CN104181275B - MATERIALS ' DYNAMIC adsorption coefficient measurement mechanism under a kind of vacuum state - Google Patents

MATERIALS ' DYNAMIC adsorption coefficient measurement mechanism under a kind of vacuum state Download PDF

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Publication number
CN104181275B
CN104181275B CN201310191200.5A CN201310191200A CN104181275B CN 104181275 B CN104181275 B CN 104181275B CN 201310191200 A CN201310191200 A CN 201310191200A CN 104181275 B CN104181275 B CN 104181275B
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gas
adsorption
tcd detector
bottle
enters
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CN104181275A (en
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魏建军
张振中
欧阳钦
江锋
张冰
刘熠
管玉峰
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Jiangsu Nuclear Power Corp
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Jiangsu Nuclear Power Corp
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Abstract

The invention belongs to material physical and chemical performance field of measuring technique, relate to MATERIALS ' DYNAMIC adsorption coefficient measurement mechanism under a kind of vacuum state. The present invention includes carrier gas bottle, gas bottle upon adsorption, TCD detector, humidification temperature regulating device, sorbing material bed, dehydrating unit, data processing equipment and vavuum pump: the upon adsorption mixed gases of the carrier gas in carrier gas bottle in TCD detector and gas bottle upon adsorption; Part mist again mixes with remaining dry mixed gas after humidification temperature regulating device; Mixed gas enters dehydrating unit through sorbing material bed again; Gas after dehumidifying enters TCD detector; TCD detector exports measurement data to data processing equipment, and the gas after detection enters vavuum pump. The invention solves prior art and be difficult to directly measure under negative pressure state active carbon for the technical problem of inert gas Dynamic Adsorption coefficient, and by the means such as vacuum conditions and temperature and humidity regulation, realize the measurement of sorbing material Dynamic Adsorption coefficient in varying environment condition.

Description

MATERIALS ' DYNAMIC adsorption coefficient measurement mechanism under a kind of vacuum state
Technical field
The invention belongs to material physical and chemical performance field of measuring technique, be specifically related to material under a kind of vacuum stateDynamic Adsorption coefficient measuring device.
Background technology
Using the radioactivity inert gases such as charcoal absorption Ar, Kr, Xe and Rn is a kind of effective sideMethod, particularly in nuclear power station, is used and active-carbon bed radioactivity inert gas is carried out to Adsorption And Retention, canTo reach its radioactivity of effective removal, protection staff is healthy exempts from contaminated object with environment.
Running status active-carbon bed in nuclear power station mostly is negative pressure state, so as not to the radioactivity in system due toMalleation reason is leaked and is entered external environment, causes the radioactive pollution of environment. At present, measuring active carbon inhalesThe device of attached performance is divided into two large classes, and a class is Static Adsorption measuring instrument, can obtain the absorption of active carbonThe parameters such as thermoisopleth; Another kind of is Dynamic Adsorption measuring instrument, mostly is gas-chromatography, mass spectrum etc. This two classInstrument all can not directly be measured under negative pressure state active carbon for the Dynamic Adsorption coefficient of inert gas.
And by measure the Dynamic Adsorption system of the sorbing materials such as active carbon for gaseous material under vacuum stateNumber, can obtain the actual performance parameter that material moves in Load System, for the design of Load System,Build and operation has great importance and value, can provide heavy for the opening of new material and optimizationWanting experimental data, is the technical problem that this area is needed solution badly.
Summary of the invention
The technical issues that need to address of the present invention are: the device of prior art is difficult to directly measure negative pressure stateLower active carbon is for the Dynamic Adsorption coefficient of inert gas.
Technical scheme of the present invention is as described below:
MATERIALS ' DYNAMIC adsorption coefficient measurement mechanism under a kind of vacuum state, comprises carrier gas bottle, gas upon adsorptionBottle, TCD detector, humidification temperature regulating device, sorbing material bed, dehydrating unit, data processing equipment andVavuum pump: the carrier gas in carrier gas bottle is mixed mutually with the gas upon adsorption in gas bottle upon adsorption through TCD detectorClose; Part mist again mixes with remaining dry mixed gas after humidification temperature regulating device; AgainInferior mixed gas enters dehydrating unit through sorbing material bed; Gas after dehumidifying enters TCD and detectsDevice; TCD detector exports measurement data to data processing equipment, and the gas after detection enters vavuum pump.
As preferred version,
Carrier gas bottle enters TCD detector by 1# pressure maintaining valve and 1# mass flowmenter; TCD detectorThe carrier gas of one outlet is by the mixed gases upon adsorption in six-way valve and gas bottle upon adsorption, through 1# tri-Logical valve, a part enters humidification temperature regulating device by 2# mass flowmenter, and another part is by 3# mass flowAfter amount meter, again mix at 2# triple valve place with the mist through humidification temperature control; Mixed gas againSuccessively process is placed in 1# spatial capacity bottle, sorbing material bed and the 2# spatial capacity bottle of 2# constant temperature heating device,Finally enter dehydrating unit; Gas after dehumidifying enters TCD detector; Described TCD detector obtainsMeasurement data export data processing equipment to; Mist after TCD detector detects is from the second outletDischarge, after elder generation, through Pressure gauge, fine adjustment valve, finally enter vavuum pump.
As further preferred version,
1# spatial capacity bottle and 2# spatial capacity bottle are respectively equipped with temperature measuring equipment and humidity measuring instrument: temperatureMeasurement mechanism can adopt RTD, and humidity measuring instrument can adopt dew point hygrometer; Described gas upon adsorptionWhat bottle was exported can be pulse gas upon adsorption; Described humidification temperature regulating device can comprise deionized water is housedBe filled with water volumetric flask and 1# constant temperature heating device, the volumetric flask that is filled with water is placed in 1# constant temperature heating device.
Beneficial effect of the present invention is:
MATERIALS ' DYNAMIC adsorption coefficient measurement mechanism under vacuum state of the present invention, can directly measure negative pressure shapeUnder state, active carbon is for the Dynamic Adsorption coefficient of inert gas; And by vacuum conditions and temperature and humidity regulation etc.Means, have realized the measurement of sorbing material Dynamic Adsorption coefficient in varying environment condition.
Brief description of the drawings
Fig. 1 is MATERIALS ' DYNAMIC adsorption coefficient measurement mechanism structural representation under vacuum state of the present invention.
In figure, wherein, 1-carrier gas bottle; 2-gas bottle upon adsorption; 3-1# pressure maintaining valve; 4-1# mass flowmenter;5-six-way valve; 6-1# triple valve; 7-2# mass flowmenter; The 8-volumetric flask that is filled with water; 9-1# constant temperature heating device;10-3# mass flowmenter; 11-2# triple valve; 12-1# RTD; 13-1# humidity measuring instrument; 14-1Spatial capacity bottle; 15-TCD detector; 16-2# RTD; 17-sorbing material bed; 18-dehydrating unit; 19-3RTD; 20-2# humidity measuring instrument; 21-2# spatial capacity bottle; 22-2# constant temperature heating device; 23-dataTreatment facility; 24-Pressure gauge; 25-fine adjustment valve; 26-vavuum pump.
Detailed description of the invention
Below in conjunction with drawings and Examples, MATERIALS ' DYNAMIC adsorption coefficient under vacuum state of the present invention is measured to dressPut and be elaborated.
As shown in Figure 1, MATERIALS ' DYNAMIC adsorption coefficient measurement mechanism under vacuum state of the present invention, comprises and carryingGas cylinder 1, gas bottle upon adsorption 2, TCD detector 15, humidification temperature regulating device, sorbing material bed 17,Dehydrating unit 18, data processing equipment 23 and vavuum pump 26.
Wherein, the treating in TCD detector 15 and gas bottle 2 upon adsorption of the carrier gas in carrier gas bottle 1 inhaledAttached mixed gases; A part mist after humidification temperature regulating device with remaining dry mixed gas againInferior mixing; Mixed gas enters dehydrating unit 18 through sorbing material bed 17 again; Gas after dehumidifyingBody enters TCD detector 15; TCD detector 15 exports measurement data to data processing equipment 23,Gas after detection enters vavuum pump 26.
In the present embodiment, carrier gas bottle 1 enters TCD inspection by 1# pressure maintaining valve 3 and 1# mass flowmenter 4Survey device 15, TCD detector 15 obtains measurement data A; The carrier gas of TCD detector 15 first outletsBy the mixed gases upon adsorption in six-way valve 5 and gas bottle 2 upon adsorption, through 1# triple valve 6,A part enters humidification temperature regulating device by 2# mass flowmenter 7, and another part is by 3# mass flowmenterAfter 10, again mix this tune that is designed at 2# triple valve 11 places with the mist through humidification temperature controlJoint relative humidity: the mode that uses dry gas and steam to mix when relative humidity is lower, relatively wetSpending when higher uses dry gas directly to pass into the mode of humidification in water; Again mixed gas first after warpCross the 1# spatial capacity bottle 14, sorbing material bed 17 and the 2# spatial capacity that are placed in 2# constant temperature heating device 22Bottle 21, finally enters dehydrating unit; Gas after dehumidifying enters TCD detector 15 and obtains measurement dataB; The measurement data A that described TCD detector 15 obtains and measurement data B export data processing to and establishStandby; Mist after TCD detector 15 detects is discharged from the second outlet, after elder generation through Pressure gauge 24,Fine adjustment valve 25, finally enters vavuum pump 26.
In the present embodiment, 1# spatial capacity bottle 14 and 2# spatial capacity bottle 21 be respectively equipped with temperature measuring equipment andHumidity measuring instrument: temperature measuring equipment can adopt RTD; Humidity measuring instrument can adopt dew pointInstrument.
In the present embodiment, what described gas bottle 2 upon adsorption was exported is pulse gas upon adsorption.
In the present embodiment, described humidification temperature regulating device comprises be filled with water volumetric flask 8 and 1# that deionized water is housedConstant temperature heating device 9, the volumetric flask 8 that is filled with water is placed in 1# constant temperature heating device 9.
The using method of apparatus of the present invention is as described below:
Starting drive, according to time-independent measurement data A and time dependent measurement data B,Determine the concentration ratio of gas upon adsorption in mist and this concentration ratio variation rule with Measuring TimeRule; Under the interior state without sorbing material of sorbing material bed 17, record the mixing that TCD detector 15 obtainsGas time to peak t1, in sorbing material bed 17, have under the state of sorbing material and record TCD detectorThe 15 mist time to peak t that obtain2, the holdup time of gas upon adsorption in sorbing materialΔt=t2-t1; The quality of sorbing material is m; The volume flow of the mist by sorbing material is f;Data processing equipment can obtain Dynamic Adsorption coefficient k by following formula, k=Δ t*f/m.
Use measurement device sorbing material active carbon of the present invention to treat the Dynamic Adsorption system of adsorbed gas KrNumber: record the mixing that TCD detector 15 obtains under the interior state without sorbing material of sorbing material bed 17Gas time to peak t1=175s; In sorbing material bed 17, have and under the state of sorbing material, record TCD inspectionSurvey the mist time to peak that device 15 obtains, twice Measuring Time is respectively 265s and 270s, t2GetMean value is 267.5s; Sorbing material quality of activated carbon m is 0.8162g; By the gaseous mixture of sorbing materialThe volume flow f of body is 18.2cm3/ min, test operating mode is 306.15K and 90kPa; Dynamic AdsorptionCoefficient k = Δt * f / m = 18.2 * ( 267.5 - 175 ) 60 * 0.8162 = 34.38 cm 3 / g . On this basis, can also adopt existingTechnology is carried out temperature, pressure correction to Dynamic Adsorption coefficient, and revised Dynamic Adsorption coefficient is27.61cm3/g。

Claims (5)

1. a MATERIALS ' DYNAMIC adsorption coefficient measurement mechanism under vacuum state, comprises carrier gas bottle (1), waits to inhaleAttached gas bottle (2), TCD detector (15), humidification temperature regulating device, sorbing material bed (17), dehumidifyingDevice (18), data processing equipment (23) and vavuum pump (26), is characterized in that: carrier gas bottle (1)In the upon adsorption mixed gases of carrier gas in TCD detector (15) and gas bottle upon adsorption (2);Part mist again mixes with remaining dry mixed gas after humidification temperature regulating device; Again mixedGas after closing enters dehydrating unit (18) through sorbing material bed (17); Gas after dehumidifying enters TCDDetector (15); TCD detector (15) exports measurement data to data processing equipment (23), inspectionGas after survey enters vavuum pump (26);
Carrier gas bottle (1) enters TCD detector by 1# pressure maintaining valve (3) and 1# mass flowmenter (4)(15); The carrier gas of TCD detector (15) first outlets is by six-way valve (5) and gas bottle upon adsorption(2) mixed gases upon adsorption in, through 1# triple valve (6), a part is by 2# mass flowMeter (7) enters humidification temperature regulating device, and another part is by after 3# mass flowmenter (10) and through humidificationThe mist of temperature control is located again to mix at 2# triple valve (11); Successively process of mixed gas againBe placed in 1# spatial capacity bottle (14), sorbing material bed (17) and the 2# of 2# constant temperature heating device (22)Spatial capacity bottle (21), finally enters dehydrating unit; Gas after dehumidifying enters TCD detector (15);The measurement data that described TCD detector (15) obtains exports data processing equipment to; TCD detector(15) detect after mist discharges from the second outlet, elder generation after through Pressure gauge (24), fine adjustment valve(25), finally enter vavuum pump (26).
2. MATERIALS ' DYNAMIC adsorption coefficient measurement mechanism under vacuum state according to claim 1, its spyLevy and be: 1# spatial capacity bottle (14) and 2# spatial capacity bottle (21) are respectively equipped with temperature measuring equipment and wetDegree measurement mechanism.
3. MATERIALS ' DYNAMIC adsorption coefficient measurement mechanism under vacuum state according to claim 2, its spyLevy and be: temperature measuring equipment adopts RTD, humidity measuring instrument adopts dew point hygrometer.
4. MATERIALS ' DYNAMIC adsorption coefficient measurement mechanism under vacuum state according to claim 1, its spyLevy and be: what described gas bottle upon adsorption (2) was exported is pulse gas upon adsorption.
5. MATERIALS ' DYNAMIC adsorption coefficient measurement mechanism under vacuum state according to claim 1, its spyLevy and be: described humidification temperature regulating device comprises the volumetric flask that is filled with water (8) and 1# constant temperature that deionized water is housedHeater (9), the volumetric flask that is filled with water (8) is placed in 1# constant temperature heating device (9).
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CN105136922A (en) * 2015-08-16 2015-12-09 常州大学 Adsorbent performance dynamic detection device
CN107132303A (en) * 2016-02-26 2017-09-05 中国辐射防护研究院 Use Dynamic Adsorption coefficient method of the gas chromatographic measurement activated carbon to inert gas
CN108279182B (en) * 2017-01-06 2020-06-16 南京林业大学 Gas adsorbent evaluation device

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CN202562896U (en) * 2012-05-11 2012-11-28 四川亚连科技有限责任公司 Dynamic adsorption testing device
CN102928323A (en) * 2012-10-18 2013-02-13 天津大学 Air purification filtering material testing experimental system
CN203275231U (en) * 2013-05-21 2013-11-06 江苏核电有限公司 Device for measuring dynamic adsorption coefficient of material in vacuum

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JP2004108967A (en) * 2002-09-19 2004-04-08 Dainippon Printing Co Ltd System and method for measuring volatilizing amount of volatile organic compound

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CN202562896U (en) * 2012-05-11 2012-11-28 四川亚连科技有限责任公司 Dynamic adsorption testing device
CN102928323A (en) * 2012-10-18 2013-02-13 天津大学 Air purification filtering material testing experimental system
CN203275231U (en) * 2013-05-21 2013-11-06 江苏核电有限公司 Device for measuring dynamic adsorption coefficient of material in vacuum

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