CN110940752A - Multi-element low-carbon hydrocarbon adsorption and desorption evaluation device and method - Google Patents
Multi-element low-carbon hydrocarbon adsorption and desorption evaluation device and method Download PDFInfo
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- CN110940752A CN110940752A CN201911299243.9A CN201911299243A CN110940752A CN 110940752 A CN110940752 A CN 110940752A CN 201911299243 A CN201911299243 A CN 201911299243A CN 110940752 A CN110940752 A CN 110940752A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/58—Conditioning of the sorbent material or stationary liquid the sorbent moving as a whole
Abstract
The invention discloses a device and a method for evaluating adsorption and desorption of multi-element low-carbon hydrocarbon, wherein the device comprises a gas supply system, a two-channel switching system I, an adsorption and desorption system, a two-channel switching system II, a chromatographic analysis system, a tail gas discharge system, a desorption gas system, an adsorbent discharge and analysis system, an adsorbent online feeding system and a blowing and conveying gas source system; the invention can perform pressurization, long-period and double-channel adsorption and desorption evaluation on various sample gases and adsorbents by utilizing an advanced double-channel switching system, a gas supply system, a high-temperature inert gas desorption system and an adsorbent analysis system, has the characteristics of simple and convenient operation and online result reading, and has better expansibility and market prospect.
Description
Technical Field
The invention relates to a gas adsorption and desorption evaluation technology in the field of energy and chemical industry, in particular to a device and a method for evaluating adsorption and desorption of multi-element low-carbon hydrocarbon.
Background
Volatile Organic Compounds (VOCs) are a generic term for organic compounds having a boiling point of < 260 ℃ at 101.3kPa (20) normal atmosphere and include aliphatic hydrocarbons, aromatic hydrocarbons, halocarbons, oxygenated hydrocarbons, nitrogenous hydrocarbons, sulfur-containing hydrocarbons, and the like. In many chemical industry production, the emission of waste gas containing VOC is always a very prominent problem, and the emission not only causes serious atmospheric pollution, but also greatly wastes resources and increases production cost.
In the energy and chemical industry, light hydrocarbon Volatile Organic Compounds (VOCs) are discharged in all links from raw material mining, transportation and processing to product production, storage and transportation, sale and the like. The low-carbon hydrocarbons pollute the environment, waste resources, cause fire hazards and harm personal safety, and bring serious harm to enterprises and society.
The low-carbon hydrocarbon generally has the characteristics of flammability, explosiveness, toxicity, harm, unstable emission and concentration and large treatment difficulty. The main treatment methods at present are classified into a recovery method and a destruction method. The recovery method may be classified into a condensation method, an absorption method, an adsorption method, a membrane separation method, etc., and the destruction method may be classified into a dilution diffusion method, a direct combustion method, a regenerative catalytic oxidation combustion method, a biological method, and a low-temperature plasma method. However, the research and application of these methods depend on the development of highly efficient adsorbents and advanced evaluation means.
Therefore, there is a need for an accurate and reliable sorbent evaluation device and method to test the performance of the sorbent to guide selection and study. The prior art can only carry out adsorption and desorption measurement on a single gas component under normal pressure, only has a unique measurement channel, has great limitation, and does not have universality and flexibility.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a universal and flexible multielement low-carbon hydrocarbon adsorption and desorption evaluation device and method, and overcomes the defects that the prior art cannot perform adsorption and desorption tests with pressure and can only perform a single channel.
In order to achieve the purpose, the invention adopts the technical scheme that: the system comprises a gas supply system, a two-channel switching system I, an adsorption and desorption system, a two-channel switching system II, a chromatographic analysis system, a tail gas discharge system, a desorption gas system, an adsorbent discharge and analysis system, an adsorbent online feeding system and a blowing and conveying gas source system;
the dual-channel switching system I is connected with the adsorption and desorption system through a pipeline M, L in parallel and then connected with the dual-channel switching system II through a pipeline K, F in parallel, and the dual-channel switching system II is connected with the chromatographic analysis system and the tail gas emission system through a pipeline Z, J in parallel; the gas supply system comprises a multi-element low-carbon hydrocarbon simulation gas system and a multi-element low-carbon hydrocarbon direct feeding system, wherein the multi-element low-carbon hydrocarbon simulation gas system is connected with the double-channel switching system I and provides test sample gas for the adsorption and desorption system; the desorption gas system is also connected with the dual-channel switching system I to provide a desorption gas source for the adsorption and desorption system;
the adsorbent discharge and analysis system is connected with the dual-channel switching system I through a parallel pipeline R, S, and the adsorbent online feeding system is obliquely connected with a pipeline K, F of the adsorption and desorption system at an interface through a parallel feeding pipeline Q, W; the purging and conveying gas source system is communicated with a feeding pipeline Q, W of the adsorbent on-line feeding system.
The multi-element low-carbon hydrocarbon simulation gas system comprises V1-Vn single-component gas supply systems; each single-component gas supply system comprises a gas supply device V, a pressure fine control valve, a flow fine control valve and an automatic flow control valve which are connected in sequence; each two groups of single-component gas supply systems are connected in parallel, then connected with the first-stage mixer and then connected in parallel;
the multi-element low-carbon hydrocarbon direct feeding system comprises a multi-element low-carbon hydrocarbon mixed gas collecting tank, a pressure fine control valve, a flow fine control valve, an automatic flow control valve and a to-be-detected gas direct interface which is vertically connected between the multi-element low-carbon hydrocarbon mixed gas collecting tank and the pressure fine control valve, wherein the multi-element low-carbon hydrocarbon mixed gas collecting tank, the pressure fine control valve, the flow fine control valve and the automatic flow control valve are sequentially;
the multi-element low-carbon hydrocarbon simulation gas system is connected with the multi-element low-carbon hydrocarbon direct feeding system in parallel and then connected with the dual-channel switching system I through the secondary mixer.
The adsorption and desorption system comprises an adsorption desorber I and an adsorption desorber II which are connected in parallel, the incoming direction of the adsorption desorber I is connected to the discharging direction of an adsorption and desorption system feed valve I arranged between the adsorption desorber I and the double-channel switching system I and is connected to a pipeline K, and the incoming direction of the adsorption desorber II is connected to the discharging direction of an adsorption and desorption system feed valve II arranged between the adsorption desorber II and the double-channel switching system I and is connected to a pipeline F.
The adsorption desorber I and the adsorption desorber II respectively comprise a barrel-shaped heater, an adsorbent positioned in the center of the barrel-shaped heater, and an adsorbent fixed filtering device and a quick loading and unloading device which are respectively arranged at two ends of the barrel-shaped heater;
the barrel-shaped heater comprises one or more of electric heating, water bath heating, oil bath heating and steam heating; the adsorbent is one or a combination of more of activated carbon, a coke powder modified product, a high-performance adsorption carbon material and aerogel; the adsorbent fixing and filtering device is one or a combination of asbestos, metal sinter, alloy net and glass wool.
The desorption gas system comprises a desorption gas source, a pressure fine control valve, a flow fine control valve and an automatic flow control valve which are connected in sequence;
the adsorbent discharging and analyzing system comprises an adsorbent discharging valve I arranged on a pipeline R and an adsorbent discharging valve II arranged on a pipeline S; the pipelines R and S are connected in parallel and then are converged and connected with an adsorbent collecting tank, and then are connected with an adsorbent analyzer;
the adsorbent analyzer is one or more combination of BET, XRD and FT-IR analyzers;
the desorption gas source is one or the combination of a plurality of nitrogen, air, carbon dioxide, helium and steam.
The blowing and conveying gas source system is divided into two paths which are connected in parallel, wherein one path is connected with the material inlet end of an adsorbent discharge valve I and an adsorbent discharge valve II on a material feeding pipeline Q, W; one path is connected with a feeding valve I of the adsorption and desorption system, a feeding valve II of the adsorption and desorption system, an adsorbent discharge valve I, an adsorbent discharge valve II and a pipeline R, S, so that the pressurized online transportation of the adsorbent and the pneumatic blockage removal of each pipeline are realized.
The chromatographic analysis system comprises a pressure remote monitor, a filter, a system back-pressure valve, a total flow monitor and a backflow prevention device which are respectively connected to a pipeline Z and a pipeline J in sequence; the total flow monitor and the backflow prevention device of the pipeline J are connected with the chromatograph through a quick-release reducing and micro-flow control valve;
the tail gas discharge system comprises a tail gas stop valve, a fire retardant device and an emptier which are sequentially connected, wherein the tail gas stop valve is connected with an outlet of a backflow prevention device of the chromatographic analysis system.
The online adsorbent feeding system comprises an adsorbent temporary storage tank, a weighing instrument and a powder cut-off valve which are sequentially connected, and the outlet of the powder cut-off valve is respectively connected with a parallel feeding pipeline Q, W.
The method for evaluating the adsorption and desorption of the multi-element low-carbon hydrocarbon is characterized by comprising the following steps of:
step one, an adsorbent loading and system cleaning process:
1.1, placing adsorbent fixing and filtering devices at the upper and lower ends of an adsorption desorber I and an adsorption desorber II, loading an adsorbent in an adsorbent temporary storage tank, opening a purging and conveying gas source system, introducing conveying gas to an adsorbent online feeding system, conveying the adsorbent into the adsorption desorption system through pneumatic conveying of the purging and conveying gas source system, and recording the loading capacity of the adsorbent after the adsorbent is completely filled;
1.2, setting the pressure, flow and replacement time of a desorption gas system, and replacing the adsorption desorption system by using a purging desorption gas source gas and simultaneously checking the air tightness of the pipeline of the device;
step two, switching the sample gas:
the control gas supply system switches under the three kinds of states of the independent gas supply of many first low carbon hydrocarbon simulation gas system, the independent gas supply of many first low carbon hydrocarbon direct feed system and two systems mix the gas supply, realizes the gas supply of different sample:
1) independent gas supply of the multi-element low-carbon hydrocarbon simulation gas system: connecting single-component gas supply systems with V1-Vn different gas components into a multi-component low-carbon hydrocarbon simulation gas system, and setting the opening degrees of a pressure fine control valve, a flow fine control valve and an automatic flow control valve of each group of single-component gas supply systems until the values of the automatic flow control valve and a total flow monitor of the single-component gas supply systems meet the test requirements;
2) independent gas supply of a multi-element low-carbon hydrocarbon direct feeding system: collecting a multi-element low-carbon hydrocarbon mixed gas sample by using a multi-element low-carbon hydrocarbon mixed gas collecting tank or directly connecting multi-element low-carbon hydrocarbon into a direct interface of gas to be tested, and setting the opening degrees of a pressure fine control valve, a flow fine control valve and an automatic flow control valve of a multi-element low-carbon hydrocarbon direct feeding system until the numerical value of the flow automatic flow control valve and the numerical value of a total flow monitor meet test requirements;
3) two systems mix the air supply: the multi-element low-carbon hydrocarbon mixed gas collection tank and the single-component gas supply system work simultaneously, the multi-element low-carbon hydrocarbon mixed gas collection tank and the single-component gas supply system are mixed in a secondary mixer, and the opening degree of a pressure fine control valve, a flow fine control valve and an automatic flow control valve of each system is set until the numerical value of the flow automatic flow control valve and the numerical value of a total flow monitor meet the test requirements;
step three, an adsorption evaluation process:
3.1, operating the dual-channel switching system I to enable the gas to be detected to enter the adsorption desorber I, and enabling the gas after adsorption to enter a chromatograph for analysis through a pipeline J by the dual-channel switching system II;
3.2, adjusting the numerical value of a system back-pressure valve on the pipeline J to be a process set value;
3.3, according to the test requirements, controlling the working state of the gas supply system according to the step two, and starting the adsorption process;
3.4, connecting the chromatograph to the system through quick disassembly and reducing, and allowing part of sample gas to enter the chromatograph for analysis and adsorption after the sample gas is adjusted by a micro-flow control valve to meet the requirement of the instrument;
3.5, a double-channel adsorption process:
when the removal rate gamma of the chromatograph analysis in the step 3.4 is lower than 10-70%, operating the dual-channel switching system I to enable the gas to be detected to enter the adsorption desorber II, enabling the gas after adsorption to enter the chromatograph for analysis through the pipeline J through the dual-channel switching system II, then repeating the step 3.2-3.4, and stopping the adsorption test or performing long-period adsorption test of online feeding by utilizing an adsorbent online feeding system to online add the adsorbent until the removal rate gamma of the chromatograph analysis is lower than 10-70%;
step four, desorption and analysis process:
with the two-channel switching system I and the two-channel switching system II, the desorption process can be switched between A, B, C three states:
a, simultaneously desorbing by an adsorption desorber I and an adsorption desorber II
a1) Operating the states of the two-channel switching system I and the two-channel switching system II to enable desorbed gas to enter the adsorption desorber I and the adsorption desorber II which are connected in parallel;
a2) setting the purging replacement pressure P of a desorption gas system to be 0.0-5.0 MPa, and enabling the numerical value of the automatic flow control valve and the numerical value of the total flow monitor to meet the test requirement;
a3) opening the barrel-shaped heater to enable the barrel-shaped heater to reach a set temperature T of 50-500 ℃, and regenerating the heating adsorbent;
a4) stopping the desorption gas system, closing the barrel-shaped heater, opening a feed valve I of the adsorption and desorption system, a feed valve II of the adsorption and desorption system, a discharge valve I of the adsorbent and a discharge valve II of the adsorbent when the pressure of the system is reduced to normal pressure, and enabling the adsorbent to enter an adsorbent collecting tank;
a5) carrying out BET, XRD and FT-IR analysis on the adsorbent in the adsorbent collecting tank by using an adsorbent analyzer, and calculating the adsorption capacity U of the adsorbent;
b, adsorption by an adsorption desorber I and desorption by an adsorption desorber II are carried out simultaneously:
b1) operating the state of the two-channel switching system I to enable the gas to be detected of the gas supply system to enter an adsorption desorber I for an adsorption test, simultaneously operating the two-channel switching system II to enable the gas after adsorption to enter a chromatograph for analysis through a pipeline J, and then performing the adsorption evaluation process of the step 3.2-3.3 by the adsorption desorber I;
b2) meanwhile, operating the state of the dual-channel switching system I to enable desorbed gas of the desorbed gas system to enter an adsorption desorber II, operating the dual-channel switching system II to enable the adsorption desorber II to be connected into a tail gas discharge system after being connected into a pipeline Z, setting a pressure fine control valve of the desorbed gas system to a blowing replacement pressure P which is 0.0-5.0 MPa, adjusting a flow fine control valve and an automatic flow control valve of the desorbed gas system until the numerical value of the flow automatic flow control valve and the numerical value of a total flow monitor reach test requirements, opening a barrel-shaped heater to enable the desorption temperature to reach a set temperature T which is 50-500 ℃, blowing a desorbed gas source to enter the adsorption desorber II to regenerate an adsorbent, stopping the desorbed gas system, closing the barrel-shaped heater, opening a feeding valve II of the adsorption desorber system and an adsorbent discharging valve II when the system pressure P is reduced to normal pressure, enabling the adsorbent to enter an adsorbent, carrying out BET, XRD and FT-IR analysis on the adsorbent in the adsorbent collecting tank by using an adsorbent analyzer, and calculating the adsorption capacity U of the adsorbent;
c, desorption of the adsorption desorber I and adsorption of the adsorption desorber II are carried out simultaneously:
c1) operating the state of the two-channel switching system I to enable the gas to be detected of the gas supply system to enter an adsorption desorber II for an adsorption test, simultaneously operating the two-channel switching system II to enable the gas after adsorption to enter a chromatograph for analysis through a pipeline J, and then performing the adsorption evaluation process of the step 3.2-3.3 by the adsorption desorber II;
c2) simultaneously, operating a dual-channel switching system I state to enable desorbed gas of a desorbed gas system to enter an adsorption desorber I, operating a dual-channel switching system II to enable the adsorption desorber I to be connected into a pipeline Z and then connected into a tail gas discharge system, setting a pressure fine control valve of the desorbed gas system to a blowing replacement pressure P which is 0.0-5.0 MPa, adjusting a flow fine control valve and an automatic flow control valve of the desorbed gas system until the numerical value of the flow automatic flow control valve and the numerical value of a total flow monitor reach test requirements, opening a barrel-shaped heater to enable the desorption temperature to reach a set temperature T which is 50-500 ℃, blowing a desorbed gas source to enter the adsorption desorber I for adsorbent regeneration, stopping the desorbed gas system, closing the barrel-shaped heater, opening an adsorption desorption system feed valve I and an adsorbent discharge valve I when the system pressure P is reduced to normal pressure, enabling the adsorbent to enter an adsorbent collection tank, carrying out BET, XRD and FT-IR analysis on the adsorbent in the adsorbent collecting tank by using an adsorbent analyzer, and calculating the adsorption capacity U of the adsorbent;
step five, removing system blockage:
and when one or more combinations of the adsorption and desorption system feed valve I, the adsorption and desorption system feed valve II, the adsorbent discharge valve I, the adsorbent discharge valve II and the pipeline R, S are blocked, the purging and conveying gas source system is opened to remove the blockage.
The calculation method of the removal rate gamma and the adsorption capacity U of the adsorbent comprises the following steps:
(1) the calculation method of the removal rate gamma comprises the following steps:
γ＝(Co-Ct)/C0×100
in the formula, Ct-component concentration at a certain moment, vol%;
C0-initial state component concentration, vol%;
gamma-removal rate,%;
(2) the method for calculating the adsorption capacity U of the adsorbent comprises the following steps:
in the formula, C0-initial concentration of a certain component, mol%;
Ct-the outlet concentration of a certain component at time t,% mol;
m-sorbent loading, g;
t-adsorption time, min;
fv-adsorbed gas flow, L/min;
Mf-the relative molecular mass of a certain component, g/mol;
u-adsorbent adsorption capacity, g/100g adsorbent.
The invention has the beneficial effects that:
the invention can realize the normal pressure and pressure adsorption and high temperature inert gas desorption of various gas samples by the gas supply system consisting of the multielement low carbon hydrocarbon simulation gas system and the multielement low carbon hydrocarbon direct feeding system, solves the defects that the prior art can not carry out the pressure adsorption and can only carry out the adsorption and desorption test by a single channel, finally realizes the pressurization, long period and two-channel evaluation of various sample gases and adsorbents by utilizing the advanced normal pressure and pressure two-channel switching system, the gas supply system, the adsorbent analysis system and the high temperature inert gas desorption, has the characteristics of simple operation and online reading of results, and has better expansibility and market prospect.
The invention also discloses a double-channel adsorption and desorption evaluation method based on the double-channel switching system I and the double-channel switching system II, which can realize a long-period adsorption test and a double-channel adsorption test and desorption test respectively; a system blockage removal method based on a blowing and conveying gas source; provides a multivariate low-carbon hydrocarbon adsorption and desorption evaluation method, a desorption rate gamma and an adsorbent adsorption capacity U calculation method.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention
FIG. 2 is a schematic view of the structure of the adsorption desorber I24 and the adsorption desorber II25 of the present invention
In the figure: 1. an air supply system; 2. a double-channel switching system I; 3. an adsorption-desorption system; 4. a dual-channel switching system II; 5. a chromatographic analysis system; 6. a tail gas exhaust system; 7. a stripping gas system; 8. an adsorbent discharge and analysis system; 9. an adsorbent on-line feeding system; 10. purging the delivery gas source system; 11. a desorption gas source; 12. a multi-element low-carbon hydrocarbon simulation gas system; 13. a multi-element low-carbon hydrocarbon direct feeding system; 14. a pressure fine control valve; 15. a flow fine control valve; 16. an automatic flow control valve; 17. a first-stage mixer; 18. a monocomponent gas supply system; 19. a multi-element low-carbon hydrocarbon mixed gas collection tank; 20. a direct interface of gas to be measured; 21. a secondary mixer; 22. a feed valve I of the adsorption and desorption system; 23. a feed valve II of the adsorption and desorption system; 24. an adsorption desorber I; 25. an adsorption desorber II; 26. an adsorbent discharge valve I; 27. an adsorbent discharge valve II; 28 an adsorbent collection tank; 29. an adsorbent analyzer; 30. an adsorbent temporary storage tank; 31. a weighing instrument; 32. a powder cut-off valve; 33. an adsorbent discharge valve I; 34. an adsorbent discharge valve II; 35. a remote monitor of pressure; 36. a filter; 37. a system pressure backup valve; 38. a total flow monitor; 39. a backflow prevention device; 40. quick-release and diameter-changing; 41. a micro flow control valve; 42. a chromatograph; 43. a shut-off valve; 44. a fire retardant device; 45. an evacuator; 46. a quick loading and unloading device; 47. an adsorbent fixed filter device; 48. a barrel heater; 49. an adsorbent.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the invention thereto.
The general structure of the invention is different from the traditional adsorption and desorption device, the special designed gas supply system 1, the double-channel switching system I2, the double-channel switching system II 4, the adsorption and desorption device I24 and the adsorption and desorption device II25 can provide the normal pressure, pressure adsorption and high temperature inert gas desorption of multiple sample gases under the conditions of special proportioning of multi-element low carbon hydrocarbon simulation gas and multi-element low carbon hydrocarbon direct feeding, and the like, and the pressurization and long-period double-channel adsorption and desorption test of multiple sample gases and adsorbents can be further realized based on the double-channel switching system I2 and the double-channel switching system II 4.
Because the invention has a plurality of operation schemes, the invention is further described in detail by taking the operation process of simulating gas double-channel pressurized adsorption by multi-element low-carbon hydrocarbon, and simultaneously carrying out adsorption by the adsorption desorber I24 and desorption by the adsorption desorber II25 as an example.
Referring to fig. 1, the multi-element low-carbon hydrocarbon adsorption desorption evaluation device comprises an air supply system 1, a two-channel switching system I2, an adsorption desorption system 3, a two-channel switching system II 4, a chromatographic analysis system 5, a tail gas discharge system 6, a desorption gas system 7, an adsorbent discharge and analysis system 8, an adsorbent online feeding system 9 and a purging and conveying air source system 10.
The gas supply system 1 is connected with the dual-channel switching system I2, then connected with the adsorption and desorption system 3 through a parallel pipeline M, L, and then connected with the dual-channel switching system II 4 through a parallel pipeline K, F, and the dual-channel switching system II 4 is connected with the chromatographic analysis system 5 through a parallel pipeline Z, J, and then connected with the tail gas discharge system 6. The sorbent discharge and analysis system 8 is connected to the two-channel switching system I2 by a parallel line R, S. The adsorbent in-line feed system 9 is connected diagonally to the outlet line K, F of the adsorption and desorption system 2 via a parallel feed line Q, W.
The multi-element low-carbon hydrocarbon simulated gas system 12 and the multi-element low-carbon hydrocarbon direct feeding system 13 form a gas supply system 1, and the multi-element low-carbon hydrocarbon simulated gas system 12 and the multi-element low-carbon hydrocarbon direct feeding system 13 are connected in parallel and then connected with the secondary mixer 21; the multi-element low-carbon hydrocarbon simulation gas system 12 comprises V1-Vn single-component gas supply systems 18; each single-component gas supply system 18 comprises a gas supply device V, a pressure fine control valve 14, a flow fine control valve 15 and an automatic flow control valve 16 which are connected in sequence; and each two groups of single-component gas supply systems 18 are connected in parallel, then are connected with the first-stage mixer 17, and then are connected in parallel.
The multi-element low-carbon hydrocarbon direct feeding system 13 comprises a multi-element low-carbon hydrocarbon mixed gas collecting tank 19, a pressure fine control valve 14, a flow fine control valve 15, an automatic flow control valve 16 and a to-be-detected gas direct interface 20 which is vertically connected between the multi-element low-carbon hydrocarbon mixed gas collecting tank 19 and the pressure fine control valve 14, wherein the multi-element low-carbon hydrocarbon mixed gas collecting tank 19, the pressure fine control valve 14, the flow fine control valve 15 and the automatic; the gas supply system 1 can automatically distribute gas according to different sample gas requirements required by evaluation tests or directly use a gas collection tank to directly supply gas.
The gas supply system 1 can realize evaluation and analysis of various gas samples:
scheme one, simulating sample gas by using multi-element low-carbon hydrocarbon. The multi-component low-carbon hydrocarbon simulated gas system 12 can simulate and evaluate sample gases with different compositions required by a test through V1-Vn single-component gas supply systems 18, each single-component gas supply system 18 is connected with a pressure fine control valve 14, a flow fine control valve 15 and an automatic flow control valve 16, and the single-component gas quantity entering a first-stage mixer 17 can be accurately controlled, so that the gas proportion of the multi-component low-carbon hydrocarbon simulated gas system 12 is accurate;
scheme two, directly feeding the multi-element low-carbon hydrocarbon. The sample gas access system can be directly acquired by adopting a multi-element low-carbon hydrocarbon mixed gas acquisition tank 19 or the multi-element low-carbon hydrocarbon mixed gas is directly accessed into a gas direct interface 20 to be detected for detection and analysis.
The gas supply system 1 can be switched between different gas source combinations A, B, C according to the experimental requirements:
A. multi-element low-carbon hydrocarbon simulation gas adsorption process
Switching the gas supply system 1 to the working state of a multi-component low-carbon hydrocarbon simulation gas system 12, connecting V1-Vn single-component gas supply systems 18 with different gas components into the multi-component low-carbon hydrocarbon simulation gas system 12, and setting the opening degrees of a pressure fine control valve 14, a flow fine control valve 15 and an automatic flow control valve 16 of each group of single-component gas supply systems 18 until the values of the automatic flow control valve 16 and a total flow monitor 38 of the single-component gas supply systems 18 reach the test requirements;
B. low carbon hydrocarbon direct feed adsorption process
Switching the gas supply system 1 to the working state of the multi-element low-carbon hydrocarbon direct feeding system 13, collecting a multi-element low-carbon hydrocarbon mixed gas sample by using a multi-element low-carbon hydrocarbon mixed gas collecting tank 19, connecting the multi-element low-carbon hydrocarbon mixed gas sample to the multi-element low-carbon hydrocarbon direct feeding system 13, setting the opening degrees of a pressure fine control valve 14, a flow fine control valve 15 and an automatic flow control valve 16 of the multi-element low-carbon hydrocarbon direct feeding system 13, and enabling the numerical value of the automatic flow control valve 16 and the numerical value of a total flow monitor 38 to meet the;
C. simulation of gas and low-carbon hydrocarbon direct feeding mixed feeding adsorption process
The gas supply system 1 is switched to the simultaneous working state of the multi-element low-carbon hydrocarbon simulation gas system 12 and the multi-element low-carbon hydrocarbon direct feeding system 13, the multi-element low-carbon hydrocarbon mixed gas collecting tank 19 is used for collecting multi-element low-carbon hydrocarbon mixed gas samples and is connected to the multi-element low-carbon hydrocarbon direct feeding system 13, the opening degrees of a pressure fine control valve 14, a flow fine control valve 15 and an automatic flow control valve 16 of the system are set to meet the test requirements, meanwhile, according to the test requirements, a corresponding single-component gas supply system 18 is connected to the multi-component low-carbon hydrocarbon simulation gas system 12, the opening degrees of a pressure fine control valve 14, a flow fine control valve 15 and an automatic flow control valve 16 of the single-component gas supply system 18 are set to meet the test requirements, the gas of the multi-component low-carbon hydrocarbon mixed gas collecting tank 19 and the gas of the single-component gas supply system 18 enter an adsorption desorber after being mixed in a secondary mixer 21, and the numerical value of a total flow monitor 38 also needs to meet the test requirements in the test process.
The desorption gas system 7 comprises a desorption gas source 11, a pressure fine control valve 14, a flow fine control valve 15 and an automatic flow control valve 16 which are connected in sequence and used for providing a desorption gas source with stable flow and controllable pressure for the system. The desorption gas source 11 is one or a combination of more of high pressure nitrogen, low pressure nitrogen, air, carbon dioxide, helium and steam.
The adsorption and desorption system 3 comprises two groups of parallel sequentially connected adsorption and desorption system feed valves I22, adsorption and desorption devices I24, adsorption and desorption system feed valves II 23 and adsorption and desorption devices II25, and the switching among three states of ① adsorption and desorption devices I24 and II25 adsorption and desorption, ② adsorption and desorption devices I24 and II25 desorption, and ③ adsorption and desorption devices I24 and II25 adsorption can be realized through a double-channel switching system I2.
The adsorbent discharge and analysis system 8 comprises a pipeline R connected with an adsorbent discharge valve I26 and a pipeline S connected with an adsorbent discharge valve II 27 which are connected in parallel, the parallel pipelines R and S are converged and then connected with an adsorbent collecting tank 28 and then connected with an adsorbent analyzer 29, three states of singly discharging the adsorbent by an ① adsorption desorber I24, singly discharging the adsorbent by an adsorption desorber ②, singly discharging the adsorbent by the adsorption desorber I24 and simultaneously discharging the adsorbent by the adsorption desorber ③ can be switched by matching among a double-channel switching system I2, the adsorption desorber II 26 and the adsorbent discharge valve II 27, and the adsorbent analyzer 29 is one or a combination of a plurality of BET, XRD and FT-IR analyzers, can specifically evaluate the characteristics of the adsorbent after adsorption is finished, and can be compared with the characteristics of fresh activated carbon to examine the analysis and regeneration effect.
The online adsorbent feeding system 9 comprises an adsorbent temporary storage tank 30, a weighing instrument 31, a powder cut-off valve 32, an adsorbent discharge valve I33 and an adsorbent discharge valve II 34 which are connected in parallel. The temporary adsorbent storage tank 30 is used for storing fresh adsorbent, the feeding amount can be calculated through the difference weight of the weighing instrument 31 before and after feeding, and the pressurized online pneumatic conveying and feeding of the adsorbent can be realized through the blowing conveying air source system 10.
The chromatographic analysis system 5 comprises a pipeline Z, J connected in parallel, and each pipeline Z, J comprises a pressure remote monitor 35, a filter 36, a system back-pressure valve 37, a total flow monitor 38 and a backflow prevention device 39 which are connected in sequence; the quick-release reducing device 40, the micro-flow control valve 41 and the chromatograph 42 are sequentially connected and then connected between the total flow monitoring device 38 and the backflow preventing device 39, and the rear end of the backflow preventing device 39 is connected to the tail gas emission system 6.
The tail gas discharge system 6 comprises a tail gas cut-off valve 43, a fire retardant device 44 and an air release device 45 which are connected in sequence. Most of a large amount of detection gas from the adsorption and desorption system 3 is discharged through the tail gas discharge system 6, and a small amount of detection gas enters the chromatograph 42 for analysis and removal rate after being controlled by the micro flow control valve 41.
The blowing and conveying gas source system 10 is divided into two paths which are connected in parallel, wherein one path is connected with the material inlet end of an adsorbent discharge valve I33 and an adsorbent discharge valve II 34 on a feeding pipeline Q, W; one path is connected with an adsorption and desorption system feed valve I22, an adsorption and desorption system feed valve II 23, an adsorbent discharge valve I26, an adsorbent discharge valve II 27, an adsorbent discharge valve I33, an adsorbent discharge valve II 34 and a pipeline R, S, so that the online conveying of the adsorbent under pressure and the pneumatic blockage removal of each pipeline are realized.
Referring to fig. 2, the adsorption desorber I24 and the adsorption desorber II25 have the same structure, and each include a barrel heater 48, an adsorbent 49 located in the center of the barrel heater 48, and an adsorbent fixing and filtering device 47 and a quick loading and unloading device 46 connected to both ends of the adsorbent 49 in the center; the adsorbent 49 is one or a combination of more of activated carbon, coke powder modified products, high-performance adsorbent carbon materials and aerogel; the barrel heater 48 comprises one or more of electric heating, water bath heating, oil bath heating and steam heating; the adsorbent fixing and filtering device 47 is one or a combination of asbestos, metal sinter, alloy mesh and glass wool. The barrel heater 48 can perform heating desorption on the adsorbent 49; the fixed filtering devices 47 of the absorbent at the two ends of the absorbent desorber can play a role in filtering or preventing the absorbent 49 particles in the bed layer from being brought out of the device by gas, and the quick loading and unloading device 46 can realize the quick loading and unloading and dredging and blockage removal of the absorbent desorber.
The method for evaluating the adsorption and desorption of the multi-element low-carbon hydrocarbon comprises the following steps:
step one, an adsorbent loading and system cleaning process:
1.1 recording initial reading W of weighing instrument 31 after loading adsorbent 49 in adsorbent temporary storage tank 301Then, adsorbent fixing and filtering devices 47 are arranged at the upper end and the lower end of the adsorption desorber I24 and the adsorption desorber II25, a blowing and conveying air source system 10 is opened to introduce conveying air to an adsorbent online feeding system 9, a powder stop valve 32, an adsorbent discharge valve I33 and an adsorbent discharge valve II 34 which are connected in parallel are opened, an adsorbent 49 is pneumatically conveyed to the adsorption desorber I24 and the adsorption desorber II25 through the blowing and conveying air source system 10, and after the adsorbent is completely filled, the finishing indication W of a weighing instrument 31 is recorded2；
1.2 setting a pressure fine control valve 14 of the desorption gas system 7 to be a replacement pressure P of 0.5-5 MPa, slowly opening a flow fine control valve 15 of the desorption gas system 7, setting an automatic flow control valve 16 to be a test requirement, replacing an adsorbent 49 bed layer T1 with a gas of a purging desorption gas source 11 for 5-20 min, and checking the air tightness of a device pipeline;
step two, switching the sample gas:
the multi-element low-carbon hydrocarbon simulation gas system 12 independently supplies gas: the method comprises the steps of connecting V1-Vn single-component gas supply systems 18 with different gas components into a multi-component low-carbon hydrocarbon simulation gas system 12, and setting the opening degrees of a pressure fine control valve 14, a flow fine control valve 15 and an automatic flow control valve 16 of each group of single-component gas supply systems 18 until the values of the automatic flow control valve 16 and a total flow monitor 38 of the single-component gas supply systems 18 meet test requirements;
the invention can also independently supply air through a multi-element low-carbon hydrocarbon direct feeding system 13: collecting a multi-element low-carbon hydrocarbon mixed gas sample by using a multi-element low-carbon hydrocarbon mixed gas collecting tank 19 or directly connecting multi-element low-carbon hydrocarbon into a direct gas interface 20 to be tested, and setting the opening degrees of a pressure fine control valve 14, a flow fine control valve 15 and an automatic flow control valve 16 of a multi-element low-carbon hydrocarbon direct feeding system 13 until the numerical value of the automatic flow control valve 16 and the numerical value of a total flow monitor 38 meet the test requirements;
the invention can also mix the gas supply through two systems: the multi-element low-carbon hydrocarbon mixed gas acquisition tank 19 and the single-component gas supply system 18 work simultaneously and are mixed in the secondary mixer 21, and the opening degrees of the pressure fine control valve 14, the flow fine control valve 15 and the automatic flow control valve 16 of each system are set until the numerical value of the flow automatic flow control valve 16 and the numerical value of the total flow monitor 38 meet the test requirements;
step three, an adsorption evaluation process:
3.1, operating a double-channel switching system I2 to enable the gas to be detected to enter an adsorption desorber I24, and enabling the gas after adsorption to enter a chromatograph 42 for analysis through a pipeline J by virtue of a double-channel switching system II 4;
3.2, adjusting the numerical value of a system back-pressure valve 37 on the pipeline J to be a process set value;
3.3, according to the test requirements, controlling the working state of the gas supply system 1 according to the step two, and starting the adsorption process;
3.4, connecting a chromatograph 42 to the system through the quick-release reducing valve 40, adjusting part of sample gas through the micro-flow control valve 41 to meet the instrument requirement, and then entering the chromatograph 42 to analyze the adsorption effect;
3.5, a double-channel adsorption process:
when the removal rate gamma of the chromatograph 42 analyzed in the step 3.4 is lower than 10-70%, operating the dual-channel switching system I2 to enable the gas to be detected to enter the adsorption desorber II25, enabling the gas after adsorption to enter the chromatograph 42 from the pipeline J through the dual-channel switching system II 4 for analysis, and then repeating the step 3.2-3.4 until the removal rate gamma of the chromatograph 42 analyzed is lower than 10-70%, and stopping the adsorption test;
step four, desorption and analysis process:
by means of the two-channel switching system I2 and the two-channel switching system II 4, the desorption process is switched to the mode B simultaneous adsorption and desorption process by the adsorption desorber I24 and desorption by the adsorption desorber II 25:
b1) operating the state of the two-channel switching system I2 to enable the gas to be detected of the gas supply system 1 to enter an adsorption desorber I24 for an adsorption test, simultaneously operating the two-channel switching system II 4 to enable the gas after adsorption to enter a chromatograph 42 for analysis through a pipeline J, and then performing the adsorption evaluation process of the steps 3.2-3.3 by the adsorption desorber I24;
b2) meanwhile, the state of the dual-channel switching system I2 is operated, so that desorbed gas of the desorbed gas system 7 enters an adsorption desorber II25, the dual-channel switching system II 4 is operated, so that the adsorption desorber II25 is connected to the pipeline Z and then connected to the tail gas discharge system 6, the pressure fine control valve 14 of the desorbed gas system 7 is set to the purging replacement pressure P which is 0.0-5.0 MPa, the flow fine control valve 15 and the automatic flow control valve 16 of the desorbed gas system 7 are adjusted until the numerical value of the automatic flow control valve 16 and the numerical value of the total flow monitor 38 reach the test requirements, the barrel heater 48 is opened to enable the desorption temperature to reach the set temperature T which is 50-500 ℃, the purging desorption gas source 11 enters the adsorption desorber II25 to regenerate the adsorbent 49, the desorbed gas system 7 is stopped, the barrel heater 48 is closed, and when the system pressure P is reduced to the normal pressure, the inlet valve II 23 of the adsorption desorption, The adsorbent discharge valve II 27 is used for introducing the adsorbent into an adsorbent collecting tank 28, and the adsorbent analyzer 29 is used for carrying out BET, XRD and FT-IR analysis on the adsorbent in the adsorbent collecting tank 28 to calculate the adsorption capacity U of the adsorbent;
the desorption and analysis process can also be performed by A, C two ways:
simultaneous desorption by the desorber I24 and the desorber II 25:
a1) operating the state of the two-channel switching system I2 and the state of the two-channel switching system II 4 to enable desorbed gas to enter an adsorption desorber I24 and an adsorption desorber II25 which are connected in parallel;
a2) setting the purging replacement pressure P of the desorption gas system 7 to be 0.0-5.0 MPa, and simultaneously enabling the numerical value of the automatic flow control valve 16 and the numerical value of the total flow monitor 38 to meet the test requirement;
a3) opening the barrel-shaped heater 48 to enable the barrel-shaped heater 48 to reach a set temperature T of 50-500 ℃, and regenerating the heating adsorbent;
a4) stopping the desorption gas system 7, closing the barrel-shaped heater 48, opening the adsorption and desorption system feed valve I22, the adsorption and desorption system feed valve II 23, the adsorbent discharge valve I26 and the adsorbent discharge valve II 27 when the system pressure is reduced to the normal pressure, and enabling the adsorbent to enter the adsorbent collecting tank 28;
a5) the adsorbent analyzer 29 is used to perform BET, XRD, and FT-IR analyses on the adsorbent 49 in the adsorbent collection tank 28, and calculate the adsorbent adsorption capacity U;
c, desorption by an adsorption desorber I24 and adsorption by an adsorption desorber II25 are carried out simultaneously:
c1) operating the state of the two-channel switching system I2 to enable the gas to be detected of the gas supply system 1 to enter an adsorption desorber II25 for an adsorption test, simultaneously operating the two-channel switching system II 4 to enable the gas after adsorption to enter a chromatograph 42 for analysis through a pipeline J, and then performing the adsorption evaluation process of the steps 3.2-3.3 on the adsorption desorber II 25;
c2) meanwhile, the state of the dual-channel switching system I2 is operated, so that desorbed gas of the desorbed gas system 7 enters an adsorption desorber I24, the dual-channel switching system II 4 is operated, so that the adsorption desorber I24 is connected to a pipeline Z and then connected to a tail gas discharge system 6, a pressure fine control valve 14 of the desorbed gas system 7 is set to a purging replacement pressure P of 0.0-5.0 MPa, a flow fine control valve 15 and an automatic flow control valve 16 of the desorbed gas system 7 are adjusted until the numerical value of a flow automatic flow control valve 16 and the numerical value of a total flow monitor 38 reach test requirements, a barrel heater 48 is opened to enable the desorption temperature to reach a set temperature T of 50-500 ℃, a purging desorption gas source 11 enters the adsorption desorber I24 to regenerate an adsorbent 49, the desorbed gas system 7 is stopped, the barrel heater 48 is closed, and when the system pressure P is reduced to normal pressure, an adsorption desorption system inlet valve I22 of the adsorption desorption, The adsorbent discharge valve I26 is used for introducing the adsorbent into an adsorbent collecting tank 28, and the adsorbent analyzer 29 is used for carrying out BET, XRD and FT-IR analysis on the adsorbent in the adsorbent collecting tank 28 to calculate the adsorption capacity U of the adsorbent;
step five: and (3) removing system blockage:
and when one or more combinations of the adsorption and desorption system feed valve I22, the adsorption and desorption system feed valve II 23, the adsorbent discharge valve I26, the adsorbent discharge valve II 27, the adsorbent discharge valve I33, the adsorbent discharge valve II 34 and the pipeline R, S are blocked, the purging and conveying gas source system 10 is opened for blockage removal.
The calculation method of the removal rate gamma and the adsorption capacity U of the adsorbent 49 comprises the following steps:
(1) the calculation method of the removal rate gamma comprises the following steps:
γ＝(Co-Ct)/C0×100
in the formula, Ct-component concentration at a certain moment, vol%;
C0-initial state component concentration, vol%;
gamma-removal rate,%;
(2) the method for calculating the adsorption capacity U of the adsorbent comprises the following steps:
in the formula, C0-initial concentration of a certain component, mol%;
Ct-the outlet concentration of a certain component at time t,% mol;
m-sorbent loading, g;
t-adsorption time, min;
fv-adsorbed gas flow, L/min;
Mf-the relative molecular mass of a certain component, g/mol;
u-adsorbent adsorption capacity, g/100g adsorbent.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.
Claims (10)
1. A device for evaluating the adsorption and desorption of multi-element low-carbon hydrocarbon is characterized in that: the system comprises a gas supply system (1), a double-channel switching system I (2), an adsorption and desorption system (3), a double-channel switching system II (4), a chromatographic analysis system (5), a tail gas discharge system (6), a desorption gas system (7), an adsorbent discharge and analysis system (8), an adsorbent online feeding system (9) and a blowing and conveying gas source system (10);
the dual-channel switching system I (2) is connected with the adsorption and desorption system (3) through a pipeline M, L in parallel and then connected with the dual-channel switching system II (4) through a pipeline K, F in parallel, and the dual-channel switching system II (4) is connected with the chromatographic analysis system (5) and the tail gas discharge system (6) through a pipeline Z, J in parallel; the gas supply system (1) comprises a multi-element low-carbon hydrocarbon simulation gas system (12) and a multi-element low-carbon hydrocarbon direct feeding system (13), wherein the multi-element low-carbon hydrocarbon simulation gas system is connected with the two-channel switching system I (2) and provides test sample gas for the adsorption and desorption system; the desorption gas system (7) is also connected with the dual-channel switching system I (2) to provide a desorption gas source for the adsorption and desorption system (3);
the adsorbent discharge and analysis system (8) is connected with the dual-channel switching system I (2) through a parallel pipeline R, S, and the adsorbent online feeding system (9) is obliquely connected with a pipeline K, F of the adsorption and desorption system (3) at an interface through a parallel feeding pipeline Q, W; the purging and conveying gas source system (10) is communicated with a feeding pipeline Q, W of the adsorbent online feeding system (9).
2. The evaluation apparatus for adsorption/desorption of the polyvalent lower hydrocarbon according to claim 1, wherein: the multi-element low-carbon hydrocarbon simulation gas system (12) comprises V1-Vn single-component gas supply systems (18); each single-component gas supply system (18) comprises a gas supply device V, a pressure fine control valve (14), a flow fine control valve (15) and an automatic flow control valve (16) which are connected in sequence; each two groups of single-component gas supply systems (18) are connected in parallel, then are connected with the first-stage mixer (17), and then are connected in parallel;
the multi-element low-carbon hydrocarbon direct feeding system (13) comprises a multi-element low-carbon hydrocarbon mixed gas collecting tank (19), a pressure fine control valve (14), a flow fine control valve (15), an automatic flow control valve (16) and a to-be-detected gas direct interface (20) which is vertically connected between the multi-element low-carbon hydrocarbon mixed gas collecting tank (19) and the pressure fine control valve (14);
the multi-element low-carbon hydrocarbon simulated gas system (12) is connected with the multi-element low-carbon hydrocarbon direct feeding system (13) in parallel and then is connected with the double-channel switching system I (2) through the secondary mixer (21).
3. The evaluation apparatus for adsorption/desorption of the polyvalent lower hydrocarbon according to claim 2, wherein: the adsorption and desorption system (3) comprises an adsorption desorber I (24) and an adsorption desorber II (25) which are connected in parallel, the incoming direction of the adsorption desorber I (24) is connected to the discharging direction of an adsorption and desorption system feed valve I (22) arranged between the adsorption desorber I (24) and the two-channel switching system I (2) and is connected to a pipeline K, and the incoming direction of the adsorption desorber II (25) is connected to the discharging direction of an adsorption and desorption system feed valve II (23) arranged between the adsorption desorber II (25) and the two-channel switching system I (2) and is connected to a pipeline F.
4. The evaluation apparatus for adsorption/desorption of the polyvalent lower hydrocarbon according to claim 3, wherein: the adsorption desorber I (24) and the adsorption desorber II (25) respectively comprise a barrel-shaped heater (48), an adsorbent (49) positioned in the center of the barrel-shaped heater (48), adsorbent fixing and filtering devices (47) and a quick loading and unloading device (46), wherein the adsorbent fixing and filtering devices are respectively arranged at two ends of the barrel-shaped heater (48);
the barrel heater (48) comprises one or more of electric heating, water bath heating, oil bath heating and steam heating; the adsorbent (49) is one or a combination of more of activated carbon, a coke powder modified product, a high-performance adsorption carbon material and aerogel; the adsorbent fixing and filtering device (47) is one or a combination of asbestos, metal sinter, alloy net and glass wool.
5. The evaluation apparatus for adsorption/desorption of the polyvalent lower hydrocarbon according to claim 1, wherein: the desorption gas system (7) comprises a desorption gas source (11), a pressure fine control valve (14), a flow fine control valve (15) and an automatic flow control valve (16) which are connected in sequence;
the adsorbent discharging and analyzing system (8) comprises an adsorbent discharging valve I (26) arranged on a pipeline R and an adsorbent discharging valve II (27) arranged on a pipeline S; the pipelines R and S are connected in parallel and then are converged and connected with an adsorbent collecting tank (28) and then are connected with an adsorbent analyzer (29);
the adsorbent analyzer (29) is one or more combination of BET, XRD and FT-IR analyzers;
the desorption gas source (11) is one or a combination of more of nitrogen, air, carbon dioxide, helium and steam.
6. The evaluation apparatus for adsorption/desorption of the polyvalent lower hydrocarbon according to claim 1, 3 or 5, wherein: the blowing and conveying gas source system (10) is divided into two paths which are connected in parallel, wherein one path is connected with the material inlet end of an adsorbent discharge valve I (33) and an adsorbent discharge valve II (34) on a feeding pipeline Q, W; one path of the pipeline is connected with an adsorption and desorption system feed valve I (22), an adsorption and desorption system feed valve II (23), an adsorbent discharge valve I (26), an adsorbent discharge valve II (27), an adsorbent discharge valve I (33), an adsorbent discharge valve II (34) and a pipeline R, S, so that the online transportation of the adsorbent under pressure and the pneumatic blockage removal of each pipeline are realized.
7. The evaluation apparatus for adsorption/desorption of the polyvalent lower hydrocarbon according to claim 1, wherein: the chromatographic analysis system (5) comprises a pressure remote monitor (35), a filter (36), a system back-pressure valve (37), a total flow monitor (38) and a backflow prevention device (39) which are respectively connected to a pipeline Z and a pipeline J in sequence; the total flow monitor (38) and the backflow prevention device (39) of the pipeline J are connected with a chromatograph (42) through a quick-release reducing valve (40) and a micro-flow control valve (41);
the tail gas emission system (6) include tail gas trip valve (43), back-fire relief device (44) and air release ware (45) that link to each other in proper order, wherein tail gas trip valve (43) and chromatographic analysis system (5) prevent that refluence device (39) export links to each other.
8. The evaluation apparatus for adsorption/desorption of the polyvalent lower hydrocarbon according to claim 1, wherein: the online adsorbent feeding system (9) comprises an adsorbent temporary storage tank (30), a weighing instrument (31) and a powder cut-off valve (32) which are sequentially connected, and the outlet of the powder cut-off valve (32) is respectively connected with a parallel feeding pipeline Q, W.
9. The method for evaluating adsorption and desorption of a plurality of lower hydrocarbons based on the evaluation device according to claim 1, comprising the steps of:
step one, an adsorbent loading and system cleaning process:
1.1, placing adsorbent fixing and filtering devices (47) at the upper and lower ends of an adsorption desorber I (24) and an adsorption desorber II (25), loading an adsorbent (49) in an adsorbent temporary storage tank (30), opening a purging and conveying gas source system (10), introducing conveying gas to an adsorbent online charging system (9), pneumatically conveying the adsorbent (49) into an adsorption and desorption system (3) through the purging and conveying gas source system (10), and recording the loading amount of the adsorbent after the adsorbent is completely charged;
1.2, setting the pressure, flow and replacement time of a desorption gas system (7), and replacing the adsorption desorption system (3) with a purging desorption gas source (11) and simultaneously checking the pipeline airtightness of the device;
step two, switching the sample gas:
the control gas supply system (1) switches under the three states of independent gas supply of the multielement low carbon hydrocarbon simulation gas system (12), independent gas supply of the multielement low carbon hydrocarbon direct feeding system (13) and mixed gas supply of the two systems, so that gas supply of different samples is realized:
1) the multi-element low-carbon hydrocarbon simulated gas system (12) independently supplies gas: connecting V1-Vn single-component gas supply systems (18) with different gas components into a multi-component low-carbon hydrocarbon simulation gas system (12), and setting the opening degrees of a pressure fine control valve (14), a flow fine control valve (15) and an automatic flow control valve (16) of each group of single-component gas supply systems (18) until the values of the automatic flow control valve (16) and a total flow monitor (38) of the single-component gas supply systems (18) meet the test requirements;
2) the multi-element low-carbon hydrocarbon direct feeding system (13) independently supplies gas: collecting a multi-element low-carbon hydrocarbon mixed gas sample by using a multi-element low-carbon hydrocarbon mixed gas collecting tank (19) or directly connecting multi-element low-carbon hydrocarbon into a direct interface (20) of gas to be detected, setting the opening degrees of a pressure fine control valve (14), a flow fine control valve (15) and an automatic flow control valve (16) of a multi-element low-carbon hydrocarbon direct feeding system (13), and enabling the numerical value of the automatic flow control valve (16) and the numerical value of a total flow monitor (38) to meet the test requirements;
3) two systems mix the air supply: the multi-element low-carbon hydrocarbon mixed gas collection tank (19) and the single-component gas supply system (18) work simultaneously, are mixed in a secondary mixer (21), and the opening degrees of a pressure fine control valve (14), a flow fine control valve (15) and an automatic flow control valve (16) of each system are set until the numerical value of the automatic flow control valve (16) and the numerical value of a total flow monitor (38) meet the test requirements;
step three, an adsorption evaluation process:
3.1, operating a dual-channel switching system I (2) to enable the gas to be detected to enter an adsorption desorber I (24), and enabling the gas after adsorption to enter a chromatograph (42) from a pipeline J through a dual-channel switching system II (4) for analysis;
3.2, adjusting the numerical value of a system back-pressure valve (37) on the pipeline J to be a process set value;
3.3, according to the test requirements, controlling the working state of the gas supply system (1) according to the step two, and starting the adsorption process;
3.4, connecting a chromatograph (42) to a system through a quick-release reducing valve (40), and allowing part of sample gas to enter the chromatograph (42) for analyzing the adsorption effect after the sample gas is adjusted by a micro-flow control valve (41) to meet the requirements of the instrument;
3.5, a double-channel adsorption process:
when the removal rate gamma of the chromatograph (42) analyzed in the step 3.4 is lower than 10-70%, operating the dual-channel switching system I (2) to enable the gas to be detected to enter the adsorption desorber II (25), enabling the gas after adsorption to enter the chromatograph (42) from a pipeline J through the dual-channel switching system II (4) for analysis, then repeating the step 3.2-3.4, and stopping an adsorption test or performing a long-period adsorption test of online feeding by utilizing an adsorbent online feeding system (9) to online add an adsorbent (49) until the removal rate gamma of the chromatograph (42) analyzed is lower than 10-70%;
step four, desorption and analysis process:
with the two-channel switching system I (2) and the two-channel switching system II (4), the desorption process can be switched between A, B, C three states:
a, simultaneous desorption of the adsorption desorber I (24) and the adsorption desorber II (25)
a1) Operating the state of the two-channel switching system I (2) and the state of the two-channel switching system II (4) to enable desorption gas to enter an adsorption desorber I (24) and an adsorption desorber II (25) which are connected in parallel;
a2) setting the purging replacement pressure P of a desorption gas system (7) to be 0.0-5.0 MPa, and simultaneously enabling the numerical value of an automatic flow control valve (16) and the numerical value of a total flow monitor (38) to meet the test requirement;
a3) opening the barrel-shaped heater (48) to enable the barrel-shaped heater (48) to reach a set temperature T of 50-500 ℃, and performing heating adsorbent regeneration;
a4) stopping the desorption gas system (7), closing the barrel-shaped heater (48), opening an adsorption and desorption system feed valve I (22), an adsorption and desorption system feed valve II (23), an adsorbent discharge valve I (26) and an adsorbent discharge valve II (27) when the system pressure is reduced to normal pressure, and enabling the adsorbent to enter an adsorbent collecting tank (28);
a5) performing BET, XRD and FT-IR analysis on the adsorbent (49) in the adsorbent collecting tank (28) by using an adsorbent analyzer (29) to calculate the adsorbent adsorption capacity U;
b, adsorption by an adsorption desorber I (24) and desorption by an adsorption desorber II (25) are carried out simultaneously:
b1) operating the state of the two-channel switching system I (2) to enable the gas to be detected of the gas supply system (1) to enter an adsorption desorber I (24) for adsorption test, simultaneously operating the two-channel switching system II (4) to enable the gas after adsorption to enter a chromatograph (42) for analysis through a pipeline J, and then performing the adsorption evaluation process of the steps 3.2-3.3 on the adsorption desorber I (24);
b2) meanwhile, operating the state of a dual-channel switching system I (2) to enable desorbed gas of a desorbed gas system (7) to enter an adsorption desorber II (25), operating a dual-channel switching system II (4) to enable the adsorption desorber II (25) to be connected into a pipeline Z and then to be connected into a tail gas discharge system (6), setting a pressure fine control valve (14) of the desorbed gas system (7) to a purging replacement pressure P of 0.0-5.0 MPa, adjusting a flow fine control valve (15) and an automatic flow control valve (16) of the desorbed gas system (7) until the numerical value of a flow automatic flow control valve (16) and the numerical value of a total flow monitor (38) reach test requirements, opening a barrel heater (48) to enable the desorption temperature to reach a set temperature T of 50-500 ℃, enabling a purging desorption gas source (11) to enter the adsorption desorber II (25) to regenerate an adsorbent (49), and stopping the desorbed gas system (7), closing the barrel-shaped heater (48), opening a feeding valve II (23) of the adsorption and desorption system and a discharge valve II (27) of the adsorbent when the pressure P of the system is reduced to the normal pressure, allowing the adsorbent to enter an adsorbent collecting tank (28), and performing BET, XRD and FT-IR analysis on the adsorbent in the adsorbent collecting tank (28) by using an adsorbent analyzer (29) to calculate the adsorption capacity U of the adsorbent;
c, desorption of an adsorption desorber I (24) and adsorption of an adsorption desorber II (25) are carried out simultaneously:
c1) operating the state of the two-channel switching system I (2) to enable the gas to be detected of the gas supply system (1) to enter an adsorption desorber II (25) for adsorption test, simultaneously operating the two-channel switching system II (4) to enable the gas after adsorption to enter a chromatograph (42) for analysis through a pipeline J, and then performing the adsorption evaluation process of the steps 3.2-3.3 on the adsorption desorber II (25);
c2) meanwhile, the state of a dual-channel switching system I (2) is operated, so that desorbed gas of a desorbed gas system (7) enters an adsorption desorber I (24), a dual-channel switching system II (4) is operated, so that the adsorption desorber I (24) is connected into a pipeline Z and then connected into a tail gas discharge system (6), a pressure fine control valve (14) of the desorbed gas system (7) is set to a purging replacement pressure P which is 0.0-5.0 MPa, a flow fine control valve (15) and an automatic flow control valve (16) of the desorbed gas system (7) are adjusted until the numerical value of the automatic flow control valve (16) and the numerical value of a total flow monitor (38) reach test requirements, a barrel heater (48) is opened to enable the desorption temperature to reach a set temperature T which is 50-500 ℃, a purging desorption gas source (11) enters the adsorption desorber I (24) to regenerate an adsorbent (49), and the desorbed gas system (7) is stopped, closing the barrel-shaped heater (48), opening a feeding valve I (22) of the adsorption and desorption system and a discharge valve I (26) of the adsorbent when the pressure P of the system is reduced to the normal pressure, allowing the adsorbent to enter an adsorbent collecting tank (28), and performing BET, XRD and FT-IR analysis on the adsorbent in the adsorbent collecting tank (28) by using an adsorbent analyzer (29) to calculate the adsorption capacity U of the adsorbent;
step five: and (3) removing system blockage:
when one or more of the combination of the adsorption and desorption system feed valve I (22), the adsorption and desorption system feed valve II (23), the adsorbent discharge valve I (26), the adsorbent discharge valve II (27), the adsorbent discharge valve I (33), the adsorbent discharge valve II (34) and the pipeline R, S is blocked, the purging and conveying gas source system (10) is opened to remove the blockage.
10. The method for evaluating the adsorption and desorption of the multi-element low carbon hydrocarbon according to claim 9, wherein the calculation method of the removal rate γ and the adsorption capacity U of the adsorbent comprises the following steps:
(1) the calculation method of the removal rate gamma comprises the following steps:
γ＝(Co-Ct)/C0×100
in the formula, Ct-component concentration at a certain moment, vol%;
C0-initial state component concentration, vol%;
gamma-removal rate,%;
(2) the method for calculating the adsorption capacity U of the adsorbent comprises the following steps:
in the formula, C0-initial concentration of a certain component, mol%;
Ct-the outlet concentration of a certain component at time t,% mol;
m-sorbent loading, g;
t-adsorption time, min;
fv-adsorbed gas flow, L/min;
Mf-the relative molecular mass of a certain component, g/mol;
u-adsorbent adsorption capacity, g/100g adsorbent.
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Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1237472A (en) * | 1999-04-02 | 1999-12-08 | 成都华西化工研究所 | Method for recovering sulfur dioxide from gas and its equipment |
| CN1242252A (en) * | 1999-06-18 | 2000-01-26 | 化学工业部西南化工研究设计院 | Removing and recovering nitrogen oxide(s) by adsorption separation method from mixed gas contg. nitrogen oxide(s) |
| US20040163383A1 (en) * | 2003-02-21 | 2004-08-26 | Khair Magdi K. | Control method for dual path NOx adsorber system |
| JP2009247962A (en) * | 2008-04-03 | 2009-10-29 | Syst Enji Service Kk | Method of cleaning large quantity of exhaust gas containing thin volatile hydrocarbon |
| US20090293717A1 (en) * | 2008-06-02 | 2009-12-03 | Jun Izumi | Method and apparatus for producing and storing ozone using adsorbent |
| CN103894039A (en) * | 2014-02-27 | 2014-07-02 | 广东电网公司电力科学研究院 | Adsorbent jet apparatus with online weighing function for flue pollution reducing of coal-fired power plant |
| CN205067265U (en) * | 2015-09-28 | 2016-03-02 | 南京天膜科技股份有限公司 | Gaseous dynamic adsorption desorption testing arrangement |
| CN105513661A (en) * | 2016-01-15 | 2016-04-20 | 中国科学技术大学 | Cleaning waste gas pressure swing adsorption purification and recycling method and device for fusion reactor hot room |
| CN105521692A (en) * | 2016-01-20 | 2016-04-27 | 义乌市中科院兰州化物所功能材料中心 | Industrial emission volatile organic compounds (VOCs) tail gas on-site detecting evaluation device and method |
| CN107930340A (en) * | 2017-11-29 | 2018-04-20 | 西南化工研究设计院有限公司 | Test the temperature swing adsorption system and method for volatile organic matter adsorbance and desorption quantity |
| CN108279182A (en) * | 2017-01-06 | 2018-07-13 | 南京林业大学 | A kind of device for estimating gas absorbent |
| CN109613143A (en) * | 2019-01-25 | 2019-04-12 | 山西普丽环境工程股份有限公司 | For the Removal of catalyst of dioxin or the Performance Appraisal System of adsorbent and method |
-
2019
- 2019-12-17 CN CN201911299243.9A patent/CN110940752B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1237472A (en) * | 1999-04-02 | 1999-12-08 | 成都华西化工研究所 | Method for recovering sulfur dioxide from gas and its equipment |
| CN1242252A (en) * | 1999-06-18 | 2000-01-26 | 化学工业部西南化工研究设计院 | Removing and recovering nitrogen oxide(s) by adsorption separation method from mixed gas contg. nitrogen oxide(s) |
| US20040163383A1 (en) * | 2003-02-21 | 2004-08-26 | Khair Magdi K. | Control method for dual path NOx adsorber system |
| JP2009247962A (en) * | 2008-04-03 | 2009-10-29 | Syst Enji Service Kk | Method of cleaning large quantity of exhaust gas containing thin volatile hydrocarbon |
| US20090293717A1 (en) * | 2008-06-02 | 2009-12-03 | Jun Izumi | Method and apparatus for producing and storing ozone using adsorbent |
| CN103894039A (en) * | 2014-02-27 | 2014-07-02 | 广东电网公司电力科学研究院 | Adsorbent jet apparatus with online weighing function for flue pollution reducing of coal-fired power plant |
| CN205067265U (en) * | 2015-09-28 | 2016-03-02 | 南京天膜科技股份有限公司 | Gaseous dynamic adsorption desorption testing arrangement |
| CN105513661A (en) * | 2016-01-15 | 2016-04-20 | 中国科学技术大学 | Cleaning waste gas pressure swing adsorption purification and recycling method and device for fusion reactor hot room |
| CN105521692A (en) * | 2016-01-20 | 2016-04-27 | 义乌市中科院兰州化物所功能材料中心 | Industrial emission volatile organic compounds (VOCs) tail gas on-site detecting evaluation device and method |
| CN108279182A (en) * | 2017-01-06 | 2018-07-13 | 南京林业大学 | A kind of device for estimating gas absorbent |
| CN107930340A (en) * | 2017-11-29 | 2018-04-20 | 西南化工研究设计院有限公司 | Test the temperature swing adsorption system and method for volatile organic matter adsorbance and desorption quantity |
| CN109613143A (en) * | 2019-01-25 | 2019-04-12 | 山西普丽环境工程股份有限公司 | For the Removal of catalyst of dioxin or the Performance Appraisal System of adsorbent and method |
Non-Patent Citations (1)
| Title |
|---|
| 刘思乐等: "CaO/γ-Al2O3吸附剂吸附CO2的性能研究", 《化工新型材料》 * |
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