be started to form turbulent disturbance on the saline solution;
step 4), the salt solution obtained in the step 3) flows out of the high-pressure reaction kettle (7), is filtered by a filter (8) and then enters a second cooler (11) for cooling, then enters a second backpressure valve (V6) for pressure reduction, and then enters a sampling bottle (13) for sampling test or flows into a collection tank (12);
step 5), water in the coil (73) in the step 2) flows into a cooler I (9) for cooling, enters a backpressure valve I (V5) for pressure reduction, and then enters a waste liquid tank (10);
step 6), after the experiment, temporarily close salt solution pump (5), preheater one (3) and preheater two (6), close stop valve two (V2), gradually slowly unscrew back pressure valve two (V6), carry out the pressure release operation to high pressure batch autoclave (7), after salt solution all flowed out high pressure batch autoclave (7) in step 4), close stop valve four (V4), open stop valve one (V1) and stop valve three (V3), restart salt solution pump (5) and continue to pump into cold salt solution cooling line in the pipeline, stop when cooling to below 80 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114858896A (en) * | 2022-05-09 | 2022-08-05 | 西安交通大学 | Multifunctional electrochemical research platform suitable for subcritical/supercritical water environment |
| CN115318235A (en) * | 2022-08-31 | 2022-11-11 | 西安交通大学 | Continuous system and method for collecting water-soluble inorganic salt deposition particles in high-temperature and high-pressure water |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101570375A (en) * | 2009-05-05 | 2009-11-04 | 西安交通大学 | Method for recovery and cascade utilization of waste heat of supercritical water treatment system of waste organic substances |
| CN101580320A (en) * | 2009-06-05 | 2009-11-18 | 西安交通大学 | Method for operating a supercritical water treatment system of waste organic substances |
| CN202129075U (en) * | 2011-07-04 | 2012-02-01 | 丹阳四达化工有限公司 | Reaction kettle suitable for low-temperature reaction and exothermic reaction |
| CN202506365U (en) * | 2012-04-20 | 2012-10-31 | 浦城县永芳香料科技有限公司 | Temperature control device of high-pressure reactor |
| CN103508589A (en) * | 2013-09-30 | 2014-01-15 | 西安交通大学 | Reactor for supercritical water oxidation or gasification treatment of high-salt organic waste water |
| CN204073484U (en) * | 2014-09-25 | 2015-01-07 | 山西同济药业有限公司 | Metronidazole crystallization reaction still |
| CN204255682U (en) * | 2014-11-28 | 2015-04-08 | 鲁西催化剂有限公司 | A kind of novel hydrogenation evaluating catalyst sampler |
| CN207085922U (en) * | 2017-08-14 | 2018-03-13 | 江苏开放大学 | A kind of permanent magnetism Stirring reactor |
| CN110038504A (en) * | 2019-04-23 | 2019-07-23 | 中海油能源发展股份有限公司 | A kind of reaction system suitable for supercritical water oxidation intermittent duty |
| CN110802077A (en) * | 2019-10-12 | 2020-02-18 | 西安交通大学 | Online cleaning system and method based on supercritical water oxidation technology |
-
2020
- 2020-07-06 CN CN202010639751.3A patent/CN111781108B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101570375A (en) * | 2009-05-05 | 2009-11-04 | 西安交通大学 | Method for recovery and cascade utilization of waste heat of supercritical water treatment system of waste organic substances |
| CN101580320A (en) * | 2009-06-05 | 2009-11-18 | 西安交通大学 | Method for operating a supercritical water treatment system of waste organic substances |
| CN202129075U (en) * | 2011-07-04 | 2012-02-01 | 丹阳四达化工有限公司 | Reaction kettle suitable for low-temperature reaction and exothermic reaction |
| CN202506365U (en) * | 2012-04-20 | 2012-10-31 | 浦城县永芳香料科技有限公司 | Temperature control device of high-pressure reactor |
| CN103508589A (en) * | 2013-09-30 | 2014-01-15 | 西安交通大学 | Reactor for supercritical water oxidation or gasification treatment of high-salt organic waste water |
| CN204073484U (en) * | 2014-09-25 | 2015-01-07 | 山西同济药业有限公司 | Metronidazole crystallization reaction still |
| CN204255682U (en) * | 2014-11-28 | 2015-04-08 | 鲁西催化剂有限公司 | A kind of novel hydrogenation evaluating catalyst sampler |
| CN207085922U (en) * | 2017-08-14 | 2018-03-13 | 江苏开放大学 | A kind of permanent magnetism Stirring reactor |
| CN110038504A (en) * | 2019-04-23 | 2019-07-23 | 中海油能源发展股份有限公司 | A kind of reaction system suitable for supercritical water oxidation intermittent duty |
| CN110802077A (en) * | 2019-10-12 | 2020-02-18 | 西安交通大学 | Online cleaning system and method based on supercritical water oxidation technology |
Non-Patent Citations (1)
| Title |
|---|
| JIANQIAO YANG,ET AL.: "Effect of salt deposit on corrosion behavior of Ni-based alloys and stainless steels in supercritical water", 《THE JOURNAL OF SUPERCRITICAL FLUIDS》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114858896A (en) * | 2022-05-09 | 2022-08-05 | 西安交通大学 | Multifunctional electrochemical research platform suitable for subcritical/supercritical water environment |
| CN114858896B (en) * | 2022-05-09 | 2023-06-27 | 西安交通大学 | Multifunctional electrochemical research platform suitable for subcritical/supercritical water environment |
| CN115318235A (en) * | 2022-08-31 | 2022-11-11 | 西安交通大学 | Continuous system and method for collecting water-soluble inorganic salt deposition particles in high-temperature and high-pressure water |
| CN115318235B (en) * | 2022-08-31 | 2024-01-05 | 西安交通大学 | Continuous system and method for collecting water-soluble inorganic salt deposition particles in high-temperature high-pressure water |
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