CN113522167B - 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 PDF

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Publication number
CN113522167B
CN113522167B CN202110555230.4A CN202110555230A CN113522167B CN 113522167 B CN113522167 B CN 113522167B CN 202110555230 A CN202110555230 A CN 202110555230A CN 113522167 B CN113522167 B CN 113522167B
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kettle
pressure
kettle body
inner kettle
cover
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CN113522167A (en
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张强
陈学东
范志超
陈炜
陈涛
孔韦海
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Hefei General Machinery Research Institute Special Equipment Inspection Station Co ltd
Hefei General Machinery Research Institute Co Ltd
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Hefei General Machinery Research Institute Special Equipment Inspection Station Co ltd
Hefei General Machinery Research Institute Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/02Apparatus characterised by being constructed of material selected for its chemically-resistant properties
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01DMEASURING 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
    • G01D21/00Measuring or testing not otherwise provided for
    • G01D21/02Measuring two or more variables by means not covered by a single other subclass
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01MTESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00Investigating fluid-tightness of structures
    • G01M3/02Investigating fluid-tightness of structures by using fluid or vacuum
    • G01M3/26Investigating 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
    • G01M3/32Investigating 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
    • G01M3/3236Investigating 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
    • G01M3/3272Investigating 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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)

Abstract

The utility model provides a high temperature autoclave that uses under strong corrosion environment, includes outer cauldron subassembly and interior cauldron subassembly, and outer cauldron subassembly includes outer cauldron body, outer cauldron lid, and interior cauldron subassembly is including the cover in outer internal and be used for placing the interior cauldron body of object to be tested, lid close including internal and be located the interior cauldron lid of outer cauldron lid below, outer cauldron lid below is provided with the suspension element that is used for the internal cauldron of elastic support, has the gap of packing the heat conduction liquid between the internal and the external cauldron of outer cauldron. The double-layer structure high-temperature high-pressure corrosion-resistant kettle designed by the application reduces the requirement of the environment on materials and expands the material selection range. The application is based on keeping internal synchronous boost between the inner kettle body and the outer kettle body, transmitting the pressure of the inner kettle body to the outer kettle body, and the inner kettle body is not bearing pressure or only bearing a small amount of external pressure, therefore, the inner kettle body only needs to be corrosion-resistant, and the heat conducting liquid arranged in the cavity can directly heat the inner kettle body, so that the inner kettle body is heated more uniformly, and the kettle with high temperature and high pressure corrosion resistance required by the test is realized.

Description

High-temperature high-pressure kettle used in strong corrosion environment and use method
Technical Field
The application belongs to the field of chemical industry 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
In the chemical production, 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. However, because dilute hydrochloric acid, dilute sulfuric acid and nitric acid are relatively strong in corrosiveness, materials used in corrosive environments need to be subjected to a material compatibility test to determine whether the selected materials meet the use requirements or not in order to ensure safe and long-period operation of equipment. The materials of the high-temperature high-pressure kettle for corrosion test in the laboratory at present mainly comprise hastelloy, monel alloy, titanium, polytetrafluoroethylene, enamel and the like, but each material has the limit, for example, the polytetrafluoroethylene can resist most chemical medium corrosion, but the use temperature is within 200 ℃ and the pressure resistance is limited; the enamel material can resist corrosion, but the enamel layer is extremely easy to be subjected to porcelain explosion due to the effects of thermal expansion and hydrogen; the metal material has more requirements on the test medium, the compatibility of different metals on the corrosive medium is different, kettles with different materials are required to be selected according to the corrosiveness of the medium, and the high-temperature high-pressure kettle with the metal material can form corrosion products which are difficult to remove in the corrosion process, so that the cost is increased intangibly.
Disclosure of Invention
In order to overcome the defect of insufficient pressure resistance and corrosion resistance of the existing high-temperature high-pressure kettle, the application provides the high-temperature high-pressure kettle used in a strong corrosion environment and the use method thereof. The application adopts the following technical scheme:
the utility model provides a high temperature autoclave that uses under strong corrosion environment, includes outer cauldron subassembly and interior cauldron subassembly, outer cauldron subassembly includes outer cauldron body, outer cauldron lid, interior cauldron subassembly is including the cover in outer internal and be used for placing the interior cauldron body, the lid of the lid on the internal and be located outer cauldron lid below of the thing that awaits measuring of outer cauldron, outer cauldron lid below is provided with the suspension element that is used for the internal cauldron of elastic support, there is the gap of packing heat conduction liquid between the internal and the internal cauldron of outer cauldron.
The method for using the high-temperature high-pressure kettle used in the strong corrosion environment comprises the following steps:
s1, placing an object to be tested on a sample hanger in an inner kettle body, then injecting test solution into the inner kettle body, and placing the inner kettle body on a bearing part of a 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 rod in the suspension assembly in the sleeve and locking the screw rod by a second fastening bolt, wherein the length ensures that a gap exists between the bottom of the suspension assembly and the inner wall of the outer kettle body;
s3, an outer kettle cover integrated with the inner kettle cover directly places the inner kettle into the outer kettle body, heat conduction liquid is input between the outer kettle body and the inner kettle body to a certain depth and passes through an air inlet pipe outlet in the outer kettle body, and the outer kettle cover and the outer kettle body are covered and locked and sealed;
s4, sealing an inner kettle air inlet pipe, an inner kettle air outlet pipe and an outer kettle air outlet pipe, and introducing inert gas into the outer kettle body through an outer kettle body air inlet pipe to perform an air tightness test, so that the outer kettle and the inner kettle form a P '(P' < P) 0 ,P 0 Maximum external pressure which can be born by the safe operation of the inner kettle), 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, and if the value of the pressure transmitter on the air inlet pipe of the inner kettle is increased, re-sealing the inner kettle is needed, and returning to the step S2; if not, entering step S5;
s5, opening an air inlet pipe of the inner kettle, starting an interlocking program, and enabling the pressure P in the outer kettle to be equal to the pressure P in the outer kettle Outer part With the pressure P in the inner kettle Inner part Is arranged to interlock to ensure P Inner part ≤P Outer part ≤P Inner part +P', and simultaneously introducing pressurized gas into the outer kettle and the inner kettle; 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 as P Outer part =P Inner part +P', continue boosting toThe airtight test pressure is about 1.1 times of the test pressure, the pressure is maintained for a period of time, and the pressure P in the outer kettle is observed Outer part Changing, if the pressure in the outer kettle is not reduced, the air tightness test of the outer kettle passes, pressure relief operation is carried out according to the requirement, then the step S6 is carried out, and if the air tightness test of the outer kettle does not pass, the step S3 is returned;
s6, cooling water is communicated with a condenser coated on the exhaust pipes of the inner kettle and the outer kettle, and the test medium in the inner container is subjected to gas replacement and saturation according to test requirements;
s7, heating; starting a heater to heat the outer kettle, automatically transferring heat to the inner kettle by the heat conducting liquid, detecting test temperature through a thermocouple in the inner kettle, heating until the set temperature, ensuring fluctuation in a set range, simultaneously introducing pressurized gas into the outer kettle due to the change of internal and external pressure difference caused by temperature rise, and keeping the relation between the internal pressure of the outer kettle and the internal pressure of the inner kettle as P Inner part ≤P Outer part ≤P Inner part When the pressure generated by the temperature rise does not meet the test requirement, the step S8 is carried out, if the pressure can meet the test requirement, the test timing is started, and after the set test time, the step S9 is carried out;
s8, pressurizing the inner kettle and the outer kettle synchronously to enable the pressure in the inner kettle to finally meet the test requirement, starting test timing, and entering a step S9 after the set test time;
s9, after the test is finished, the heating furnace stops heating, the device automatically cools, and when the temperature is lowered, the electromagnetic valve on the exhaust pipe of the outer kettle is timely opened according to the pressure in the kettle of the inner kettle, so that the synchronous depressurization of the inner kettle and the outer kettle is realized, and P is ensured Inner part ≤P Outer part ≤P Inner part +P', after the high-temperature high-pressure kettle is completely cooled, starting an inner kettle stop valve, after the gas in the inner kettle is exhausted, closing an interlocking procedure, starting an outer kettle stop valve, and exhausting pressurized gas in the kettle;
s10, uncovering, taking a sample, opening an outer kettle cover, removing a fixing piece on the inner kettle, taking down the inner kettle body, and then taking out the sample.
The application has the advantages that:
(1) The double-layer structure high-temperature high-pressure corrosion-resistant kettle designed by the application reduces the requirement of the environment on materials and expands the material selection range. The application is based on keeping synchronous boost between the inner kettle body and the outer kettle body, and can transfer the pressure of the inner kettle body to the outer kettle body, while the inner kettle body is not bearing pressure or only bears a small amount of external pressure, therefore, 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 with high temperature and high pressure corrosion resistance required by the test is realized.
(2) The consumption of corrosion-resistant metal can be greatly reduced, the multi-purpose function of one kettle can be realized, and the cost is reduced.
(3) The application accurately adjusts the air inlet and outlet flow through each safety adjusting component and the measuring meter group, and adjusts the pressure of the inner kettle and the outer kettle.
(4) The thermowell plays a role in protecting a thermocouple, the condenser plays a role in cooling gas phases in the inlet pipe and the exhaust pipe, and corrosion of a strong corrosion medium to the inlet pipe and the exhaust pipe is reduced.
(5) The thermowell may communicate with an external kettle exhaust pipe or an internal kettle exhaust pipe such that the internal pressure and the external pressure of the thermowell are balanced, preventing the thermowell from being broken. In the present application, it is preferable that the thermowell is communicable with the inner tank vent pipe.
(6) The top end of the spring is provided with a hemispherical or flat bearing part for placing and bearing the inner kettle. The spring mainly prevents the expansion coefficients of the inner container and the support column from being different at high temperature, and realizes the compensation of pretightening force, thereby ensuring the sealing of the inner kettle.
(7) The setting of pillar and screw rod can be applicable to different inside and outside cauldron to conveniently adjust.
(8) According to the application, the inner kettle and the outer kettle are made of different materials according to different environments, so that the kettles are 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 view of the present application.
Fig. 2 is a block diagram of a suspension assembly.
Fig. 3 is a top view of the support platform.
The meaning of the reference symbols in the figures is as follows:
11-an outer kettle cover 12-a sealing gasket 13-an outer kettle body 14-a first fastening bolt
15-outer kettle air inlet pipe
16-first flow regulating valve of outer kettle 17-first electromagnetic valve of outer kettle
18-outer cauldron pressure measurement subassembly 19-outer cauldron relief valve
110-outer kettle rupture disk 111-outer kettle temperature thermocouple 112-outer kettle second flow regulating valve
113-external kettle stop valve 114-external 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 gasket 23-inner kettle body 24-clamp
25-inner kettle air inlet pipe 26-inner kettle first flow regulating valve 27-inner kettle first electromagnetic valve
28-inner tank pressure measurement assembly 29-inner tank safety valve 210-inner tank rupture disk
211-inner kettle temperature thermocouple 2111-thermocouple pressure balance pipe
212-inner kettle second flow regulating valve 213-inner kettle stop valve 214-inner kettle second electromagnetic valve
216-inner tank thermowell 217-inner tank first condenser
218-inner kettle second condenser 219-inner kettle exhaust pipe 220-sample hanging rack
221-support platform 222-bearing 223-spring 224-support column
225-second fastening bolt
Detailed Description
Example 1
As shown in FIG. 1, the high-temperature high-pressure kettle used in a strong corrosion environment and the use method thereof comprise an outer kettle assembly and an inner kettle assembly, wherein the outer kettle assembly comprises an outer kettle body 13 and an outer kettle cover 11, the inner kettle assembly comprises an inner kettle body 23 sleeved in the outer kettle body 13 and used for placing objects to be tested, and an inner kettle cover 21 covered on the inner kettle body 23 and positioned below the outer kettle cover 11, a suspension assembly used for elastically supporting the inner kettle body 23 is arranged below the outer kettle cover 11, and a gap filled with heat conducting liquid is reserved between the outer kettle body 13 and the inner kettle body 23. For the test, the autoclave was placed in a furnace 117. The heat conducting liquid makes the inner kettle heated uniformly.
The sample hanger is arranged in the inner kettle, so that samples can be selected to be placed at different positions according to the solution quantity in the inner kettle and experimental 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 material selected from 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 prepared by 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 prepared by glass, and when the use temperature is within the strong alkaline environment, the hydrofluoric acid-containing environment and the glass corrosion-resistant environment, the inner kettle body 23 and the inner kettle cover 21 are prepared by Monel alloy or other corrosion-resistant materials.
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 adjusting component and a measuring meter group, and the end parts of the air inlet pipe, the air outlet pipe and the temperature measuring component 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 the air inlet pipe, the measuring meter group on the exhaust pipe comprises an exhaust flow regulating valve and an exhaust electromagnetic valve, and the safety regulating assembly also comprises 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 outer kettle is adjusted by adjusting the air inlet and outlet flow. The temperature measuring assembly comprises thermocouples extending into the inner kettle and the outer kettle and thermowells sleeved on the outer walls of the thermocouples, specifically, the inner kettle temperature measuring thermocouples extending into the inner kettle body and the inner kettle thermowells arranged outside the inner kettle temperature measuring thermocouples, the outer kettle temperature measuring thermocouples extending into the outer kettle body and the outer kettle thermowells arranged outside the outer kettle thermowells. The inner kettle thermowell can be communicated with the outer kettle exhaust pipe or the inner kettle exhaust pipe through a thermocouple pressure balance pipe, so that the inner pressure and the outer pressure of the inner kettle thermowell are balanced, and the inner kettle thermowell is prevented from being broken. In this embodiment, the inner tank thermowell is preferably in communication with the inner tank vent pipe.
Specifically, as shown in fig. 1, the outer tank cover 11 is provided with an outer tank air inlet pipe 15 and an outer tank air outlet pipe 119, and is located at two sides of the inner tank body 23, the lower end of the outer tank air inlet pipe 25 is close to the bottom of the outer tank body 13, and the outer tank air outlet pipe 119 is located inside the cavity of the outer tank body 13 and is flush with the bottom of the outer tank cover 11. 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 assembly 18, an outer kettle safety valve 19 and an outer kettle rupture disk 110. An outer tank second flow regulating valve 112, an outer tank stop valve 113 and an outer tank second electromagnetic valve 114 are arranged on the outer end part of the outer tank exhaust pipe 119. An outer kettle condenser 118 is arranged on the outer kettle exhaust pipe 119, and an outer kettle thermocouple 111 extending into the outer kettle body 13 and an outer kettle thermowell 116 sleeved on the outer surface of the outer kettle cover 11 are arranged on the outer kettle cover. The external tank pressure measurement assembly 18 includes an external tank pressure gauge and a pressure transmitter.
Similarly, the inner kettle cover 21 is provided with an inner kettle air inlet pipe 25 and an inner kettle air outlet pipe 219, the lower end part of the inner kettle air inlet pipe 25 is close to the bottom of the inner kettle body 23, and the inner kettle air outlet pipe 219 is positioned inside the cavity of the inner kettle body 23 and is flush with the bottom of the inner kettle cover 21. An inner tank first flow regulating valve 26, an inner tank first electromagnetic valve 27, an inner tank pressure measuring assembly 28, an inner tank safety valve 29 and an inner tank rupture disk 210 are arranged on the outer end part of the inner tank air inlet pipe 25. An inner kettle second flow regulating valve 212, an inner kettle stop valve 213 and an inner kettle second electromagnetic valve 214 are arranged on the outer end part of the inner kettle exhaust pipe. 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 thermocouple 211 extending into the inner kettle body 23 and an inner kettle thermowell 216 sleeved on the inner surface of the inner kettle cover 21 are arranged on the inner kettle cover 21. The inner tank pressure measurement assembly 28 includes an inner tank pressure gauge and a pressure transmitter.
The inner kettle temperature thermocouple 211 comprises a thermocouple and a thermocouple pressure balance tube 2111 arranged on the outer kettle cover 11. The inner tank thermowell 216 on the inner tank cover 21 may communicate with the outer tank vent pipe 119 or the inner tank vent pipe 219, preferably with the inner tank vent pipe 219, so that the inner pressure and the outer pressure of the thermowell are balanced, preventing the thermowell from being broken.
In order to realize the tightness 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 a certain pretightening force is applied, and then the sealing is realized by fixing the outer kettle body 13 and the outer kettle cover 11 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 inner kettle sealing gasket is fixed by a clamp 24 to realize sealing.
As shown in fig. 2-3, the suspension assembly includes a support platform 221, and a strut 224 suspending the support platform 221 at the bottom of the outer kettle cover 11, where 3 or 4 screws are fixed on the support platform, and the annular array is at the outer edge of the support platform 221, the strut 224 includes 3 or 4 sleeves corresponding to the screws, respectively corresponding to the screws, two ends of the corresponding sleeve are respectively connected with the outer kettle cover 11 and the screws on the support platform 221 in a threaded manner, and a second fastening bolt 225 capable of propping against the screws is further provided in the vertical direction of the sleeve, and the length of the strut 224 is determined by locking the second fastening bolt 225. The middle part of the platform is provided with a spring 223, and a bearing part 222 at the bottom of the inner kettle body 23 is supported above the spring 223. The supporting portion 222 is hemispherical or flat. The spring 223 mainly prevents the expansion coefficients of the inner container and the strut 224 from being different at high temperature, and realizes the compensation of pretightening force, thereby ensuring the sealing of the inner kettle.
Example 2
The method of using the high temperature autoclave and the method of using the same in a highly corrosive environment as described in example 1 was used to develop a uniform corrosion resistance measurement of super austenitic stainless steel in 30% sulfuric acid solution at 300 ℃ under 9MPa pressure as required. The method comprises the following steps:
s1, cleaning and drying a test sample, measuring several sizes and masses of the sample, preparing sulfuric acid solution with a mass fraction of 30%, calculating the required solution amount according to the surface area of the sample, placing an object to be tested on a sample hanger in an 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 a suspension assembly;
s2, butting the two parts of 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 rod in the suspension assembly in the sleeve and locking by using a second fastening bolt 225, wherein the length ensures that a gap exists between the bottom of the suspension assembly and the inner wall of the outer kettle body 13;
s3, an inner kettle is directly placed into the outer kettle body 13 by the outer kettle cover 11 which is integrated with the inner kettle cover 21, heat conduction liquid is input between the outer kettle body 13 and the inner kettle body 23 to a certain depth and is prevented from passing through an air inlet pipe outlet in the outer kettle body 13, and the outer kettle cover 11 and the outer kettle body 13 are covered and locked and sealed;
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 air inlet pipe of the outer kettle body 13 to perform an air tightness test, enabling the outer kettle and the inner kettle to form a pressure difference of P ', setting the pressure difference P' between the inner kettle and the outer 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 increases, re-sealing is needed, returning to the step S2, and if not, entering the step S5;
s5, opening an air inlet pipe of the inner kettle, starting an interlocking program, and enabling the pressure P in the outer kettle to be equal to the pressure P in the outer kettle Outer part With the pressure P in the inner kettle Inner part Is arranged to interlock to ensure P Inner part ≤P Outer part ≤P Inner part +P', and simultaneously introducing pressurized gas into the outer kettle and the inner kettle; 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 as P Outer part =P Inner part +P', since the saturated vapor pressure of water at 300℃is about 9MPa, the pressure in the airtight test is 10 to 11MPa. After the pressure maintaining is carried out for a set time, the pressure P in the outer kettle is observed Outer part If the pressure P in the outer kettle is changed Outer part Wave motion occurs, which indicates that the outer kettle has leakage and returnsStep S3, otherwise, entering a step S6;
s6, cooling water is communicated for the condensers coated on the outer kettle exhaust pipe 119, the inner kettle air inlet pipe 25 and the inner kettle exhaust pipe 219, and according to test requirements, gas replacement and saturation are carried out on test mediums in the inner container;
s7, heating; opening the first flow regulating valve 16, the first flow regulating valve 26, the second flow regulating valve 112 and the second flow regulating valve 212, setting the pressure difference P' =0.3 MPa, the test temperature T=300 ℃, the test pressure P=9 MPa, the test period t=168 h and the overtemperature alarm value T Super-energy storage device =310 ℃, overpressure alarm value P Super-energy storage device The method comprises the steps of (1) starting up internal interlocking of external pressure P and internal pressure P of an external kettle of a high-temperature high-pressure kettle with test parameters of 10MPa and the like, starting up a heating and boosting program, automatically heating up to a set test temperature by a control program according to the setting, entering a step S8 when the pressure generated by the temperature rise does not meet the test requirement, starting test timing if the test requirement can be met, and entering the step S9 after the set test time;
s8, pressurizing the inner kettle and the outer kettle synchronously to enable the pressure in the inner kettle to finally meet the test requirement, starting test timing, and after the set time, entering a step S9; the internal kettle can theoretically raise the temperature first and then raise the pressure and then raise the temperature, and it is preferable that the temperature is raised first and then raise the pressure, and the external kettle synchronously raises the pressure along with the pressure of the internal kettle.
S9, after the test is finished, the heating furnace stops heating, the device automatically cools, and simultaneously, 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 the inner kettle and the outer kettle synchronously decompress, and P is ensured Inner part ≤P Outer part ≤P Inner 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 procedure, starting an outer kettle stop valve 113, and exhausting 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 control the pressure P of the inner kettle Inner part Control the opening and closing of the second electromagnetic valve 114 to regulate the pressure P in the outer kettle Outer part Let P Outer part =P Inner part When the temperature of the inner kettle is reduced to 30 ℃, the inner kettle stop valve 213 on the inner kettle exhaust pipe is opened to discharge the gas in the inner kettle, and the gas in the outer kettle is synchronously discharged through the outer kettle exhaust pipe 119 according to the interlocking relationship. And after the gas in the inner kettle is exhausted, closing the interlocking procedure. 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.
S10, uncovering, taking a sample, opening the outer kettle cover 11, removing a fixing piece on the inner kettle, taking down the inner kettle body, and then 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, airing and taking care.
The above embodiments are merely preferred embodiments of the present application and are not intended to limit the present application, and any modifications, equivalent substitutions and improvements made within the spirit and principles of the present application should be included in the scope of the present application.

Claims (6)

1. The high-temperature high-pressure kettle used in a strong corrosion environment is characterized by comprising an outer kettle assembly and an inner kettle assembly, wherein the outer kettle assembly comprises an outer kettle body (13) and an outer kettle cover (11), the inner kettle assembly comprises an inner kettle body (23) sleeved in the outer kettle body (13) and used for placing objects to be tested, and an inner kettle cover (21) covered on the inner kettle body (23) and 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 filled with heat conducting liquid is reserved between the outer kettle body (13) and the inner kettle body (23);
the suspension assembly comprises a support platform (221) and a support column (224) for suspending the support platform (221) at the bottom of the outer kettle cover (11), a spring (223) is arranged on the platform, and a bearing part (222) for supporting the bottom of the inner kettle body (23) is arranged above the spring (223);
the support platform (221) is fixedly provided with a plurality of screws, the support column (224) comprises a plurality of sleeves, two ends of each corresponding sleeve are respectively in threaded connection with the outer kettle cover (11) and the screws on the support platform (221), and a second fastening bolt (225) capable of propping against the screws is further arranged in the vertical direction of each sleeve;
the use method of the high-temperature high-pressure kettle used in the strong corrosion environment comprises the following steps:
s1, placing an object to be tested on a sample hanger (220) in an inner kettle body (23), then injecting a test solution into the inner kettle body (23), and placing the inner kettle body (23) on a bearing part (222) of a suspension assembly;
s2, butting two parts of 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 rod in the suspension assembly in the sleeve and locking by a second fastening bolt (225), wherein the length ensures that a gap exists between the bottom of the suspension assembly and the inner wall of the outer kettle body (13);
s3, an outer kettle cover (11) which is integrated with the inner kettle cover (21) directly places the inner kettle into the outer kettle body (13), heat conduction liquid is input between the outer kettle body (13) and the inner kettle body (23) to a certain depth and is prevented from passing through an air inlet pipe outlet in the outer kettle body (13), and the outer kettle cover (11) and the outer kettle body (13) are covered and locked and sealed;
s4, sealing an inner kettle air inlet pipe (25), an inner kettle air outlet pipe (219) and an outer kettle air outlet pipe (119), and introducing inert gas into the outer kettle body (13) through the air inlet pipe of the outer kettle body (13) to carry out an air tightness test, so that the outer kettle and the inner kettle form a pressure difference of P ', and the P' is less than P 0 ,P 0 For the maximum external pressure which can be borne by the safe operation of the inner kettle, maintaining the pressure for a set time, checking the change of the value of the pressure transmitter on the air inlet pipe (25) of the inner kettle to judge the tightness of the kettle, and if the value of the pressure transmitter on the air inlet pipe (25) of the inner kettle is increased, the inner kettle needs to be resealed and returns to the step S2; if not, entering step S5;
s5, opening an air inlet pipe (25) of the inner kettle, starting an interlocking program, and controlling the pressure P in the outer kettle Outer part With the pressure P in the inner kettle Inner part Is arranged to interlock to ensure P Inner part ≤P Outer part ≤P Inner part +P', and simultaneously introducing pressurized gas into the outer kettle and the inner kettle; 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 as P Outer part =P Inner part +P', continuously boosting to the airtight test pressure, maintaining the pressure for a period of time, and observing the pressure P in the outer kettle Outer part If the pressure in the outer kettle is not reduced, the air tightness test of the outer kettle passes, the pressure relief operation is carried out according to the requirement, then the step S6 is carried out, and if the air tightness test of the outer kettle does not pass, the step S3 is returned;
s6, cooling water is communicated with a condenser coated on the exhaust pipes of the inner kettle and the outer kettle;
s7, heating; starting a heating furnace (117) to heat the outer kettle, automatically transferring heat to the inner kettle by heat conducting liquid, detecting test temperature through a thermocouple in the inner kettle, heating until the set temperature is reached, ensuring fluctuation in the set range, simultaneously introducing pressurized gas into the outer kettle due to the change of internal and external pressure difference caused by temperature rise, and keeping the relation between the pressure in the outer kettle and the pressure in the inner kettle as P Inner part ≤P Outer part ≤P Inner part When the pressure generated by the temperature rise does not meet the test requirement, the step S8 is carried out, if the pressure can meet the test requirement, the test timing is started, and after the set test time, the step S9 is carried out;
s8, pressurizing the inner kettle and the outer kettle synchronously to enable the pressure in the inner kettle to finally meet the test requirement, starting test timing, and entering a step S9 after the set test time;
s9, after the test is finished, the heating furnace (117) stops heating, the device automatically cools, and when the temperature is lowered, the electromagnetic valve on the exhaust pipe (119) of the outer kettle is timely opened according to the pressure in the inner kettle, so that the synchronous depressurization of the inner kettle and the outer kettle is realized, and P is ensured Inner part ≤P Outer part ≤P Inner part +P', after the high-temperature high-pressure kettle is completely cooled, starting an inner kettle stop valve (213) on an inner kettle exhaust pipe (219), after the gas in the inner kettle is exhausted, closing an interlocking program, and starting an outer kettle stop valve (113) on an outer kettle exhaust pipe (119), and exhausting pressurized gas in the kettle;
s10, uncovering, taking a sample, opening an outer kettle cover (11), removing a fixing piece on the inner kettle, taking down an inner kettle body (23), and then taking out the sample;
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.
2. 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 adjusting component and a measuring meter group, and the end parts of the air inlet pipe, the air outlet pipe and the temperature measuring component on the inner kettle cover (21) outside the kettle are penetrated through the outer kettle cover (11).
3. The autoclave of claim 2, wherein the safety regulating assembly comprises an intake air flow regulating valve, an intake air electromagnetic valve, a safety valve and a rupture disk which are arranged on an intake pipe, and the measuring meter group on an exhaust pipe comprises an exhaust air flow regulating valve, an exhaust electromagnetic valve and an exhaust stop valve which is arranged on a branch pipe of the exhaust pipe; the measuring meter group comprises a pressure meter and a pressure transmitter which are arranged on the air inlet pipe.
4. A high temperature autoclave for use in a highly corrosive environment according to claim 3, wherein the condenser is provided on the inner autoclave exhaust pipe (219) and on the inner autoclave intake pipe (25), and the temperature measuring assembly comprises a thermocouple extending into the inner autoclave and a thermowell sleeved on the outer wall of the thermocouple.
5. The autoclave of claim 4, wherein the thermowell is in communication with either an inner autoclave exhaust pipe (219) or an outer autoclave exhaust pipe (119).
6. The high-temperature high-pressure kettle used in the strong corrosion environment according to claim 1, wherein the outer kettle body (13) and the outer kettle cover (11) are made of one of carbon steel, alloy steel and stainless steel; when the use temperature is within 200 ℃, the inner kettle body (23) and the inner kettle cover (21) are prepared by polytetrafluoroethylene, when the use temperature is above 200 ℃, the inner kettle body (23) and the inner kettle cover (21) are prepared by 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 prepared by Monel alloy.
CN202110555230.4A 2021-05-21 2021-05-21 High-temperature high-pressure kettle used in strong corrosion environment and use method Active CN113522167B (en)

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CH363970A (en) * 1958-01-27 1962-08-31 Ciba Geigy Process for carrying out processes under high pressure and with a large temporal and / or local temperature gradient and an autoclave for carrying out the process
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JP2014161790A (en) * 2013-02-25 2014-09-08 Ricoh Co Ltd Effluent treatment apparatus
CN205361266U (en) * 2016-02-27 2016-07-06 杭州若水化学科技有限公司 Can remove pressure reaction unit of water that produces among reaction sequence
CN208032519U (en) * 2018-02-08 2018-11-02 北京柏墨达科技有限公司 A kind of autoclave
CN210675104U (en) * 2019-09-05 2020-06-05 广州市钢立科学仪器有限公司 Hydrothermal reaction kettle structure with internal support
CN112221433A (en) * 2020-08-18 2021-01-15 华电电力科学研究院有限公司 Double-kettle test device and method suitable for high-temperature and high-pressure water environment or steam environment
CN213032443U (en) * 2018-10-08 2021-04-23 山东第一医科大学(山东省医学科学院) Miniature high-pressure reaction kettle for laboratory

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH363970A (en) * 1958-01-27 1962-08-31 Ciba Geigy Process for carrying out processes under high pressure and with a large temporal and / or local temperature gradient and an autoclave for carrying out the process
CN201195058Y (en) * 2008-05-22 2009-02-18 中国石油天然气股份有限公司 Nano-stuffing production apparatus
JP2014161790A (en) * 2013-02-25 2014-09-08 Ricoh Co Ltd Effluent treatment apparatus
CN205361266U (en) * 2016-02-27 2016-07-06 杭州若水化学科技有限公司 Can remove pressure reaction unit of water that produces among reaction sequence
CN208032519U (en) * 2018-02-08 2018-11-02 北京柏墨达科技有限公司 A kind of autoclave
CN213032443U (en) * 2018-10-08 2021-04-23 山东第一医科大学(山东省医学科学院) Miniature high-pressure reaction kettle for laboratory
CN210675104U (en) * 2019-09-05 2020-06-05 广州市钢立科学仪器有限公司 Hydrothermal reaction kettle structure with internal support
CN112221433A (en) * 2020-08-18 2021-01-15 华电电力科学研究院有限公司 Double-kettle test device and method suitable for high-temperature and high-pressure water environment or steam environment

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