CN111781130A - Flowing corrosion-salt deposition online test system and method used in supercritical water treatment environment - Google Patents
Flowing corrosion-salt deposition online test system and method used in supercritical water treatment environment Download PDFInfo
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Abstract
An in-line mobile corrosion-salt deposition test system for use in a supercritical water processing environment, comprising: the preheating unit is used for respectively preheating hydrogen peroxide, the solution and deionized water; the mixing unit comprises a mixing main pipe, and the preheated hydrogen peroxide, the solution and the deionized water are mixed in the mixing main pipe; the test unit comprises a test tube with an inlet connected with an outlet of the mixing main tube, the test tube is of a composite structure with a built-in detachable inner bushing, and is provided with an electric heater, a plurality of thermocouples and a pressure sensor; the cooling unit is used for cooling the material out of the test tube; the pressure reduction unit is used for reducing the pressure of the material discharged from the cooling unit; and the sampling unit comprises a conductivity detector, a solution collecting tank and a sampling tank. The method can be used for testing the corrosion-salt deposition condition of the organic solution and the oxidant after oxidation reaction under different flow rates and different atmospheres on line.
Description
Technical Field
The invention belongs to the technical field of energy, chemical industry and environmental protection, and particularly relates to a flowing corrosion-salt deposition online test system and method used in a supercritical water treatment environment.
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 excellent effects in the aspects of treating phenolic compounds, polychlorinated biphenyl organic matters, pesticides, fuel intermediate aniline, sludge, human metabolites and other pollutants. From the perspective of sustainable development of the environment and from the perspective of industrial development, supercritical water oxidation technology is a new green and environmental-friendly technology with 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.
The supercritical water gasification technology is carried out in a reducing atmosphere rich in hydrogen and free of oxygen, various organic matters in biomass are dissolved by utilizing the strong dissolving capacity of supercritical water, and then the biomass is finally converted into small molecular compounds such as hydrogen-rich gas and the like through reaction processes such as rapid decomposition, water vapor reforming, water vapor conversion and the like under the condition of homogeneous reaction, so that the technology is known as the hydrogen production technology with the most development potential. Compared with the traditional pyrolysis gasification hydrogen production technology, the supercritical water gasification technology has the advantages that the temperature is milder, the hydrogen content in the gas product can exceed 70%, the water content of the material is not required, the method is suitable for most of biomass, high-concentration organic pollutants and the like, and no secondary pollution is generated.
Compared with the traditional gasification technology, the supercritical water gasification hydrogen production process has the following advantages:
1. the reaction conditions are mild: the temperature of the conventional organic matter gasification hydrogen production reaction is usually over 1100 ℃, and the temperature of the supercritical water gasification reaction is 600-800 ℃;
2. the volume fraction of hydrogen is high: the volume ratio of hydrogen in the synthesis gas obtained by traditional coal gasification is usually 30%, and the volume share of hydrogen in the supercritical water gasification technology can reach 60-75%, so that the subsequent hydrogen purification cost is greatly reduced;
3. the hydrogen gasification rate is high: almost all CO in supercritical water gasification reaction products is generated into H through in-situ water-gas conversion reaction2The hydrogen gasification efficiency can reach 180% (in other words, 80% of the obtained hydrogen comes from water);
4. no requirement for water content of the material and no secondary pollutant.
SCWO and SCWG technologies are carried out in high temperature, high pressure, high salt concentration environments, where the harsh conditions are prone to corrosion of the equipment and salt precipitation in the equipment. The high oxygen environment in the SCWO process and the hydrogen rich environment in the SCWG process can also lead to different types of material corrosion. 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. Supercritical water gasification technology also suffers from salt deposition and corrosion problems. Thus, in order to make these processes economically viable, the bottleneck problems of corrosion and salt deposition must be addressed.
Currently, the basic method for inhibiting corrosion is to select a base metal for use in different parts of the system based on the corrosion resistance characteristics of different materials. In addition, the special design of the reactor is also included, and anti-corrosion measures are added to local corrosion-prone areas of the equipment, such as installing an inner sleeve, and performing surface spraying or pre-oxidation treatment on the surface of the equipment in direct contact with a highly corrosive fluid. In addition, from the material perspective, can also adopt modes such as material preneutralization technique, material cold state to spout and dilute material to restrain pipeline, the corruption of equipment material. 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 inhibiting corrosion and solving salt deposition 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 microscopic characteristics of material corrosion and 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 taken according to the symptoms.
Disclosure of Invention
In order to overcome the defects of the prior art, solve the problems of corrosion and salt deposition in supercritical water oxidation and explore the microscopic characteristics of material corrosion and the crystallization deposition characteristics of inorganic salt, the invention aims to provide a flowing corrosion-salt deposition online test system and a flowing corrosion-salt deposition online test method for a supercritical water treatment environment, which can online test the corrosion-salt deposition condition after the oxidation reaction of an organic solution and an oxidant under different flow rates and different atmospheres.
In order to achieve the purpose, the invention adopts the technical scheme that:
an in-line mobile corrosion-salt deposition test system for use in a supercritical water processing environment, comprising:
the preheating unit is used for respectively preheating hydrogen peroxide, the solution and deionized water;
the mixing unit comprises a mixing main pipe 16, and the preheated hydrogen peroxide, the solution and the deionized water are mixed in the mixing main pipe 16;
the testing unit comprises a testing pipe 17 with an inlet connected with an outlet of the mixing main pipe 16, the testing pipe 17 is of a composite structure with a built-in detachable inner bushing, the front end of the testing pipe is wrapped with an electric heater four 18, a thermocouple two T2 and a thermocouple three T3 are sequentially arranged on two sides of the electric heater four 18, a thermocouple four T4 is arranged at the tail end of the testing pipe 17, the thermocouple three T3 and the electric heater four 18 are interlocked through a control line, a pressure sensor two P2, a pressure sensor three P3 and a pressure sensor four P4 are respectively and radially and symmetrically arranged with the thermocouple two T2, the thermocouple three T3 and the thermocouple four T4, and the pressure sensor two P2, the pressure sensor three P3 and the pressure sensor four P4 are interlocked through differential pressure control lines;
the cooling unit is connected with the outlet of the test tube 17 and cools the material out of the test tube 17;
the pressure reduction unit is connected with the outlet of the cooling unit and is used for reducing the pressure of the material discharged from the cooling unit;
and the sampling unit comprises a second conductivity detector 22 arranged in the outlet pipeline of the depressurization unit, and a pipeline behind the second conductivity detector 22 is connected with the solution collecting tank 24 and is connected with a branch with a regulating valve seven V8 and a sampling tank 23.
The unit of preheating includes that hydrogen peroxide solution preheats unit, solution preheats unit and deionized water and preheats the unit, hydrogen peroxide solution preheats the unit and includes hydrogen peroxide solution jar 1 and sets gradually hydrogen peroxide pump 2 and electric heater one 3 on 1 outlet pipeline of hydrogen peroxide solution jar, solution preheats the unit and includes solution tank 4 and set gradually solution pump 5 and electric heater two 6 on 4 outlet pipeline of solution tank, deionized water preheats the unit and includes deionized water tank 10 and set gradually deoxidization water pump 11 and electric heater three 12 on 10 outlet pipeline of deionized water tank.
An adjusting valve I V1 is arranged on the outlet pipeline of the hydrogen peroxide tank 1 after the electric heater I3, an adjusting valve II V2 is arranged on the outlet pipeline of the solution tank 4 after the electric heater II 6, and an adjusting valve III V3 is arranged on the outlet pipeline of the deionized water tank 10 after the electric heater III 12.
An inlet of the deionized water tank 10 is connected with outlets of the oxygen cylinder 7, the hydrogen cylinder 8 and the nitrogen cylinder 9, an aeration pipe 101 is arranged in the deionized water tank 10, a plurality of small holes are formed in the aeration pipe 101, and an inlet of the aeration pipe 101 is connected with outlets of the oxygen cylinder 7, the hydrogen cylinder 8 and the nitrogen cylinder 9; an oxygen content detector 102 and a first conductivity detector 103 are sequentially arranged between the deionized water tank 10 and the deoxygenation water pump 11.
The axial center of the mixing main pipe 16 is provided with a material spray pipe 13, the preheated solution is axially fed into the mixing main pipe 16 through the material spray pipe 13, the periphery of the mixing main pipe 16 is circumferentially provided with a hydrogen peroxide mixer 14 and a deionized water mixer 15, outlets of the hydrogen peroxide mixer 14 and the deionized water mixer 15 are positioned on the inner wall surface of the mixing main pipe 16, the preheated hydrogen peroxide and the deionized water are respectively fed into the mixing main pipe 16 through the hydrogen peroxide mixer 14 and the deionized water mixer 15, and the tail part of the mixing main pipe 16 is provided with a first thermocouple T1 and a first pressure sensor P1 which are radially symmetrical.
The cooling unit comprises a cooling water jacket 19, a circulating cooling tower 20 and a cooler 21, wherein the cooling water jacket 19 is wrapped outside the tail end of a testing pipe 17, an inlet is connected with an outlet of the circulating cooling tower 20, an outlet is connected with an inlet of the circulating cooling tower 20, a cooling water inlet N1 is positioned at the upper part of the tail end of the cooling water jacket 19, a cooling water outlet N2 is positioned at the lower part of the front end of the cooling water jacket 19, an inlet of the cooler 21 is connected with an outlet of the testing pipe 17, a thermocouple five T5 is arranged behind the cooling water jacket 19 on the testing pipe 17, a regulating valve four V4 is arranged on a cooling water inlet N1 pipeline, the thermocouple five T5 and the regulating valve four V4 are interlocked through a control line, and a pressure sensor five P5 is radially.
The cooler 21 is a spiral coil or a tube type heat exchanger, and the hydrogen peroxide pump 2, the solution pump 5 and the deionized water pump 11 are plug type high-pressure pumps or diaphragm type high-pressure pumps.
The pressure reduction unit comprises a regulating valve five V5, a backpressure valve V6 and a regulating valve six V7 which are sequentially arranged on an outlet pipeline of the cooling unit, and the backpressure valve V6 is interlocked with the pressure sensor one P1 through a control line.
The conductivity detector 22 in the sampling unit is positioned behind the pressure reduction unit, the conductivity detector 22 is connected with a regulating valve seven V8 through a branched sampling pipeline, and a sampling tank 23 is connected below the regulating valve seven V8.
The invention also provides a testing method based on the flowing corrosion-salt deposition online testing system used in the supercritical water treatment environment, which comprises the following steps:
1) the solution enters a solution tank 4, is pressurized and conveyed through a solution pump 5, enters an electric heater II 6 for heating, and opens a pressure regulating valve II V2;
2) the solution treated in the step 1) enters a main mixing pipe 16 through a material spray pipe 13;
3) the solution treated in the step 2) flows through a fourth electric heater 18 to be continuously heated or the temperature is kept stable, at the moment, the solution is in contact with the inner bushing, and inorganic salt is deposited on the inner bushing or the inner bushing is corroded;
4) the fluid after the step 3) is primarily cooled through a cooling water jacket 19, then flows into a cooler 21 for continuous cooling, then sequentially passes through a five-valve V5, a back pressure valve V6 and a six-valve V7 in a pressure reduction unit for pressure reduction, and then flows into a solution collecting tank 24, or opens a seven-valve V8, so that part of the solution flows into a sampling tank 23 for sampling, and a subsequent analysis test is carried out to obtain the flowing corrosion-salt deposition condition of the solution;
5) if hydrogen peroxide needs to be added, opening a regulating valve I V1, conveying the hydrogen peroxide in a hydrogen peroxide tank 1 through a hydrogen peroxide pump 2 under pressure, wherein the pressure is 0.5-1 MPa higher than the pressure of the solution, heating the hydrogen peroxide in an electric heater I3, mixing the hydrogen peroxide in a mixing main pipe 16 through a hydrogen peroxide mixer 14, reacting the hydrogen peroxide with the solution in the step 2), and repeating the steps 3) and 4) to obtain the flowing corrosion-salt deposition condition after the solution reacts with an oxidant;
6) if deionized water needs to be added, opening a regulating valve III V3, enabling the deionized water to enter a deionized water tank 10, processing the deionized water by oxygen, hydrogen or nitrogen in an oxygen cylinder 7, a hydrogen cylinder 8 or a nitrogen cylinder 9 to obtain deionized water under different atmospheres, pressurizing and conveying the deionized water by a deionized water pump 11, enabling the pressure to be higher than the solution pressure by 0.5-1 MPa, enabling the deionized water to enter an electric heater III 12 for heating, enabling the deionized water to enter a mixing main pipe 16 through a deionized water mixer 15 to be mixed with the solution in the step 2), and repeating the steps 3) and 4) to obtain the flowing corrosion-salt deposition conditions under different flow rates and flow conditions;
7) only opening the regulating valve three V3, closing the regulating valve one V1 and the regulating valve two V2, and repeating the steps 6), 3) and 4) in sequence to obtain the flowing corrosion-salt deposition conditions under different atmospheres.
Compared with the prior art, the invention has the beneficial effects that:
the device can collect samples such as salt crystal deposition particles or corrosion products on line through the design of the detachable inner bushing test tube in the test unit for subsequent corrosion-salt deposition characteristic analysis; through the arrangement of the sampling device, the solution sample can be collected on line for subsequent test analysis; the multistage accurate and stable pressure reduction of the system can be realized through the arrangement of the combined valve in the pressure reduction unit; by arranging the hydrogen peroxide system and the mixing unit, the flow corrosion-salt deposition condition under the SCWO reaction mixing condition can be tested; by arranging the deionized water system and the mixing unit, the flowing corrosion-salt deposition condition under different flow speed and flow conditions can be tested; the flow corrosion-salt deposition conditions under different atmospheres can be tested by designing an aeration pipe and an oxygen, hydrogen and nitrogen system in the deionized water tank; through the arrangement of the deionized water tank outlet oxygen content detector and the first conductivity detector and the arrangement of the pressure reduction unit outlet conductivity detector II, the properties of the solution can be mastered in real time.
Drawings
FIG. 1 is a schematic structural diagram of a flowing corrosion-salt deposition on-line testing system in a supercritical water treatment environment according to the present invention.
Wherein 1 is a hydrogen peroxide tank; 2 is a hydrogen peroxide pump; 3 is an electric heater I; 4 is a solution tank; 5 is a solution pump; 6 is an electric heater II; 7 is an oxygen tank; 8 is a hydrogen tank; 9 is a nitrogen tank; 10 is a deionized water tank; 101 is an aeration pipe; 102 is an oxygen content detector; 103 is a conductivity detector; 11 is a deionized water pump; 12 is an electric heater III; 13 is a material spray pipe; 14 is a hydrogen peroxide mixer; 15 is a deionized water mixer; 16 is a mixing main pipe; 17 is a test tube; 18 is an electric heater IV; 19 is a cooling water jacket; 20 is a circulating cooling tower; 21 is a cooler; 22 is a second conductivity detector; 23 is a sampling tank; and 24 is a solution collecting tank. V1 is a regulating valve I; v2 is a regulating valve II; v3 is regulating valve III; v4 is regulating valve IV; v5 is regulating valve V; v6 is a backpressure valve; v7 is regulating valve six; v8 is regulating valve VII; t1 is thermocouple I; t2 is thermocouple II; t3 is thermocouple III; t4 is thermocouple IV; t5 is thermocouple five; p1 is pressure sensor I; p2 is pressure sensor II; p3 is pressure sensor III; p4 is pressure sensor four; p5 is pressure sensor five; n1 is a cooling water inlet; n2 is a cooling water outlet.
Detailed Description
The embodiments of the present invention will be described in detail below with reference to the drawings and examples.
As shown in FIG. 1, the invention relates to a flowing corrosion-salt deposition online test system used in a supercritical water treatment environment, which comprises a preheating unit, a mixing unit, a test unit, a cooling unit, a pressure reduction unit and a sampling unit, wherein:
the preheating unit is used for respectively preheating hydrogen peroxide, the solution and deionized water. In this embodiment, it specifically includes that hydrogen peroxide solution preheats the unit, solution preheats unit and deionized water and preheats the unit, hydrogen peroxide solution preheats the unit and includes hydrogen peroxide solution jar 1 and set gradually hydrogen peroxide pump 2 and the electric heater 3 on 1 outlet pipeline of hydrogen peroxide solution jar, solution preheats the unit and includes solution jar 4 and set gradually solution pump 5 and the electric heater two 6 on 4 outlet pipeline of solution jar, deionized water preheats the unit and includes deionized water jar 10 and set gradually deoxidization water pump 11 and the electric heater three 12 on 10 outlet pipeline of deionized water jar. Wherein, a regulating valve I V1 is arranged on the outlet pipeline of the hydrogen peroxide tank 1 after the electric heater I3, a regulating valve II V2 is arranged on the outlet pipeline of the solution tank 4 after the electric heater II 6, and a regulating valve III V3 is arranged on the outlet pipeline of the deionized water tank 10 after the electric heater III 12. An inlet of the deionized water tank 10 is connected with outlets of the oxygen cylinder 7, the hydrogen cylinder 8 and the nitrogen cylinder 9, an aerator pipe 101 is arranged in the deionized water tank 10, a plurality of small holes are arranged on the aerator pipe 101, and an inlet of the aerator pipe 101 is connected with outlets of the oxygen cylinder 7, the hydrogen cylinder 8 and the nitrogen cylinder 9; an oxygen content detector 102 and a first conductivity detector 103 are sequentially arranged between the deionized water tank 10 and the deoxygenation water pump 11.
The mixing unit comprises a mixing main pipe 16 for mixing the preheated hydrogen peroxide, the solution and the deionized water in the mixing main pipe 16. In this embodiment, a material spray pipe 13 is disposed at an inner axial center of the main mixing pipe 16, the preheated solution is axially fed into the main mixing pipe 16 through the material spray pipe 13, a hydrogen peroxide mixer 14 and a deionized water mixer 15 are circumferentially disposed on an outer periphery of the main mixing pipe 16, outlets of the hydrogen peroxide mixer 14 and the deionized water mixer 15 are located on an inner wall surface of the main mixing pipe 16, the preheated hydrogen peroxide and deionized water are respectively fed into the main mixing pipe 16 through the hydrogen peroxide mixer 14 and the deionized water mixer 15, and a thermocouple T1 and a pressure sensor P1 which are radially symmetrical are disposed at a tail portion of the main mixing pipe 16.
The test unit completes the test and comprises a test pipe 17, the inlet of the test pipe 17 is connected with the outlet of the mixing main pipe 16, and the outlet of the test pipe is connected with the cooling unit. The test tube 17 is of a composite structure with a built-in detachable inner bushing, the front end of the test tube is wrapped and provided with an electric heater four 18, two sides of the electric heater four 18 are sequentially provided with a thermocouple two T2 and a thermocouple three T3, the tail end of the test tube 17 is provided with a thermocouple four T4, the thermocouple three T3 is interlocked with the electric heater four 18 through a control line, a pressure sensor two P2, a pressure sensor three P3 and a pressure sensor four P4 are radially and symmetrically arranged with the thermocouple two T2, the thermocouple three T3 and the thermocouple four T4 respectively, and the pressure sensor two P2, the pressure sensor three P3 and the pressure sensor four P4 are interlocked through a pressure difference control line.
The cooling unit is used for cooling the material out of the test tube 17, and in this embodiment, the cooling unit includes a cooling water jacket 19, a circulating cooling tower 20 and a cooler 21, the cooling water jacket 19 is wrapped outside the tail end of the test tube 17, an inlet is connected with an outlet of the circulating cooling tower 20, an outlet is connected with an inlet of the circulating cooling tower 20, a cooling water inlet N1 is located at the upper portion of the tail end of the cooling water jacket 19, a cooling water outlet N2 is located at the lower portion of the front end of the cooling water jacket 19, an inlet of the cooler 21 is connected with an outlet of the test tube 17, and an outlet is connected with the depressurization unit. A thermocouple five T5 is arranged on the test tube 17 behind the cooling water jacket 19, a regulating valve four V4 is arranged on a cooling water inlet N1 pipeline, the thermocouple five T5 and the regulating valve four V4 are interlocked by a control line, a pressure sensor five P5 is radially and symmetrically arranged with the thermocouple five T5, and the cooler 21 is a shell-and-tube heat exchanger such as a spiral coil pipe and a tube array type.
The pressure reduction unit is used for reducing the pressure of the material discharged from the cooling unit, the inlet of the pressure reduction unit is connected with the outlet of the cooler 21, and the outlet of the pressure reduction unit is connected with the inlet of the sampling unit. In the embodiment, the device comprises a regulating valve five V5, a backpressure valve V6 and a regulating valve six V7 which are arranged on an outlet pipeline of the cooling unit in sequence, and the backpressure valve V6 is interlocked with a pressure sensor P1 through a control line.
The sampling unit is used for sampling the finally discharged materials, and in the embodiment, the sampling unit comprises a second conductivity detector 22 arranged in an outlet pipeline of the depressurization unit, and a pipeline behind the second conductivity detector 22 is connected with the solution collecting tank 24 and is connected with a branch with a regulating valve seven V8 and a sampling tank 23. Specifically, the conductivity detector 22 is located after the depressurization unit, and the conductivity detector 22 is connected to a regulating valve seven V8 through a branched sampling line, and the sampling tank 23 is connected below the regulating valve seven V8.
In this embodiment, the hydrogen peroxide pump 2, the solution pump 5, and the deionized water pump 11 are high-pressure pumps, and may be plunger-type high-pressure pumps or diaphragm-type high-pressure pumps.
Based on the flowing corrosion-salt deposition online test system, the flowing corrosion-salt deposition online test method in the supercritical water treatment environment comprises the following steps:
step 1), the solution enters a solution tank 4, is pressurized and conveyed through a solution pump 5, enters an electric heater II 6 for heating, and a pressure regulating valve II V2 is opened;
step 2) the solution treated in the step 1) enters a mixing main pipe 16 through a material spray pipe 13;
step 3), the solution treated in the step 2) flows through a fourth electric heater 18 to be continuously heated or the temperature is kept stable, at the moment, the solution is in contact with the inner lining, and inorganic salt is deposited on the inner lining or the inner lining is corroded;
step 4) the fluid after the step 3) is primarily cooled through a cooling water jacket 19, then flows into a cooler 21 to be continuously cooled, then sequentially passes through a five-valve V5, a back pressure valve V6 and a six-valve V7 in a depressurization unit to be depressurized, and then flows into a solution collecting tank 24, or opens a seven-valve V8 regulating valve to allow part of the solution to flow into a sampling tank 23 for sampling, and a subsequent analysis test is carried out to obtain the flowing corrosion-salt deposition condition of the solution;
step 5) if hydrogen peroxide needs to be added, opening a regulating valve I V1, conveying the hydrogen peroxide in a hydrogen peroxide tank 1 through a hydrogen peroxide pump 2 under pressure, wherein the pressure is generally 0.5-1 MPa higher than the solution pressure, heating the hydrogen peroxide in an electric heater I3, mixing the hydrogen peroxide in a mixing main pipe 16 through a hydrogen peroxide mixer 14, reacting the hydrogen peroxide with the solution in the step 2), and repeating the steps 3) and 4), so that the flowing corrosion-salt deposition condition after the solution reacts with an oxidant can be obtained;
step 6) if deionized water needs to be added, opening a regulating valve III V3, enabling the deionized water to enter a deionized water tank 10, processing the deionized water by oxygen, hydrogen or nitrogen in an oxygen cylinder 7, a hydrogen cylinder 8 or a nitrogen cylinder 9 to obtain deionized water under different atmospheres, pressurizing and conveying the deionized water by a deionized water pump 11, enabling the deionized water to enter an electric heater III 12 for heating, enabling the deionized water to enter a mixing main pipe 16 through a deionized water mixer 15 to be mixed with the solution in the step 2), and repeating the steps 3) and 4), thereby obtaining the flow corrosion-salt deposition conditions under different flow rates and flow conditions;
and 7) only opening the regulating valve III V3, closing the regulating valve I V1 and the regulating valve II V2, and repeating the steps 6), 3) and 4) in sequence, so that the flowing corrosion-salt deposition conditions under different atmospheres can be obtained.
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 in-line mobile corrosion-salt deposit testing system for use in a supercritical water processing environment, comprising:
the preheating unit is used for respectively preheating hydrogen peroxide, the solution and deionized water;
the mixing unit comprises a mixing main pipe (16), and the preheated hydrogen peroxide, the solution and the deionized water are mixed in the mixing main pipe (16);
the testing unit comprises a testing pipe (17) with an inlet connected with an outlet of a mixing main pipe (16), the testing pipe (17) is of a composite structure with a built-in detachable inner bushing, the front end of the testing pipe is wrapped with an electric heater II (18), two sides of the electric heater II (18) are sequentially provided with a thermocouple II (T2) and a thermocouple III (T3), the tail end of the testing pipe (17) is provided with a thermocouple IV (T4), the thermocouple III (T3) and the electric heater IV (18) are interlocked through a control line, and the testing pipe, the thermocouple II (T2), the thermocouple III (T3) and the thermocouple IV (T4) are respectively and radially and symmetrically provided with a pressure sensor II (P2), a pressure sensor III (P3) and a pressure sensor IV (P4) which are interlocked through a pressure difference control line;
the cooling unit is connected with the outlet of the test tube (17) and cools the material out of the test tube (17);
the pressure reduction unit is connected with the outlet of the cooling unit and is used for reducing the pressure of the material discharged from the cooling unit;
and the sampling unit comprises a second conductivity detector (22) arranged in an outlet pipeline of the depressurization unit, and a pipeline behind the second conductivity detector (22) is connected with the solution collecting tank (24) and is connected with a branch with a seventh regulating valve (V8) and a sampling tank (23).
2. The flowing corrosion-salt deposition online test system for the supercritical water treatment environment of claim 1, wherein the preheating unit comprises a hydrogen peroxide preheating unit, a solution preheating unit and a deionized water preheating unit, the hydrogen peroxide preheating unit comprises a hydrogen peroxide tank (1) and a hydrogen peroxide pump (2) and an electric heater (3) which are sequentially arranged on an outlet pipeline of the hydrogen peroxide tank (1), the solution preheating unit comprises a solution tank (4) and a solution pump (5) and an electric heater (6) which are sequentially arranged on an outlet pipeline of the solution tank (4), and the deionized water preheating unit comprises a deionized water tank (10) and a deoxygenated water pump (11) and an electric heater (12) which are sequentially arranged on an outlet pipeline of the deionized water tank (10).
3. The on-line flowing corrosion-salt deposition test system for supercritical water treatment environment of claim 2 wherein the outlet line of the hydrogen peroxide tank (1) is provided with a first regulating valve (V1) after the first electric heater (3), the outlet line of the solution tank (4) is provided with a second regulating valve (V2) after the second electric heater (6), and the outlet line of the deionized water tank (10) is provided with a third regulating valve (V3) after the third electric heater (12).
4. The on-line testing system for mobile corrosion-salt deposition in supercritical water treatment environment of claim 2 is characterized in that the inlet of the deionized water tank (10) is connected with the outlets of the oxygen cylinder (7), the hydrogen cylinder (8) and the nitrogen cylinder (9), the inside of the deionized water tank (10) is provided with an aeration pipe (101), the aeration pipe (101) is provided with a plurality of small holes, and the inlet of the aeration pipe (101) is connected with the outlets of the oxygen cylinder (7), the hydrogen cylinder (8) and the nitrogen cylinder (9); an oxygen content detector (102) and a first conductivity detector (103) are sequentially arranged between the deionized water tank (10) and the deoxygenation water pump (11).
5. The flowing corrosion-salt deposition online test system for supercritical water treatment environment of claim 1, wherein a material spray pipe (13) is disposed at the inner axial center of the mixing main pipe (16), the preheated solution is axially fed into the mixing main pipe (16) through the material spray pipe (13), a hydrogen peroxide mixer (14) and a deionized water mixer (15) are circumferentially disposed on the outer circumference of the mixing main pipe (16), the outlets of the hydrogen peroxide mixer (14) and the deionized water mixer (15) are located on the inner wall surface of the mixing main pipe (16), the preheated hydrogen peroxide and deionized water are respectively fed into the mixing main pipe (16) through the hydrogen peroxide mixer (14) and the deionized water mixer (15), and a thermocouple I (T1) and a pressure sensor I (P1) which are radially symmetrical are disposed at the tail of the mixing main pipe (16).
6. The flowing corrosion-salt deposition online test system used in supercritical water treatment environment of claim 1, characterized in that the cooling unit comprises a cooling water jacket (19), a circulating cooling tower (20) and a cooler (21), the cooling water jacket (19) wraps the outside of the tail end of the test tube (17), the inlet is connected with the outlet of the circulating cooling tower (20), the outlet is connected with the inlet of the circulating cooling tower (20), a cooling water inlet (N1) is located at the upper part of the tail end of the cooling water jacket (19), a cooling water outlet (N2) is located at the lower part of the front end of the cooling water jacket (19), the inlet of the cooler (21) is connected with the outlet of the test tube (17), a thermocouple five (T5) is arranged on the test tube (17) behind the cooling water jacket (19), a regulating valve four (V4) is arranged on the cooling water inlet (N1), and the thermocouple five (T5) and the regulating valve four (V4) are interlocked by a control line, a pressure sensor five (P5) is arranged radially symmetrically to the thermocouple five (T5).
7. The on-line flowing corrosion-salt deposition test system for use in supercritical water processing environment of claim 6 wherein the cooler (21) is a spiral coil or a tube and tube heat exchanger and the hydrogen peroxide pump (2), the solution pump (5) and the deionized water pump (11) are plug type high pressure pump or diaphragm type high pressure pump.
8. The on-line flowing corrosion-salt deposition test system for supercritical water treatment environment of claim 1 wherein the depressurization unit comprises a regulating valve five (V5), a backpressure valve (V6) and a regulating valve six (V7) which are arranged on the outlet pipeline of the cooling unit in sequence, and the backpressure valve (V6) is interlocked with the pressure sensor one (P1) through a control line.
9. The on-line flowing corrosion-salt deposition test system for supercritical water treatment environment of claim 1, wherein the conductivity detector (22) is located after the pressure reduction unit in the sampling unit, the conductivity detector (22) is connected with a seventh adjusting valve (V8) through a branched sampling pipeline, and a sampling tank (23) is connected below the seventh adjusting valve (V8).
10. The method for testing the flowing corrosion-salt deposition online test system in the supercritical water treatment environment according to any one of claims 1 to 9, is characterized by comprising the following steps:
step 1), feeding the solution into a solution tank (4), pressurizing and conveying the solution by a solution pump (5), feeding the solution into an electric heater II (6), heating the solution, and opening a pressure regulating valve II (V2);
step 2), the solution treated in the step 1) enters a mixing main pipe (16) through a material spray pipe (13);
step 3), the solution treated in the step 2) flows through a fourth electric heater (18) to be continuously heated or the temperature is kept stable, at the moment, the solution is in contact with the inner lining, and inorganic salt is deposited on the inner lining or the inner lining is corroded;
step 4), the fluid after the step 3) is primarily cooled through a cooling water jacket (19), then flows into a cooler (21) to be continuously cooled, then sequentially passes through a valve five (V5), a backpressure valve (V6) and a regulating valve six (V7) in a depressurization unit to be depressurized, and then flows into a solution collecting tank (24), or a regulating valve seven (V8) is opened to enable part of the solution to flow into a sampling tank (23) for sampling, and subsequent analysis and test are carried out to obtain the flowing corrosion-salt deposition condition of the solution;
step 5), if hydrogen peroxide needs to be added, opening a regulating valve I (V1), conveying the hydrogen peroxide in a hydrogen peroxide tank (1) through a hydrogen peroxide pump (2) in a pressurized mode, enabling the pressure to be 0.5-1 MPa higher than the pressure of the solution, heating the hydrogen peroxide in an electric heater I (3), enabling the hydrogen peroxide to enter a mixing main pipe (16) through a hydrogen peroxide mixer (14) to be mixed and react with the solution in the step 2), and repeating the steps 3) and 4) to obtain the flowing corrosion-salt deposition condition after the solution and an oxidant react;
step 6), if deionized water needs to be added, opening a regulating valve III (V3), allowing the deionized water to enter a deionized water tank (10), treating the deionized water by oxygen, hydrogen or nitrogen in an oxygen cylinder (7), a hydrogen cylinder (8) or a nitrogen cylinder (9) to obtain deionized water under different atmospheres, pressurizing and conveying the deionized water by a deionized water pump (11), allowing the deionized water to enter an electric heater III (12) for heating, allowing the deionized water to enter a mixing main pipe (16) through an ion water mixer (15) to be mixed with the solution in the step 2), and repeating the steps 3) and 4 to obtain the flowing corrosion-salt deposition conditions under different flow rates and flow conditions;
and 7), only opening the regulating valve III (V3), closing the regulating valve I (V1) and the regulating valve II (V2), and repeating the steps 6), 3) and 4) in sequence to obtain the flowing corrosion-salt deposition conditions under different atmospheres.
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