CN113522167A - High-temperature high-pressure kettle used in strong corrosion environment and use method - Google Patents
High-temperature high-pressure kettle used in strong corrosion environment and use method Download PDFInfo
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- CN113522167A CN113522167A CN202110555230.4A CN202110555230A CN113522167A CN 113522167 A CN113522167 A CN 113522167A CN 202110555230 A CN202110555230 A CN 202110555230A CN 113522167 A CN113522167 A CN 113522167A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
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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
- B01J19/0006—Controlling or regulating processes
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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
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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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
- B01J19/02—Apparatus characterised by being constructed of material selected for its chemically-resistant properties
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
- G01M3/26—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors
- G01M3/32—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators
- G01M3/3236—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators by monitoring the interior space of the containers
- G01M3/3272—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators by monitoring the interior space of the containers for verifying the internal pressure of closed containers
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Abstract
The utility model provides a high-temperature autoclave who uses under strong corrosive environment, includes outer cauldron subassembly and interior cauldron subassembly, and outer cauldron subassembly includes the outer cauldron body, outer cauldron lid, and interior cauldron subassembly closes the interior cauldron lid that just is located outer cauldron below on the cauldron body including the cover is internal and be used for placing the determinand outside the cauldron, lid, and outer cauldron lid below is provided with the subassembly that hangs that is used for the interior cauldron body of elastic support, has the gap of packing heat-conducting liquid between the outer cauldron body and the interior cauldron body. The high-temperature high-pressure corrosion-resistant kettle with the double-layer structure reduces the requirement of the environment on materials and enlarges the material selection range. This application is based on including the cauldron body with keep interior synchronous stepping up between the cauldron body, with the pressure transmission of the internal cauldron body to the outer cauldron body, and the internal cauldron body itself does not bear the pressure or only bears a small amount of external pressure, consequently, the internal cauldron body only need accomplish corrosion-resistant can, because the heat-conducting liquid that sets up in the cavity can directly heat the internal cauldron body, the internal cauldron body is heated more evenly like this, realizes experimental required cauldron of high temperature and high pressure corrosion resistance.
Description
Technical Field
The invention belongs to the field of chemical engineering and laboratory detection, and particularly relates to a high-temperature high-pressure kettle used in a strong corrosion environment and a use method thereof.
Background
Materials such as hydrochloric acid, sulfuric acid, nitric acid and the like appear in the technical processes such as chlorination, sulfonation, flue gas desulfurization, denitration and the like in chemical production. However, since dilute hydrochloric acid, dilute sulfuric acid and nitric acid have strong corrosivity, in order to ensure safe and long-term operation of equipment, materials used in a corrosive environment need to be subjected to a material compatibility test in advance so as to determine whether the selected materials meet the use requirements. At present, the materials of high-temperature high-pressure autoclave for corrosion test in laboratory mainly include hastelloy, monel, titanium material, polytetrafluoroethylene, enamel and the like, but the use of each material is limited, for example, although polytetrafluoroethylene can resist corrosion of most chemical engineering media, the use temperature is within 200 ℃, and the pressure resistance is limited; the enamel material can resist corrosion, but the enamel layer is easy to generate porcelain exposure due to the action of thermal expansion and hydrogen; the metal material has more requirements on test media, different metals have different compatibility with corrosive media, kettles made of different materials are required to be selected according to the corrosivity of the media, and high-temperature high-pressure kettles made of the metal material can form corrosion products which are difficult to remove in the corrosion process, so that the cost is increased invisibly.
Disclosure of Invention
In order to overcome the defects of insufficient pressure resistance and corrosion resistance of the conventional high-temperature high-pressure kettle, the invention provides the high-temperature high-pressure kettle used in a strong corrosion environment and a using method thereof. The invention adopts the following technical scheme:
the utility model provides a high-temperature autoclave who uses under strong corrosive environment, includes outer cauldron subassembly and interior cauldron subassembly, outer cauldron subassembly includes outer cauldron body, outer cauldron lid, interior cauldron subassembly closes including the cover the internal interior cauldron body that just is used for placing the determinand of outer cauldron, lid and is located the interior cauldron lid of outer cauldron lid below, outer cauldron lid below is provided with the subassembly that hangs that is used for the interior cauldron body of elastic support, there is the gap of packing the heat-conducting liquid between the outer cauldron body and the interior cauldron body.
The method for using the high-temperature autoclave used in the strong corrosion environment comprises the following steps:
s1, placing the object to be tested on a sample hanger in the inner kettle body, then injecting a test solution into the inner kettle body, and placing the inner kettle body on a bearing part of the suspension assembly;
s2, butting the inner kettle body and the inner kettle cover, applying a certain pretightening force to seal the inner kettle body and the inner kettle cover, adjusting the length of a screw in the suspension assembly in the sleeve and locking the screw by a second fastening bolt, wherein the length ensures that a gap is formed between the bottom of the suspension assembly and the inner wall of the outer kettle body;
s3, directly placing the inner kettle into the outer kettle body by the outer kettle cover integrated with the inner kettle cover, inputting heat-conducting liquid between the outer kettle body and the inner kettle body to a certain depth and enabling the heat-conducting liquid to pass through an outlet of an air inlet pipe in the outer kettle body, covering the outer kettle cover and the outer kettle body, and locking and sealing the outer kettle cover and the outer kettle body;
s4, sealing the air inlet pipe of the inner kettle, the air outlet pipe of the inner kettle and the air outlet pipe of the outer kettle, and introducing inert gas into the outer kettle through the air inlet pipe of the outer kettle to perform an air tightness test so that the outer kettle and the inner kettle form a P '(P' is less than P)0，P0Can bear the maximum for the safe work of the inner kettleExternal pressure), maintaining the pressure for a set time, checking the change of the value of the pressure transmitter on the air pipe of the inner kettle to judge the tightness of the kettle, if the value of the pressure transmitter on the air pipe of the inner kettle rises, the inner kettle needs to be sealed again, and the step S2 is returned; if not, go to step S5;
s5, opening the air inlet pipe of the inner kettle, starting the interlocking program, and adjusting the pressure P in the outer kettleOuter coverWith the pressure P in the inner kettleInner partSet to interlock, guarantee PInner part≤POuter cover≤PInner part+ P', and introducing pressurized gas into the outer kettle and the inner kettle simultaneously; continuously adjusting the pressure in the outer kettle according to the pressure in the inner kettle, and keeping the relation between the pressure in the outer kettle and the pressure in the inner kettle to be POuter cover＝PInner part+ P', continuously increasing the pressure to the air tightness test pressure which is about 1.1 times of the test pressure, maintaining the pressure for a period of time, and observing the pressure P in the outer kettleOuter coverIf the pressure in the outer kettle is not reduced, the air tightness test of the outer kettle is passed, the pressure relief operation is carried out according to the requirement, and then the step S6 is carried out, if the air tightness test of the outer kettle is not passed, the step S3 is returned;
s6, connecting cooling water to a condenser coated on the exhaust pipes of the inner and outer kettles, and performing gas replacement and saturation on the test medium in the inner container according to the test requirement;
s7, heating; the heater is started to heat the outer kettle, the heat conducting liquid automatically transfers heat to the inner kettle, the test temperature is detected through the thermocouple in the inner kettle, the heating is carried out until the set temperature, the fluctuation in the set range is ensured, meanwhile, the change of the pressure difference between the inside and the outside is caused due to the temperature rise, the pressurizing gas is introduced into the outer kettle, and the relation between the pressure in the outer kettle and the pressure in the inner kettle is kept as PInner part≤POuter cover≤PInner part+ P', when the pressure generated by the temperature rise does not reach the test requirement, the step S8 is proceeded, if the pressure can reach the requirement, the test timing is started, and after the set test time, the step S9 is proceeded;
s8, synchronously pressurizing the inner kettle and the outer kettle to enable the pressure in the inner kettle to finally reach the test requirement, starting the test timing, and entering the step S9 after the set test time;
s9, after the test, the heating furnace stops heating, the device automatically cools, and when cooling, according to the cauldron internal pressure of interior cauldron, the solenoid valve on the outer cauldron blast pipe is opened in good time, realizes interior cauldron, outer cauldron synchronous step-down, guarantees PInner part≤POuter cover≤PInner part+ P', after the high temperature high pressure kettle is completely cooled, starting the inner kettle stop valve, after the gas in the inner kettle is exhausted, closing the interlocking program, starting the outer kettle stop valve, and exhausting the pressurized gas in the kettle;
and S10, opening a cover, taking the sample, opening the cover of the outer kettle, detaching the fixing piece on the inner kettle, taking down the inner kettle body, and taking out the sample.
The invention has the advantages that:
(1) the high-temperature high-pressure corrosion-resistant kettle with the double-layer structure reduces the requirement of the environment on materials and enlarges the material selection range. The pressure of the inner kettle body can be transmitted to the outer kettle body based on the synchronous pressure rise between the inner kettle body and the outer kettle body, and the inner kettle body does not bear pressure or only bears a small amount of external pressure, so that the inner kettle body only needs to be corrosion-resistant, and the heat conducting liquid arranged in the cavity can directly heat the outer kettle body, so that the inner kettle body is heated more uniformly, and the kettle which is required by a test and is resistant to high temperature and high pressure corrosion is realized.
(2) Can greatly reduce the consumption of corrosion-resistant metal, realize the multi-purpose function of one kettle and reduce the cost.
(3) The air inlet and outlet flow is accurately adjusted through each safety adjusting assembly and the measuring meter group, and the pressure of the inner kettle and the pressure of the outer kettle are adjusted.
(4) The thermocouple sleeve plays a role in protecting the thermocouple, and the condenser plays a role in cooling gas phases in the gas inlet pipe and the gas outlet pipe, so that the corrosion of a strong corrosive medium to the gas inlet pipe and the gas outlet pipe is reduced.
(5) The thermocouple sleeve can be communicated with the outer kettle exhaust pipe or the inner kettle exhaust pipe, so that the internal pressure and the external pressure of the thermocouple sleeve are balanced, and the thermocouple sleeve is prevented from being broken. In the present invention, it is preferable that the thermowell is communicable with the inner pot vent pipe.
(6) The top end of the spring is provided with a hemispherical or flat-plate-shaped bearing part for placing and bearing the inner kettle. The spring mainly prevents that the coefficient of expansion of inlayer container and pillar is different under the high temperature, realizes the compensation of pretightning force to guarantee interior cauldron sealed.
(7) The support and the screw rod are arranged to be suitable for different inner kettles and outer kettles, and are convenient to adjust.
(8) Different materials are adopted according to the environment of difference to outer cauldron in this application for the cauldron is more durable.
(9) The setting of the interlocking program in the using method ensures the use safety of the equipment.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Fig. 2 is a block diagram of a suspension assembly.
FIG. 3 is a top view of the support platform.
The notations in the figures have the following meanings:
11-outer kettle cover 12-sealing gasket 13-outer kettle body 14-first fastening bolt
15-outer kettle air inlet pipe
16-outer kettle first flow regulating valve 17-outer kettle first electromagnetic valve
18-outer kettle pressure measuring component 19-outer kettle safety valve
110-outer kettle rupture disk 111-outer kettle temperature thermocouple 112-outer kettle second flow regulating valve
113-outer kettle stop valve 114-outer kettle second electromagnetic valve
116-outer kettle thermowell 117-heating furnace 118-outer kettle condenser
119-outer kettle exhaust pipe
21-inner kettle cover 22-inner kettle sealing gasket 23-inner kettle body 24-hoop
25-inner kettle air inlet pipe 26-inner kettle first flow regulating valve 27-inner kettle first electromagnetic valve
28-inner kettle pressure measuring component 29-inner kettle safety valve 210-inner kettle rupture disk
211-inner kettle temperature thermocouple 2111-thermocouple pressure balance tube
212-inner kettle second flow regulating valve 213-inner kettle stop valve 214-inner kettle second electromagnetic valve
216-inner kettle thermowell 217-inner kettle first condenser
218-inner kettle second condenser 219-inner kettle vent pipe 220-sample hanger
221-support platform 222-bearing 223-spring 224-support
225-second fastening screw
Detailed Description
Example 1
As shown in fig. 1, a high-temperature autoclave used in a strong corrosion environment and a using method thereof include an outer kettle assembly and an inner kettle assembly, the outer kettle assembly includes an outer kettle body 13 and an outer kettle cover 11, the inner kettle assembly includes an inner kettle body 23 which is sleeved in the outer kettle body 13 and used for placing an object to be tested, an inner kettle cover 21 which covers the inner kettle body 23 and is positioned below the outer kettle cover 11, a hanging assembly used for elastically supporting the inner kettle body 23 is arranged below the outer kettle cover 11, and a gap for filling a heat-conducting liquid is formed between the outer kettle body 13 and the inner kettle body 23. For testing, the high temperature autoclave was placed in a furnace 117. The heat-conducting liquid enables the inner kettle to be heated uniformly.
The inner kettle is provided with a sample hanging rack, so that different placing positions can be selected for samples according to the solution amount in the inner kettle and the experiment requirements.
The outer kettle body 13 and the outer kettle cover 11 are made of metal materials, and the inner kettle body 23 and the inner kettle cover 21 are made of corrosion-resistant and high-temperature-resistant materials. Specifically, the outer kettle body 13 and the outer kettle cover 11 are made of one of carbon steel, alloy steel, stainless steel and corrosion-resistant alloy; when the use temperature is within 200 ℃, the inner kettle body 23 and the inner kettle cover 21 are made of polytetrafluoroethylene or other corrosion-resistant materials, when the use temperature is above 200 ℃, the inner kettle body 23 and the inner kettle cover 21 are made of glass, and when the use temperature is in a strong alkaline environment, a hydrofluoric acid-containing environment and a non-corrosion-resistant environment, the inner kettle body 23 and the inner kettle cover 21 are made of Monel alloy and other corrosion-resistant materials.
The kettle cover is provided with an air inlet pipe, an exhaust pipe and a temperature measurement assembly, the end parts of the air inlet pipe and the exhaust pipe outside the kettle are provided with a safety regulation assembly and a measurement meter assembly, and the end parts of the air inlet pipe, the exhaust pipe and the temperature measurement assembly on the inner kettle cover 21 outside the kettle penetrate through the outer kettle cover 11. The safety regulating assembly comprises an air inlet flow regulating valve, an air inlet electromagnetic valve, a safety valve and a rupture disk which are arranged on an air inlet pipe, and the measuring meter group on the exhaust pipe comprises an exhaust flow regulating valve, an exhaust electromagnetic valve and an exhaust stop valve arranged on a branch pipeline of the exhaust pipe; the measuring meter group comprises a pressure meter and a transmitter which are arranged on the air inlet pipe, and the pressure of the inner kettle and the pressure of the outer kettle are adjusted by adjusting the air inlet and outlet flow. The temperature measuring component comprises thermocouples extending into the inner kettle and the outer kettle and thermocouple sleeves sleeved on the outer walls of the thermocouples, specifically, the inner kettle temperature measuring thermocouples extending into the inner kettle body, the inner kettle thermocouple sleeves arranged on the outer side of the inner kettle temperature measuring thermocouples, the outer kettle temperature measuring thermocouples extending into the outer kettle body and the outer kettle thermocouple sleeves arranged on the outer side of the outer kettle temperature measuring thermocouples. The inner kettle thermocouple sleeve can be communicated with the outer kettle exhaust pipe or the inner kettle exhaust pipe through a thermocouple pressure balance pipe, so that the internal pressure and the external pressure of the inner kettle thermocouple sleeve are balanced, and the inner kettle thermocouple sleeve is prevented from being broken. In this embodiment, it is preferable that the inner pot thermowell is communicated with the inner pot vent pipe.
Specifically, as shown in fig. 1, the outer kettle cover 11 is provided with an outer kettle gas inlet pipe 15 and an outer kettle gas outlet pipe 119, and the outer kettle gas inlet pipe 15 and the outer kettle gas outlet pipe 119 are located at two sides of the inner kettle body 23, the lower end of the outer kettle gas inlet pipe 25 is close to the bottom of the outer kettle body 13, and the outer kettle gas outlet pipe 119 is located inside the cavity of the outer kettle body 13 and flush with the bottom of the outer kettle cover 11. And the outer end part of the outer kettle air inlet pipe 15 is provided with an outer kettle first flow regulating valve 16, an outer kettle first electromagnetic valve 17, an outer kettle pressure measuring component 18, an outer kettle safety valve 19 and an outer kettle rupture disc 110. And an outer kettle second flow regulating valve 112, an outer kettle stop valve 113 and an outer kettle second electromagnetic valve 114 are arranged at the outer end part of the outer kettle exhaust pipe 119. An outer kettle condenser 118 is arranged on the outer kettle exhaust pipe 119, and an outer kettle temperature thermocouple 111 extending into the outer kettle body 13 and an outer kettle thermocouple well 116 sleeved on the outer surface of the outer kettle temperature thermocouple well are arranged on the outer kettle cover 11. The outer kettle pressure measuring assembly 18 includes an outer kettle pressure gauge and a pressure transmitter.
The same, be provided with interior cauldron intake pipe 25 and interior cauldron blast pipe 219 on the interior cauldron cover 21, the lower tip of interior cauldron intake pipe 25 is close to the bottom of the interior cauldron body 23, interior cauldron blast pipe 219 is located the inside in the interior cauldron body 23 chamber and with the bottom parallel and level of interior cauldron cover 21. The outer end part of the inner kettle air inlet pipe 25 is provided with an inner kettle first flow regulating valve 26, an inner kettle first electromagnetic valve 27, an inner kettle pressure measuring assembly 28, an inner kettle safety valve 29 and an inner kettle rupture disk 210. And the outer end part of the inner kettle exhaust pipe is provided with an inner kettle second flow regulating valve 212, an inner kettle stop valve 213 and an inner kettle second electromagnetic valve 214. An inner kettle first condenser 217 is arranged on the inner kettle air inlet pipe 25, an inner kettle second condenser 218 is arranged on the inner kettle air outlet pipe 219, and an inner kettle temperature measuring thermocouple 211 stretching into the inner kettle body 23 and an inner kettle thermocouple well 216 sleeved on the inner surface of the inner kettle temperature measuring thermocouple well are arranged on the inner kettle cover 21. The inner kettle pressure measuring assembly 28 comprises an inner kettle pressure gauge and a pressure transmitter.
The inner kettle temperature thermocouple 211 comprises a thermocouple and a thermocouple pressure balance pipe 2111 arranged on the outer kettle cover 11. Inner kettle thermowell 216 on inner kettle cover 21 may be in communication with outer kettle vent pipe 119 or inner kettle vent pipe 219, preferably inner kettle vent pipe 219, such that the internal and external pressures of the thermowell are balanced to prevent thermowell rupture.
In order to realize the sealing performance of the outer kettle body 13 and the outer kettle cover 11, a sealing gasket 12 for sealing is arranged between the outer kettle body 13 and the outer kettle cover 11, and then sealing is realized by applying a certain pretightening force and then fixing by using a first fastening bolt 14. In order to realize the sealing of the inner kettle body 23 and the inner kettle cover 21, an inner kettle sealing gasket 22 is arranged between the inner kettle body 23 and the inner kettle cover 21, and then the sealing is realized through the fixing of a clamp 24.
As shown in fig. 2-3, the suspension assembly includes a support platform 221, and a support post 224 for suspending the support platform 221 at the bottom of the outer kettle cover 11, wherein 3 or 4 screws are fixed on the support platform, and are annularly arranged at the outer edge of the support platform 221, the support post 224 includes 3 or 4 sleeves corresponding to the screws, and respectively correspond to the screws, two ends of the corresponding sleeves are respectively in threaded connection with the screws on the outer kettle cover 11 and the support platform 221, a second fastening bolt 225 capable of abutting against the screws is further provided in the vertical direction of the sleeves, and the second fastening bolt 225 is locked to determine the length of the support post 224. The middle part of the platform is provided with a spring 223, and a supporting part 222 at the bottom of the inner kettle body 23 is supported above the spring 223. The support portion 222 is shaped like a hemisphere or a flat plate. The spring 223 is mainly used for preventing the expansion coefficients of the inner container and the support post 224 from being different at high temperature, so that the pre-tightening force is compensated, and the sealing of the inner kettle is ensured.
Example 2
The method of using the high-temperature autoclave used in the strongly corrosive environment and the method of using the same described in example 1 were used to perform the uniform corrosion resistance measurement of the super austenitic stainless steel in a 30% sulfuric acid solution at 300 ℃ and 9MPa as required. The method comprises the following steps:
s1, cleaning and drying the test sample, measuring several sizes and masses of the test sample, preparing a sulfuric acid solution with the mass fraction of 30%, calculating the required solution amount according to the surface area of the test sample, placing the object to be tested on a sample hanger in the inner kettle body 23, then injecting the test solution into the inner kettle body 23, and placing the inner kettle body 23 on a bearing part 222 of the suspension assembly;
s2, butting the inner kettle body 23 and the inner kettle cover 21, applying a certain pretightening force to seal the inner kettle body 23 and the inner kettle cover 21, adjusting the length of a screw in the suspension assembly in the sleeve and locking the screw by using a second fastening bolt 225, wherein the length ensures that a gap is formed between the bottom of the suspension assembly and the inner wall of the outer kettle body 13;
s3, directly placing the inner kettle into the outer kettle body 13 through the outer kettle cover 11 integrated with the inner kettle cover 21, inputting heat-conducting liquid between the outer kettle body 13 and the inner kettle body 23 to a certain depth and enabling the heat-conducting liquid to pass through an outlet of an air inlet pipe in the outer kettle body 13, covering the outer kettle cover 11 and the outer kettle body 13, and locking and sealing;
s4, sealing an air inlet pipe 25 of the inner kettle, an air outlet pipe 219 of the inner kettle and an air outlet pipe 119 of the outer kettle, introducing inert gas into the outer kettle 13 through the air inlet pipe of the outer kettle 13 to perform an air tightness test, so that a pressure difference P 'is formed between the outer kettle and the inner kettle, setting the pressure difference P' between the inside and the outside of the inner kettle to be 0.3MPa, introducing the inert gas of 0.3MPa into the outer kettle, maintaining the pressure for a set time, checking whether the value of a pressure transmitter on the air inlet pipe of the inner kettle changes to judge the tightness of the inner kettle, if the value of the pressure transmitter on the air inlet pipe of the inner kettle rises, resealing the inner kettle, returning to the step S2, and if the value of the pressure transmitter on the air inlet pipe of the inner kettle does not change, entering the step S5;
s5, opening the air inlet pipe of the inner kettle, starting the interlocking program, and adjusting the pressure P in the outer kettleOuter coverWith the pressure P in the inner kettleInner partSet to interlock, guarantee PInner part≤POuter cover≤PInner part+ P', and introducing pressurized gas into the outer kettle and the inner kettle simultaneously; continuously adjusting the pressure in the outer kettle according to the pressure in the inner kettle, and keeping the relation between the pressure in the outer kettle and the pressure in the inner kettle to be POuter cover＝PInner part+ P', the saturated vapor pressure of water at 300 ℃ is about 9MPa, so the pressure of the air tightness test is 10-11 MPa. After the pressure maintaining is carried out for a set time, observing the pressure P in the outer kettleOuter coverIf the pressure P in the outer kettle is changedOuter coverIf the fluctuation occurs, the leakage of the outer kettle is indicated, the step is returned to S3, otherwise, the step is carried out S6;
s6, connecting cooling water to condensers coated on the outer kettle exhaust pipe 119, the inner kettle air inlet pipe 25 and the inner kettle exhaust pipe 219, and performing gas replacement and saturation on the test medium in the inner container according to test requirements;
s7, heating; opening the outer kettle first flow regulating valve 16, the inner kettle first flow regulating valve 26, the outer kettle second flow regulating valve 112 and the inner kettle second flow regulating valve 212, and setting the pressure difference P' between the inside and the outside of the inner kettle to 0.3MPa, the test temperature T to 300 ℃, the test pressure P to 9MPa, the test period T to 168h and the overtemperature alarm value TSuper-super310 deg.C, overpressure alarm value PSuper-superStarting a heating and boosting program, automatically raising the temperature of the control program to a set test temperature according to the setting, entering a step S8 when the pressure generated by temperature rise does not meet the test requirement, if the test requirement can be met, starting test timing, and entering a step S9 after the set test time;
s8, synchronously pressurizing the inner kettle and the outer kettle to enable the pressure in the inner kettle to finally reach the test requirement, starting the test timing, and entering the step S9 after the set time; the inner kettle theoretically can be heated up first and then boosted and can be heated up first and then boosted, preferably, the inner kettle is heated up first and then boosted, and the outer kettle is synchronously boosted along with the boosting of the inner kettle.
S9, after the test is finished, the heating furnace stops heating, the device automatically cools, and when cooling, according to the pressure in the inner kettle, the second electromagnetic valve 214 on the outer kettle exhaust pipe 119 is timely opened, so that synchronous pressure reduction of the inner kettle and the outer kettle is realized, and P is ensuredInner part≤POuter cover≤PInner part+ P', after the high-temperature high-pressure kettle is completely cooled, starting the inner kettle stop valve 213, after the gas in the inner kettle is exhausted, closing the interlocking program, starting the outer kettle stop valve 113, and exhausting the pressurized gas in the kettle; specifically, after the test period is reached, the heating furnace 117 is powered off, the first electromagnetic valve 17 of the outer kettle and the first electromagnetic valve 27 of the inner kettle are closed, the high-temperature high-pressure kettle enters a natural cooling and pressure relief link, and the control system can perform the steps according to the pressure P of the inner kettleInner partThe pressure P in the outer kettle is adjusted by controlling the opening and closing of the second electromagnetic valve 114 of the outer kettleOuter coverLet P standOuter cover＝PInner part+ P', when the temperature of the inner kettle is reduced to 30 ℃, the stop valve 213 of the inner kettle on the exhaust pipe of the inner kettle is opened to discharge the gas in the inner kettle, and the gas in the outer kettle is also discharged synchronously through the exhaust pipe 119 of the outer kettle according to the interlocking relationship. And after the gas in the inner kettle is exhausted, closing the interlocking program. And then the outer kettle stop valve 113 on the outer kettle exhaust pipe 119 is opened to exhaust the gas in the outer kettle.
And S10, opening the cover, taking the sample, opening the outer kettle cover 11, detaching the fixing piece on the inner kettle, taking down the inner kettle body, and taking out the sample. Weighing after cleaning and blow-drying, calculating the corrosion rate according to the mass change before and after the test, cleaning the inner kettle, then airing, and carefully collecting.
The invention is not to be considered as limited to the specific embodiments shown and described, but is to be understood to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The utility model provides a high-temperature high-pressure kettle who uses under strong corrosive environment, its characterized in that, includes outer cauldron subassembly and interior cauldron subassembly, outer cauldron subassembly includes the outer cauldron body (13), outer cauldron lid (11), interior cauldron subassembly closes including the cover in the outer cauldron body (13) and be used for placing interior cauldron body (23), the lid of determinand and interior cauldron lid (21) that just are located outer cauldron lid (11) below, outer cauldron lid (11) below is provided with the subassembly that hangs that is used for the interior cauldron body (23) of elastic support, there is the gap of packing heat-conducting liquid between the outer cauldron body (13) and the interior cauldron body (23).
2. The autoclave used in the highly corrosive environment according to claim 1, wherein the outer kettle body (13) and the outer kettle cover (11) are made of metal, and the inner kettle body (23) and the inner kettle cover (21) are made of corrosion-resistant and high temperature-resistant materials.
3. The high-temperature high-pressure kettle used in the strong corrosion environment according to claim 1, wherein the kettle cover is provided with an air inlet pipe, an air outlet pipe and a temperature measuring component, the end parts of the air inlet pipe and the air outlet pipe outside the kettle are provided with a safety regulating component and a measuring meter group, and the end parts of the air inlet pipe, the air outlet pipe and the temperature measuring component outside the kettle on the inner kettle cover (21) penetrate through the outer kettle cover (11).
4. The autoclave of claim 3, wherein the safety regulating assembly comprises an inlet flow regulating valve, an inlet solenoid valve, a safety valve, a rupture disk arranged on an inlet pipe, the measuring gauge set on the outlet pipe comprises an exhaust flow regulating valve, an exhaust solenoid valve, and an exhaust stop valve arranged on an outlet pipe branch line; the measuring gauge group comprises a pressure gauge and a pressure transmitter which are arranged on the air inlet pipe.
5. The autoclave used in the strongly corrosive environment according to claim 4, wherein condensers are arranged on the inner kettle exhaust pipe (219) and the inner kettle intake pipe (25), and the temperature measurement assembly comprises a thermocouple extending into the inner and outer kettles and a thermowell sleeved on the outer wall of the thermocouple.
6. A high-temperature autoclave used in a highly corrosive environment according to claim 4, wherein said thermowell is in communication with inner vessel vent pipe (219) or outer vessel vent pipe (119).
7. The autoclave for use in a highly corrosive environment according to claim 1, wherein the suspension assembly comprises a support platform (221), a support column (224) for suspending the support platform (221) from the bottom of the outer vessel cover (11), the support platform being provided with a spring (223), and a support portion (222) for supporting the bottom of the inner vessel body (23) is provided above the spring (223).
8. The autoclave used in the highly corrosive environment according to claim 7, wherein a plurality of screws are fixed on the supporting platform, the support column (224) comprises a plurality of sleeves, two ends of the corresponding sleeves are respectively in threaded connection with the screws on the outer pot cover (11) and the supporting platform (221), and second fastening bolts (225) capable of abutting against the screws are further arranged in the vertical direction of the sleeves.
9. The autoclave used in the highly corrosive environment according to claim 2, wherein the outer vessel body (13) and the outer vessel cover (11) are made of one of carbon steel, alloy steel, stainless steel and corrosion resistant alloy; when the use temperature is within 200 ℃, the inner kettle body (23) and the inner kettle cover (21) are made of polytetrafluoroethylene, when the use temperature is above 200 ℃, the inner kettle body (23) and the inner kettle cover (21) are made of quartz glass, and when the use temperature is in a strong alkaline environment, a hydrofluoric acid-containing environment and a weak corrosive environment, the inner kettle body (23) and the inner kettle cover (21) are made of Monel alloy and the like.
10. A method of using a high temperature autoclave for use in a highly corrosive environment according to any of claims 1 to 9, comprising the steps of:
s1, placing the object to be tested on the sample hanger (220) in the inner kettle body (23), then injecting a test solution into the inner kettle body (23), and placing the inner kettle body (23) on the bearing part (222) of the suspension assembly;
s2, butting the inner kettle body (23) and the inner kettle cover (21), applying a certain pretightening force to seal the inner kettle body (23) and the inner kettle cover (21), adjusting the length of a screw in the suspension assembly in the sleeve and locking the screw by a second fastening bolt (225), wherein the length ensures that a gap is formed between the bottom of the suspension assembly and the inner wall of the outer kettle body (13);
s3, directly placing the inner kettle into the outer kettle body (13) through the outer kettle cover (11) integrated with the inner kettle cover (21), inputting heat-conducting liquid between the outer kettle body (13) and the inner kettle body (23) to a certain depth and enabling the heat-conducting liquid to pass through an outlet of an air inlet pipe in the outer kettle body (13), and covering the outer kettle cover (11) and the outer kettle body (13) and locking and sealing the outer kettle cover (11) and the outer kettle body (13);
s4, sealing an inner kettle air inlet pipe (25), an inner kettle air outlet pipe (219) and an outer kettle air outlet pipe (119), introducing inert gas into the outer kettle body (13) through the outer kettle body (13) air inlet pipe to carry out an air tightness test, so that the outer kettle and the inner kettle form a P ', (P' < P)0，P0Maximum external pressure which can be borne by the inner kettle during safe operation), maintaining the pressure for a set time, checking the change of the value of the pressure transmitter on the air pipe of the inner kettle to judge the tightness of the kettle, if the value of the pressure transmitter on the air inlet pipe (25) of the inner kettle rises, the inner kettle needs to be sealed again, and the step S2 is returned; if not, go to step S5;
s5, opening the air inlet pipe (25) of the inner kettle, starting the interlocking program, and connecting the pressure P in the outer kettleOuter coverWith the pressure P in the inner kettleInner partSet to interlock, guarantee PInner part≤POuter cover≤PInner part+ P', and introducing pressurized gas into the outer kettle and the inner kettle simultaneously; continuously adjusting the pressure in the outer kettle according to the pressure in the inner kettle, and keeping the relation between the pressure in the outer kettle and the pressure in the inner kettle to be POuter cover＝PInner part+ P', continuously increasing the pressure to the air tightness test pressure, maintaining the pressure for a period of time, and observing the pressure P in the outer kettleOuter coverIf the pressure in the outer kettle is not reduced, the air tightness test of the outer kettle is passed, the pressure relief operation is carried out according to the requirement, and then the step S6 is carried out, if the air tightness test of the outer kettle is not passed, the step S3 is carried out;
s6, connecting cooling water to a condenser coated on an exhaust pipe (119) of the inner and outer kettles, and performing gas replacement and saturation on the test medium in the inner container according to test requirements;
s7, heating; the heater is started to heat the outer kettle, the heat conducting liquid automatically transfers heat to the inner kettle, the test temperature is detected through the thermocouple in the inner kettle, the heating is carried out until the set temperature, the fluctuation in the set range is ensured, meanwhile, the change of the pressure difference between the inside and the outside is caused due to the temperature rise, the pressurizing gas is introduced into the outer kettle, and the relation between the pressure in the outer kettle and the pressure in the inner kettle is kept as PInner part≤POuter cover≤PInner part+ P', when the pressure generated by the temperature rise does not reach the test requirement, the step S8 is proceeded, if the pressure can reach the requirement, the test timing is started, and after the set test time, the step S9 is proceeded;
s8, synchronously pressurizing the inner kettle and the outer kettle to enable the pressure in the inner kettle to finally reach the test requirement, starting the test timing, and entering the step S9 after the set test time;
s9, after the test is finished, the heating furnace (117) stops heating, the device automatically cools down, and when cooling, according to the pressure in the inner kettle, the electromagnetic valve on the exhaust pipe (119) of the outer kettle is timely opened, so that synchronous pressure reduction of the inner kettle and the outer kettle is realized, and P is ensuredInner part≤POuter cover≤PInner part+ P', after the high-temperature high-pressure kettle is completely cooled, starting an inner kettle stop valve (213), after the gas in the inner kettle is exhausted, closing an interlocking program, starting an outer kettle stop valve (113) again, and exhausting the pressurized gas in the kettle;
and S10, opening the cover, taking the sample, opening the outer kettle cover (11), detaching the fixing piece on the inner kettle, taking down the inner kettle body (23), and taking out the sample.
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Cited By (1)
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| TWI863277B (en) * | 2023-05-16 | 2024-11-21 | 藍星材料股份有限公司 | Autoclave reactor for reaction under autogenic pressure at elevated temperature |
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