CN109701296A - Corrosion-resistant more working method supercritical carbon dioxide extracting systems - Google Patents
Corrosion-resistant more working method supercritical carbon dioxide extracting systems Download PDFInfo
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- CN109701296A CN109701296A CN201910000240.4A CN201910000240A CN109701296A CN 109701296 A CN109701296 A CN 109701296A CN 201910000240 A CN201910000240 A CN 201910000240A CN 109701296 A CN109701296 A CN 109701296A
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Abstract
The invention discloses a kind of corrosion-resistant more working method supercritical carbon dioxide extracting systems, including mounting rack, high pressure constant-flux pump, control cabinet, carbon dioxide pump, preheating mixer, the first constant temperature extracting kettle, the second constant temperature extracting kettle, gas-liquid separator, thermostatic water bath, high-pressure carbon dioxide steel cylinder, holding tank and low pressure recycle to pump.Corrosion-resistant more working method supercritical carbon dioxide extracting systems, when carrying out contaminated soil elution decontamination, it is used cooperatively by the first valve, the second valve, third valve, the 4th valve with the 5th valve, choosing multiple working method, most suitable working method is selected according to different needs, flexible working mode is optional, effectively save search time, more scientific datas are obtained simultaneously, first constant temperature extracting kettle and the second constant temperature extracting kettle are all made of using Hastelloy inner liner polytetrafluoroethylene layer, being capable of resistance to strong acid corrosion for a long time at high temperature under high pressure.
Description
Technical field
The present invention relates to nuclear environment scientific domain, specifically corrosion-resistant more working method supercritical carbon dioxide extractings system
System.
Background technique
Solid radiation pollutant Study on decontamination is constantly subjected to the attention of people, as a kind of efficient isolation technics side
Method, supercritical extraction technique (SFE), especially supercritical CO 2 have lower critical condition (31.3 DEG C, 7.4MPa) extensively
It is general to separate with the decontamination of heavy metal for organic pollutant in solid phase environment medium.In recent years, the U.S., Japan, Russia, English
State and South Korea have all carried out research of the SFE for nuclear waste decontamination and spentnuclear fuel post-processing, it was demonstrated that SFE, which has, is applied to nuclear waste
The potentiality of decontamination have its unique advantage.However, commercial supercritical extraction unit is applied to the fields such as organic, biological medicine more
Research, applied to the elution decontamination of radioactive solid waste, there is also extracting system structure is simple, the material of extraction kettle is long-term
Corrosion resistance (especially strong acid corrosion) and to the particular problems such as the anti-adsorption of nucleic is not high enough under high temperature and pressure, it is difficult to full
Sufficient scientific research demand.
Summary of the invention
The purpose of the present invention is to provide a kind of corrosion-resistant more working method supercritical carbon dioxide extracting systems, to solve
The problems mentioned above in the background art.
To achieve the above object, the invention provides the following technical scheme:
A kind of corrosion-resistant more working method supercritical carbon dioxide extracting systems, including mounting rack, high pressure constant-flux pump, control cabinet,
Carbon dioxide pump, preheating mixer, the first constant temperature extracting kettle, the second constant temperature extracting kettle, gas-liquid separator, thermostatic water bath, high pressure
Carbon dioxide steel cylinder, holding tank and low pressure recycle pump, and the top part of the first constant temperature extracting kettle is installed with temperature-measuring port and surveys
Mouth is pressed, is fixedly installed with first pipe between the gas outlet of the high-pressure carbon dioxide steel cylinder and the input port of carbon dioxide pump,
It is fixedly installed with strainer valve at the top of the first pipe, the top of the first pipe and two sides for being located at strainer valve are solid respectively
Dingan County is equipped with pressure reducing valve and valve, is fixedly installed between the delivery outlet of the carbon dioxide pump and the input port of preheating mixer
Second pipe, the top of the second pipe are fixedly installed with valve and check valve, the input port of the high pressure constant-flux pump respectively
Third pipeline is fixedly installed between holding tank, the top of the third pipeline is fixedly installed with strainer valve and valve respectively,
The 4th pipeline, the top part of the 4th pipeline are fixedly installed between the delivery outlet and preheating mixer of the high pressure constant-flux pump
It is not fixedly installed with valve and check valve, the side of the preheating mixer is fixedly installed with the 5th pipeline, the 5th pipeline
Top be fixedly installed with the first inlet branch and the second inlet branch respectively, and the first inlet branch and the second inlet branch
Top is fixedly connected with the bottom of the first constant temperature extracting kettle and the second constant temperature extracting kettle respectively, the side of first inlet branch
It is fixedly installed with the first valve, the top of the 5th pipeline and the fixation between the first inlet branch and the second inlet branch
Second valve is installed, the input port of the gas-liquid separator is fixedly installed with the 6th pipeline, the first constant temperature extracting kettle
Discharge port is fixedly installed with the first output branch pipe, and one end of the first output branch pipe is fixedly connected with the 6th pipeline, and described second
The discharge port of constant temperature extracting kettle is fixedly installed with the second output branch pipe, and one end of the second output branch pipe and the fixed company of the 6th pipeline
It connects, communicating pipe is fixedly installed between the 5th pipeline and the 6th pipeline, the side of the communicating pipe is fixedly installed with third
Valve, the side of the 6th pipeline are fixedly installed with the 4th valve, the 5th valve and counterbalance valve, the low pressure recycle pump respectively
Delivery outlet and input port be fixedly installed with circulation pipe, two circulation pipe is fixedly connected with gas-liquid separator, and two are followed
The top of endless tube is fixedly installed with valve.
As a further solution of the present invention: gas sample mouth is fixedly installed at the top of the gas-liquid separator, it is described
The bottom of gas-liquid separator is fixedly installed with liquid sampling mouth, the fixed peace in the side of the gas sample mouth and liquid sampling mouth
Equipped with valve.
As the present invention further scheme: first valve, the second valve, third valve, the 4th valve and the
Five valves realize several working ways, the first valve, the 4th valve and the 5th valve opening, the second valve by different closed manners
Door is closed with third valve, and the first constant temperature extracting kettle, the second valve and the 5th valve opening, the first valve, third is used alone
Valve and the 4th valve are closed, and the second constant temperature extracting kettle are used alone, the first valve, the second valve, the 4th valve and valve are opened
It opens, third valve is closed, synchronous to use the first constant temperature extracting kettle and the second constant temperature extracting kettle, the first valve, third valve and the
Five valve openings, the second valve and the 4th valve are closed, and the first constant temperature extracting kettle and the second constant temperature extracting kettle are used in series.
As further scheme of the invention: the holding tank can store modifying agent, such as methanol, concentrated nitric acid, ionic liquid
Body, the holding tank can also store the different types of extractant of various concentration, such as TBP, TOA, CMPO, TTA.
As further scheme of the invention: the discharge port of the first constant temperature extracting kettle and the second constant temperature extracting kettle is equal
It is provided with filter core, and the pore diameter range of filter core is 1nm to 1 μm.
As the present invention further scheme: the first constant temperature extracting kettle is jacketed constant-temp extraction kettle, described the
One constant temperature extracting kettle is connected using gland-type spiral, and it uses air outlet structure in lower charging, and the first constant temperature extracting kettle is adopted
Structure size with Hastelloy inner liner polytetrafluoroethylene layer, the first constant temperature extracting kettle and the second constant temperature extracting kettle is uniform
It causes.
Compared with prior art, the beneficial effects of the present invention are:
This it is practical carry out contaminated soil elution decontamination when, by the first valve, the second valve, third valve, the 4th valve with
5th valve is used cooperatively, choosing multiple working method, selects most suitable working method according to different needs, work
Mode flexible and selectable, effectively save search time, while more scientific datas are obtained, the first constant temperature extracting kettle and the second constant temperature extract
It takes kettle to be all made of using Hastelloy inner liner polytetrafluoroethylene layer, the resistance to strong acid of long-time can corrode at high temperature under high pressure, simultaneously
The useful good anti-adsorption of polytetrafluoroethylene (PTFE) material effectively avoids the nucleic eluted from adsorbing in wall surface and is enriched with, can
Allow the more extreme extraction conditions such as high temperature, high pressure, strong acid, it can absorption damage of the effectively easy absorbing elements on extraction kettle wall
It loses, more accurate data is provided, by the filter core and strainer valve of setting, it is solid to can effectively avoid the ultra-fine pollution of fluid carry-over
Body particle causes secondary pollution, and this system automatically controls, and the unattended overcritical elution of radioactive waste solid may be implemented
Decontamination.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of corrosion-resistant more working method supercritical carbon dioxide extracting systems.
Fig. 2 is the workflow schematic diagram of corrosion-resistant more working method supercritical carbon dioxide extracting systems.
In figure: mounting rack 1, high pressure constant-flux pump 2, control cabinet 3, carbon dioxide pump 4, pressure reducing valve 5, preheating mixer 6, first
Constant temperature extracting kettle 7, the second constant temperature extracting kettle 8, counterbalance valve 9, gas-liquid separator 10, thermostatic water bath 11.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Please refer to Fig. 1~2, in the embodiment of the present invention, a kind of corrosion-resistant more working method supercritical carbon dioxide extractings system
System, including mounting rack 1, high pressure constant-flux pump 2, control cabinet 3, carbon dioxide pump 4, preheating mixer 6, the first constant temperature extracting kettle 7, the
Two constant temperature extracting kettles 8, gas-liquid separator 10, thermostatic water bath 11, high-pressure carbon dioxide steel cylinder, holding tank and low pressure recycle pump, high
There is carbon dioxide inside pressure carbon dioxide steel cylinder, and its purity is 99.9%, the top part of the first constant temperature extracting kettle 7 is installed with
Temperature-measuring port and pressure tap, temperature-measuring port and pressure tap can be convenient for the temperature and pressure in monitoring extraction kettle, high-pressure carbon dioxide steel cylinders
Gas outlet and carbon dioxide pump 4 input port between be fixedly installed with first pipe, be fixedly installed at the top of first pipe
Strainer valve, the top of first pipe and the two sides for being located at strainer valve are fixedly installed with pressure reducing valve 5 and valve, carbon dioxide pump respectively
Second pipe is fixedly installed between 4 delivery outlet and the input port of preheating mixer 6, the top of second pipe is fixed respectively to pacify
Equipped with valve and check valve, third pipeline is fixedly installed between the input port and holding tank of high pressure constant-flux pump 2, third pipeline
Top is fixedly installed with strainer valve and valve respectively, is fixedly installed between the delivery outlet and preheating mixer 6 of high pressure constant-flux pump 2
4th pipeline, the top of the 4th pipeline are fixedly installed with valve and check valve respectively, and the side of preheating mixer 6 is fixedly installed with
5th pipeline, the top of the 5th pipeline are fixedly installed with the first inlet branch and the second inlet branch, and the first input branch respectively
The top of pipe and the second inlet branch is fixedly connected with the bottom of the first constant temperature extracting kettle 7 and the second constant temperature extracting kettle 8 respectively, the
The side of one inlet branch is fixedly installed with the first valve, the top of the 5th pipeline and is located at the first inlet branch and inputs with second
The second valve is fixedly installed between branch pipe, the input port of gas-liquid separator 10 is fixedly installed with the 6th pipeline, gas-liquid separator
10 can will be divided into after the supercritical fluid discharge of the radioactive pollution nucleic such as the carrying plutonium flowed out in extraction kettle and its compound
Liquids and gases, air-liquid sample are collected in gas sample mouth and liquid sampling mouth respectively, for analyzing emission pollution and grinding
Study carefully extraction efficiency, the discharge port of the first constant temperature extracting kettle 7 is fixedly installed with the first output branch pipe, and one end of the first output branch pipe
It is fixedly connected with the 6th pipeline, the discharge port of the second constant temperature extracting kettle 8 is fixedly installed with the second output branch pipe, and the second output branch
One end of pipe is fixedly connected with the 6th pipeline, is fixedly installed with communicating pipe between the 5th pipeline and the 6th pipeline, and the one of communicating pipe
Side is fixedly installed with third valve, and the side of the 6th pipeline is fixedly installed with the 4th valve, the 5th valve and counterbalance valve 9 respectively,
The delivery outlet of low pressure recycle pump and input port are fixedly installed with circulation pipe, two circulation pipe is fixed with gas-liquid separator 10
Connection, the top of two circulation pipes are fixedly installed with valve, and the top of gas-liquid separator 10 is fixedly installed with gas sample mouth,
The bottom of gas-liquid separator 10 is fixedly installed with liquid sampling mouth, and gas sample mouth and the side of liquid sampling mouth are fixedly mounted
There is valve, the first valve, the second valve, third valve, the 4th valve are realized from the 5th valve by different closed manners a variety of
Working method, the first valve, the 4th valve and the 5th valve opening, the second valve and third valve are closed, and are used alone first
Constant temperature extracting kettle 7, the second valve and the 5th valve opening, the first valve, third valve and the 4th valve are closed, and are used alone the
Two constant temperature extracting kettles 8, the first valve, the second valve, the 4th valve and the 5th valve opening, third valve are closed, synchronous to use
First constant temperature extracting kettle 7 and the second constant temperature extracting kettle 8, the first valve, third valve and the 5th valve opening, the second valve and
Four valves are closed, and are used in series the first constant temperature extracting kettle 7 and the second constant temperature extracting kettle 8, holding tank can store modifying agent, such as first
Alcohol, concentrated nitric acid, ionic liquid, holding tank can also store the different types of extractant of various concentration, such as TBP, TOA, CMPO, TTA,
The discharge port of first constant temperature extracting kettle 7 and the second constant temperature extracting kettle 8 is provided with filter core, and the pore diameter range of filter core is 1nm to 1
μm, the first constant temperature extracting kettle 7 is jacketed constant-temp extraction kettle, and the first constant temperature extracting kettle 7 is connected using gland-type spiral, and it is adopted
With air outlet structure in lower charging, the first constant temperature extracting kettle 7 uses Hastelloy inner liner polytetrafluoroethylene layer, the first constant temperature extracting kettle
7 is consistent with the structure size of the second constant temperature extracting kettle 8.
The working principle of the invention is:
In use, extractant uses TBP-HNO3 by taking supercritical carbon dioxide extraction 1Kg contaminated soil containing plutonium as an example, it will
1Kg contaminated soil containing plutonium is placed in the first constant temperature extracting kettle 7, and the temperature and pressure of the first constant temperature extracting kettle 7 of setting is respectively
65 DEG C and 35Mpa, the second valve, third valve, the 4th valve and the 5th valve are closed, using the first constant temperature extracting is used alone
The working method of kettle 7, the carbinol-modified extractant of 200mL is pre-placed in holding vessel, and (TBP content is 2.7mol%, every 100mL first
The high-purity dense HNO3 of 2mL is added in alcohol), set the flow velocity of carbon dioxide pump 4 as constant speed 25mL/min, the flow velocity of high pressure constant-flux pump 2
For 0.5mL/min, the temperature of preheating mixer 6 is set as 65 DEG C, by first after carbon oxide fluid and modifier solution mixing
Valve introduces the first constant temperature extracting kettle 7, and temperature and pressure reaches setting value in about 1 hour the first constant temperature extracting kettle 7, closes dioxy
Change carbon pump 4, high pressure constant-flux pump 2, check valve and the first valve, extraction time and be set as 2 hours, the radioactivity such as plutonium are carried after extraction
The supercritical fluid of nucleic and its compound is polluted from two after 7 top of the first constant temperature extracting kettle inflow gas-liquid separator 10, discharge
Carbon oxide gas is discharged from gas sample mouth and collects, and the complex compound and unreacting reagent of the radionuclides such as plutonium reside in gas-liquid point
It is to be studied in sample container from device, excluding and collecting through liquid sampling mouth, pass through the first valve, the second valve, third valve
Door, the 4th valve are used cooperatively with the 5th valve, and choosing multiple working method selects most suitable according to different needs
Working method, flexible working mode is optional, effectively save search time, while obtaining more scientific datas, the first constant temperature extracting
Kettle 7 and the second constant temperature extracting kettle 8 are all made of using Hastelloy inner liner polytetrafluoroethylene layer, can at high temperature under high pressure for a long time
Resistance to strong acid corrosion, while the useful good anti-adsorption of polytetrafluoroethylene (PTFE) material, effectively avoid the nucleic eluted in wall
Adsorption enrichment, allows the more extreme extraction conditions such as high temperature, high pressure, strong acid, can effectively easy absorbing elements extracting
Adsorption loss on kettle wall provides more accurate data, can be solid according to pollution by the filter core and strainer valve of setting
Body sample takes the circumstances into consideration to select filter core aperture specification, can effectively avoid the ultra-fine pollution solid particle of fluid carry-over, causes secondary pollution, and
This system automatically controls, and the unattended overcritical elution decontamination of radioactive waste solid may be implemented.
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art,
It is still possible to modify the technical solutions described in the foregoing embodiments, or part of technical characteristic is carried out etc.
With replacement, all within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in this
Within the protection scope of invention.
Claims (6)
1. a kind of corrosion-resistant more working method supercritical carbon dioxide extracting systems, it is characterised in that: including mounting rack (1), height
Press constant-flux pump (2), control cabinet (3), carbon dioxide pump (4), preheating mixer (6), the first constant temperature extracting kettle (7), the second constant temperature
Extraction kettle (8), gas-liquid separator (10), thermostatic water bath (11), high-pressure carbon dioxide steel cylinder, holding tank and low pressure recycle pump, institute
The top part for stating the first constant temperature extracting kettle (7) is installed with temperature-measuring port and pressure tap, the outlet of the high-pressure carbon dioxide steel cylinder
It is fixedly installed with first pipe between mouth and the input port of carbon dioxide pump (4), is fixedly installed at the top of the first pipe
Strainer valve, the top of the first pipe and the two sides for being located at strainer valve are fixedly installed with pressure reducing valve (5) and valve respectively, described
Second pipe, second pipe are fixedly installed between the delivery outlet of carbon dioxide pump (4) and the input port of preheating mixer (6)
The top in road is fixedly installed with valve and check valve respectively, fixed between the input port and holding tank of the high pressure constant-flux pump (2)
Third pipeline is installed, the top of the third pipeline is fixedly installed with strainer valve and valve, the high pressure constant-flux pump (2) respectively
Delivery outlet and preheating mixer (6) between be fixedly installed with the 4th pipeline, the top of the 4th pipeline is fixedly mounted respectively
There are valve and check valve, the side of the preheating mixer (6) is fixedly installed with the 5th pipeline, the top part of the 5th pipeline
It is not fixedly installed with the first inlet branch and the second inlet branch, and the top of the first inlet branch and the second inlet branch is distinguished
It is fixedly connected with the bottom of the first constant temperature extracting kettle (7) and the second constant temperature extracting kettle (8), the side of first inlet branch is solid
Dingan County is equipped with the first valve, the top of the 5th pipeline and the fixed peace between the first inlet branch and the second inlet branch
Equipped with the second valve, the input port of the gas-liquid separator (10) is fixedly installed with the 6th pipeline, the first constant temperature extracting kettle
(7) discharge port is fixedly installed with the first output branch pipe, and one end of the first output branch pipe is fixedly connected with the 6th pipeline, described
The discharge port of second constant temperature extracting kettle (8) is fixedly installed with the second output branch pipe, and one end of the second output branch pipe and the 6th pipe
Road is fixedly connected, and communicating pipe, the fixed peace in the side of the communicating pipe are fixedly installed between the 5th pipeline and the 6th pipeline
Equipped with third valve, the side of the 6th pipeline is fixedly installed with the 4th valve, the 5th valve and counterbalance valve (9), institute respectively
State low pressure recycle pump delivery outlet and input port be fixedly installed with circulation pipe, two circulation pipe with gas-liquid separator (10)
It is fixedly connected, the top of two circulation pipes is fixedly installed with valve.
2. corrosion-resistant more working method supercritical carbon dioxide extracting systems according to claim 1, it is characterised in that: institute
It states and is fixedly installed with gas sample mouth at the top of gas-liquid separator (10), the bottom of the gas-liquid separator (10) is fixedly installed with
The side of liquid sampling mouth, the gas sample mouth and liquid sampling mouth is fixedly installed with valve.
3. corrosion-resistant more working method supercritical carbon dioxide extracting systems according to claim 1, it is characterised in that: institute
It states the first valve, the second valve, third valve, the 4th valve and realizes a variety of work sides by different closed manners from the 5th valve
Formula, the first valve, the 4th valve and the 5th valve opening, the second valve and third valve are closed, and the first constant temperature extraction is used alone
Kettle (7), the second valve and the 5th valve opening are taken, the first valve, third valve and the 4th valve are closed, and it is permanent to be used alone second
Warm extraction kettle (8), the first valve, the second valve, the 4th valve and the 5th valve opening, third valve are closed, synchronous to use the
One constant temperature extracting kettle (7) and the second constant temperature extracting kettle (8), the first valve, third valve and the 5th valve opening, the second valve and
4th valve is closed, and the first constant temperature extracting kettle (7) and the second constant temperature extracting kettle (8) are used in series.
4. corrosion-resistant more working method supercritical carbon dioxide extracting systems according to claim 1, it is characterised in that: institute
Modifying agent can be stored by stating holding tank, and the holding tank can also store the different types of extractant of various concentration.
5. corrosion-resistant more working method supercritical carbon dioxide extracting systems according to claim 1, it is characterised in that: institute
The discharge port for stating the first constant temperature extracting kettle (7) and the second constant temperature extracting kettle (8) is provided with filter core, and the pore diameter range of filter core is
1nm to 1 μm.
6. corrosion-resistant more working method supercritical carbon dioxide extracting systems according to claim 1, it is characterised in that: institute
Stating the first constant temperature extracting kettle (7) is jacketed constant-temp extraction kettle, and the first constant temperature extracting kettle (7) is connected using gland-type spiral
It connects, and it uses air outlet structure in lower charging, the first constant temperature extracting kettle (7) uses Hastelloy inner liner polytetrafluoroethylene
Layer, the first constant temperature extracting kettle (7) are consistent with the structure size of the second constant temperature extracting kettle (8).
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CN112974412A (en) * | 2021-02-23 | 2021-06-18 | 中国核动力研究设计院 | Chemical decontamination method and device for radioactive pollution by supercritical carbon dioxide |
CN113521796A (en) * | 2021-06-10 | 2021-10-22 | 江苏高科制药设备有限公司 | Air-lift adsorption type supercritical extraction pharmaceutical system |
CN114295791A (en) * | 2022-03-09 | 2022-04-08 | 新疆广陆能源科技股份有限公司 | Tail gas detection system of thermal fluid generator and multi-medium thermal fluid generation system |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN110899248A (en) * | 2019-06-21 | 2020-03-24 | 杭州杭氧股份有限公司 | System and method for cleaning ultrahigh-purity gas steel cylinders in batch by using supercritical fluid |
CN112974412A (en) * | 2021-02-23 | 2021-06-18 | 中国核动力研究设计院 | Chemical decontamination method and device for radioactive pollution by supercritical carbon dioxide |
CN113521796A (en) * | 2021-06-10 | 2021-10-22 | 江苏高科制药设备有限公司 | Air-lift adsorption type supercritical extraction pharmaceutical system |
CN113521796B (en) * | 2021-06-10 | 2022-05-27 | 江苏高科制药设备有限公司 | Air-lift adsorption type supercritical extraction pharmaceutical system |
CN114295791A (en) * | 2022-03-09 | 2022-04-08 | 新疆广陆能源科技股份有限公司 | Tail gas detection system of thermal fluid generator and multi-medium thermal fluid generation system |
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