CN101354333A - Method and apparatus for evaluating hole structural property using imbibition gas-discharging method - Google Patents
Method and apparatus for evaluating hole structural property using imbibition gas-discharging method Download PDFInfo
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- CN101354333A CN101354333A CNA2008100125980A CN200810012598A CN101354333A CN 101354333 A CN101354333 A CN 101354333A CN A2008100125980 A CNA2008100125980 A CN A2008100125980A CN 200810012598 A CN200810012598 A CN 200810012598A CN 101354333 A CN101354333 A CN 101354333A
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Abstract
The invention provides a method for evaluating the performance of pore structures of amesoporous and microporous materials by imbibing and purging and a device which conducts the evaluation by the method thereof. A sample which adsorbs a scheduled gas in equilibrium is immersed into a scheduled liquid, and then the rate of change of the imbibing and purging volume with time and the equilibrium volume of imbibing and purging are measured; pore structures and information of surface property of the sample are judged according to the rate of imbibing and purging and significant differences represented by the equilibrium volume of imbibing and purging according to the type of imbibition and purge; structural parameters of the sample pore are calculated according to a rate curve of imbibing and purging and a dynamical equation of imbibing and purging of the material; the obtained pore structure information is used for evaluating the performance of the pore structure of the sample. The method of the invention improves the accuracy of measurement and is especially applicable to microporous materials. In addition, the invention has simple apparatus and easy operation, and can evaluate pore structures of amesoporous and microporous materials accurately and quickly.
Description
Technical field
The invention belongs to chemical material field, relate to a kind of method and device of evaluating material hole structural property, particularly a kind of utilize imbibition purging method estimate in, the method and the device of poromerics hole structural property.
Background technology
Porosint has been widely used in fields such as food, chemical industry, medicine, electronics, space flight and aviation owing to have good absorption, permeance property.The absorption of porosint, permeance property and its pore texture are closely related, therefore, can estimate its performance by measuring material parameter of pore structure (as average pore size, pore diameter distribution etc.).
At present, the most frequently used measurement and evaluation method have molecular probe method, gas adsorption method, low-angle X scattering collimation method and imbibition KINETIC METHOD etc., and these methods cut both ways.
The molecular probe method is that a kind of molecule of different size that utilizes adsorbs on porosint, comes the method for calculated hole diameters distribution according to the difference of adsorbance.This method is applicable to poromerics, and measuring process is very loaded down with trivial details, is subjected to the restriction of molecular species, can only provide limited pore diameter distribution information.
Gas adsorption method is a kind of according to the adsorption isothermal of single-component gas on porosint, according to the method for certain method calculated hole diameters distribution.The method that calculated hole diameters distributes has multiple, as early stage BJH, MP, HK with based on the whole bag of tricks of Dubinin filling theory, and recent years around the method for GAI expansion, the scope of application of these methods has tangible difference.BJH method and MP model have been ignored micropore internal potential energy synergistic effect, only are fit to describe the mesopore pore diameter distribution; The H-K model has been considered microcosmic potential energy synergistic effect, can well describe micropore size to a certain extent and distribute, but suppose that the interaction between adsorption molecule and the adsorbent hole wall molecule all is the identical limitation that has on each aspect of space; Considered microcosmic potential energy synergistic effect based on the whole bag of tricks of Dubinin filling theory, can well describe micropore size to a certain extent distributes, because of under low pressure, DR equation and Henry law are inconsistent, therefore lack enough theoretical foundations, can not correctly reflect the absorption under the low pressure, and these class methods to be subjected to the restriction of pore size distribution function form; The DFT that launches around the GAI equation and the method for GCMC simulation have overcome the shortcoming of this respect, also are used to determine the pore diameter distribution of microporous medium, and these two kinds of methods are considered to effective method, but its validity also needs more experimental result to prove.Gas adsorption method exists also that required instrument costs an arm and a leg, test condition harshness, long problem of test duration except that above-mentioned limitation.
The low-angle x-ray method is got on the sample parallel monoergic X-ray beam or neutron beam and scattering under low-angle, draws the function figure line of scattering strength I as scattering wave vector q.Scattering function I (q) depends on the inner structure of sample, and every kind has any porous body that distributes of equidimension spherical void work and all can produce 1 characteristic function.Suppose a kind of so simple model, just can draw the distribution of pore radius or pore-size.But because the restriction of aspect factors such as X ray intensity, detecting devices, the application of low-angle x-ray method has bigger limitation.
The imbibition KINETIC METHOD is a kind of capillary nature imbibition phenomenon of liquid in porosint of utilizing, and in conjunction with the equation of motion of liquid in pore, measures the method for material parameter of pore structure and its performance of evaluation.Measuring method comprises following two kinds, a kind of measurement liquid absorption is speed (Trong Dang-Vu over time, et al.Characterization of porous materials bycapillary rise method.Physicochemical Problems of Mineral Processing, 2005,39:47-65.); The another kind of suction range speed (E.P.Ka-logianni over time that measures, et al.A dynamic wicking technique for de-termining the effective pore radius of pregelatinized starch sheets.Colloids and Surfaces B:Biointerfaces, 2004,35:159-167).Because used equipment is simple, the gained conclusion is reliable, be widely used in the measurement of material hole gap structures such as concrete, soil and the evaluation of performance, be considered to promising method.The imbibition KINETIC METHOD adopts the equation of motion of liquid in pore, does not consider the variation of the liquid flow situation in the micropore, so be not suitable for poromerics, in being only applicable to, large pore material, when micropore size reduced, liquid absorption reduced, and the precision of measurement also descends.
Summary of the invention
The purpose of this invention is to provide and a kind ofly become big characteristic, utilize the natural imbibition purging phenomenon of material, in estimating simply, accurately and rapidly, the method and the device of poromerics pore texture performance according to gas density in the nanometer restricted clearance.
The principle of institute of the present invention foundation is, with equilibrium adsorption the sample of predetermined gas when being immersed in the predetermined liquid, liquid enters the sample hole and replaces wherein gas under capillary force or class capillary force, i.e. the imbibition purging.The dynamics of imbibition purging and thermodynamic behavior, promptly rule and final balance imbibition purging amount have reflected pore texture and the surface nature feature that institute measures and monitor the growth of standing timber and expects to imbibition purging amount over time.Because gas density is big under more macroscopical situation in the nanometer restricted clearance, the gas volume that displaces is much larger than the liquid volume that enters, therefore measure imbibition purging volume over time speed and balance imbibition purging volume method and traditional imbibition mensuration mutually specific energy reflect the hole and the surface texture featur of measuring and monitoring the growth of standing timber and expecting more accurately.Under specific or different temperature and pressure conditions, according to single or multiple different predetermined gas and predetermined liquid porosint is carried out the experiment of imbibition purging, the pore texture and the surface nature information of material of measuring and monitoring the growth of standing timber that can obtain to enrich, and further obtain the parameter of pore structure of material on this basis.
Technical scheme of the present invention is: the method for utilizing imbibition purging method mensuration and evaluating material hole structural property, at first the testing sample with the prescribed particle size of accurate weighing places sample cell, under design temperature, feed predetermined gas in the sample cell and reach adsorption equilibrium, switch then and feed the predetermined liquid identical with design temperature, the imbibition purging of beginning sample, the volume that feeds liquid should be greater than testing sample volume and imbibition purging volume sum, and testing sample still can be by the submergence of liquid institute after guaranteeing to reach imbibition purging balance; Utilize the constant voltage fluid-discharge therapy to measure imbibition purging volume speed and balance imbibition purging volume over time, or under the constant volume condition in the measuring samples pond pressure of gas change and determine imbibition purging volume; Obtain sample imbibition purging rate curve under the different condition by change imbibition and purging kind, imbibition purging temperature, as the basic data of qualitative and quantitative analysis sample well gap structure and surface nature, judgement sample pore texture and surface nature information; According to imbibition purging rate curve, the kinetics equation of bond material imbibition purging, calculation sample parameter of pore structure; Utilize gained pore structural information assess sample hole structural property.Predetermined gas is nitrogen, oxygen, hydrogen, helium, argon gas, methane, carbon monoxide, carbon dioxide, alkene, alkane or other pure gas, or is mixed gas such as air; Predetermined liquid is water, methyl alcohol, ethanol, isopropyl alcohol, phenixin, benzene, toluene, glycerine or alkane.
The present invention also provides this method of a kind of application to measure the device of material hole structural behaviour.This device by constant temperature oven 1, sample cell 2, hopper 3, measure source of the gas 4, drive liquid source of the gas 5, drying tube 6, data acquisition system (DAS) 7, solenoid valve V1, solenoid valve V2, solenoid valve V3, solenoid valve V4, feed liquor valve V5, T-valve V6 and tensimeter P and form, sample cell 2 is the container with the top seal of three conduits, and a conduit links to each other with data acquisition system (DAS) 7 for the test pipeline; Another conduit is that blowdown piping communicates with atmosphere by solenoid valve V4; The 3rd conduit is divided into two-way through solenoid valve V1 by threeway, the one tunnel through solenoid valve V3 and drying tube 6 with measure source of the gas 4 and be connected, the one tunnel is connected with hopper 3 through solenoid valve V2; The other end of hopper 3 drives liquid source of the gas 5 through tensimeter P, T-valve V6 connection; Feed liquor valve V5 is connected between solenoid valve V2 and the hopper 3; Hopper 3, sample cell 2, and the pipeline of connection hopper 3 and sample cell 2 is positioned at constant temperature oven 1.
This device can adopt dual mode to obtain the imbibition purging kinetic curve and the balance imbibition purging amount of sample, corresponding data acquisition system (DAS) 7 is made of liquid metering device and pressure transducer respectively: the A sample is the imbibition purging under the isothermal and isobaric condition, the volume of the gas that employing fluid-discharge therapy measurement imbibition purging displaces.At this moment, the test pipeline inlet end of sample cell 2 is arranged in sample cell 2 bottom liquids, under the pressure-driven of the gas that the imbibition purging produces in sample cell 2, in the pond liquid after tested pipeline be discharged from, by the liquid metering device continuous acquisition record of data acquisition system (DAS) 7, be converted into the volume of sample imbibition purging then; The B sample is the imbibition purging under constant volume transformation condition.At this moment, the test pipeline inlet end of sample cell 2 is positioned at sample cell 2 tops, and the endpiece of test pipeline connects pressure transducer, and the pressure of continuous recording sample cell changes, and is converted to the volume of sample imbibition purging then.More than two kinds of test modes all near carrying out under the normal pressure.
The invention has the beneficial effects as follows: method of the present invention has improved the accuracy of measuring; Be particularly useful for estimating poromerics; Device of the present invention is simple, and is easy to operate, and the required sample size of evaluation procedure is few, and Measuring Time is short.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples.
Fig. 1 imbibition purging experimental provision synoptic diagram;
Among the figure: 1, constant temperature oven, 2, sample cell, 3, hopper, 4, measure source of the gas, 5, drive the liquid source of the gas; 6, drying tube, 7, data acquisition system (DAS), V1, solenoid valve, V2, solenoid valve, V3, solenoid valve, V4, solenoid valve, V5, feed liquor valve, V6, T-valve, P, tensimeter.
Suction purging (air) kinetic curve of Fig. 2 carbon molecular sieve sample.
Embodiment
Fig. 1 is the suction purging kinetic determination schematic representation of apparatus of carbon molecular sieve.This device by constant temperature oven 1, sample cell 2, hopper 3, measure source of the gas 4, drive liquid source of the gas 5, drying tube 6, data acquisition system (DAS) 7, solenoid valve V1, solenoid valve V2, solenoid valve V3, solenoid valve V4, feed liquor valve V5, T-valve V6 and tensimeter P and form, sample cell 2 is the container with the top seal of three conduits, and a conduit links to each other with data acquisition system (DAS) 7 for the test pipeline; Another conduit is that blowdown piping communicates with atmosphere by solenoid valve V4; The 3rd conduit is divided into two-way through solenoid valve V1 by threeway, the one tunnel through solenoid valve V3 and drying tube 6 with measure source of the gas 4 and be connected, the one tunnel is connected with hopper 3 through solenoid valve V2; The other end of hopper 3 drives liquid source of the gas 5 through tensimeter P, T-valve V6 connection; Feed liquor valve V5 is connected between solenoid valve V2 and the hopper 3; Hopper 3, sample cell 2, and the pipeline of connection hopper 3 and sample cell 2 is positioned at constant temperature oven 1.The test pipeline inlet end of sample cell 2 is arranged in sample cell 2 bottom liquids.
Measuring process is as follows:
(1) with the sample fragmentation, sieve 14-20 order particle, place in the air dry oven and be dried to constant weight under 105 ℃, put into exsiccator and cool off standby.This moment sample particle equilibrium adsorption air.
(2) solenoid valve V1, solenoid valve V3, solenoid valve V4 leave, and solenoid valve V2 closes, and feed liquor valve V5 closes.Gas (air that comes out in the air compressor) enters sample cell 2 by measuring source of the gas 4 through drying tubes 6, solenoid valve V3 and solenoid valve V1, enters atmosphere from blowdown piping through solenoid valve V4, pipeline is purged clean.
(3) solenoid valve V1, solenoid valve V3, solenoid valve V4 leave, and solenoid valve V2 closes, and feed liquor valve V5 opens.Water is pushed hopper 3 from feed liquor valve V5 through connecting line, standby.
(4) solenoid valve V1, solenoid valve V3, solenoid valve V4 leave, and solenoid valve V2 closes, and feed liquor valve V5 closes.The about 0.5000g sample of weighing is put into sample cell 2, and gas (air) enters sample cell 2 by measuring source of the gas 4 through drying tube 6, solenoid valve V3, solenoid valve V1, enters atmosphere from blowdown piping through solenoid valve V4.Rise constant temperature oven 1 temperature to 30 ℃ simultaneously, water and sample are heated to temperature to be measured.
(5) solenoid valve V2, solenoid valve V1, solenoid valve V4 leave, and solenoid valve V3 closes, and feed liquor valve V5 closes.Gas (air that comes out in the air compressor) is pressed into hopper 3 by driving liquid source of the gas 5 through T-valve V6, water is pressed into sample cell 2 by connecting line through solenoid valve V2, solenoid valve V1, water is full of sample cell 2 through blowdown piping, solenoid valve V4 discharges, enter data acquisition system (DAS) 7 through measuring pipeline, at this moment sample cell 2, blowdown piping, measurement pipeline are full of water, have formed a fluid-tight system.The beginning of clocking.
(6) solenoid valve V1, solenoid valve V2, solenoid valve V3, solenoid valve V4 close, and feed liquor valve V5 closes.Under the pressure-driven of the gas that the sample of 2 li of sample cells suction purging produces, in the sample cell 2 water after tested pipeline be discharged from, by the liquid metering device continuous acquisition record of data acquisition system (DAS) 7, be converted into the volume of sample suction purging then.
In the present embodiment, sample is 6 kinds of different carbon molecular sieves, and CMS1 is commercial carbon molecular sieve sample, and CMS2, CMS3, CMS4, CMS5 and CMS6 are the homemade samples in laboratory, and these selected samples have different sky branch performances.Suction purging (air) kinetic measurement of sample the results are shown in Figure 2.
As shown in Figure 2, method of the present invention and device can obtain the suction purging curve of sample exactly, and there is significant difference in the imbibition purging amount of six kinds of samples rule over time with final balance imbibition purging amount.
Claims (5)
1, utilizes the method for imbibition purging method evaluating material hole structural property, at first with the testing sample of the prescribed particle size of accurate weighing, promptly pass through after fragmentation, screening, the dried in, poromerics, place sample cell, under design temperature, feed predetermined gas in the sample cell and reach adsorption equilibrium; Switch the feeding predetermined liquid identical then with design temperature, the imbibition purging of beginning sample, the volume that feeds liquid should be greater than testing sample volume and imbibition purging volume sum, and testing sample still can be by the submergence of liquid institute after guaranteeing to reach imbibition purging balance; Utilize constant voltage fluid-discharge therapy measuring samples imbibition purging volume speed and balance imbibition purging volume over time, or under the constant volume condition in the measuring samples pond pressure of gas change to determine imbibition purging volume; Obtain sample imbibition purging rate curve under the different condition by change imbibition and purging kind, imbibition purging temperature, as the basic data of qualitative and quantitative analysis sample well gap structure and surface nature, judgement sample pore texture and surface nature information; According to imbibition purging rate curve, the kinetics equation of bond material imbibition purging, calculation sample parameter of pore structure; Utilize gained pore structural information assess sample hole structural property.
2, the method for utilizing imbibition purging method evaluating material hole structural property according to claim 1, it is characterized in that, described predetermined gas is nitrogen, oxygen, hydrogen, helium, argon gas, methane, carbon monoxide, carbon dioxide, alkene, alkane or other pure gas, perhaps is mixed gas; Predetermined liquid is water, methyl alcohol, ethanol, isopropyl alcohol, phenixin, benzene, toluene, glycerine or alkane.
3, application rights requires the 1 described device that utilizes the method for imbibition purging method evaluating material hole structural property, it is characterized in that, this device is by constant temperature oven (1), sample cell (2), hopper (3), measure source of the gas (4), drive liquid source of the gas (5), drying tube (6), data acquisition system (DAS) (7), solenoid valve (V1), solenoid valve (V2), solenoid valve (V3), solenoid valve (V4), feed liquor valve (V5), T-valve (V6) and tensimeter (P) are formed, sample cell (2) is the container with the top seal of three conduits, and conduit is test pipeline link to each other with data acquisition system (DAS) (7); Another conduit is that blowdown piping passes through solenoid valve (V4) and communicates with atmosphere; The 3rd conduit is divided into two-way through solenoid valve (V1) by threeway, the one tunnel through solenoid valve (V3) and drying tube (6) with measure source of the gas (4) and be connected, the one tunnel is connected with hopper (3) through solenoid valve (V2); The other end of hopper (3) drives liquid source of the gas (5) through tensimeter (P), T-valve (V6) connection; Feed liquor valve (V5) is connected between solenoid valve (V2) and the hopper (3); Hopper (3), sample cell (2), and the pipeline of connection hopper (3) and sample cell (2) is positioned at constant temperature oven (1).
4, application rights according to claim 3 requires the 1 described device that utilizes the method for imbibition purging method evaluating material hole structural property, it is characterized in that described data acquisition system (DAS) (7) is liquid metering device or pressure transducer.
5, application rights according to claim 3 requires the 1 described device that utilizes the method for imbibition purging method evaluating material hole structural property, it is characterized in that, this device adopts dual mode to obtain the imbibition purging kinetic curve and balance imbibition purging amount: the A of sample, sample is the imbibition purging under the isothermal and isobaric condition, the volume of the gas that employing fluid-discharge therapy measurement imbibition purging displaces, at this moment, the test pipeline inlet end of sample cell (2) is arranged in sample cell (2) bottom liquid, under the pressure-driven of the gas that the imbibition purging produces in sample cell (2), in the pond liquid after tested pipeline be discharged from, by the liquid metering device continuous acquisition record of data acquisition system (DAS) (7), be converted into the volume of sample imbibition purging then; B, sample imbibition purging under constant volume transformation condition, at this moment, the test pipeline inlet end of sample cell (2) is positioned at sample cell (2) top, and the endpiece of test pipeline connects pressure transducer, the pressure of continuous recording sample cell changes, and is converted to the volume of sample imbibition purging then; More than two kinds of test modes all near carrying out under the normal pressure.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104535473A (en) * | 2014-12-29 | 2015-04-22 | 新奥科技发展有限公司 | Method and device for representing whole pore-diameter structure distribution of chromatographic column |
| CN105203440A (en) * | 2015-09-14 | 2015-12-30 | 大连理工大学 | Method of measuring variable-pressure absorption gas separation performance of carbon molecular sieve on basis of liquid absorption gas flooding principle |
| CN108345766A (en) * | 2018-01-11 | 2018-07-31 | 大连理工大学 | A method of porous material microcellular structure is characterized based on imbibition purging process |
| CN109696380A (en) * | 2019-03-04 | 2019-04-30 | 大连理工大学 | A kind of method and device for evaluating poromerics gas separating property |
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2008
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104535473A (en) * | 2014-12-29 | 2015-04-22 | 新奥科技发展有限公司 | Method and device for representing whole pore-diameter structure distribution of chromatographic column |
| CN104535473B (en) * | 2014-12-29 | 2017-10-27 | 新奥科技发展有限公司 | A kind of overall aperture structure distribution of chromatographic column characterizes method and device |
| CN105203440A (en) * | 2015-09-14 | 2015-12-30 | 大连理工大学 | Method of measuring variable-pressure absorption gas separation performance of carbon molecular sieve on basis of liquid absorption gas flooding principle |
| CN105203440B (en) * | 2015-09-14 | 2017-10-17 | 大连理工大学 | A kind of method that carbon molecular sieve PSA Gas separating property is determined based on imbibition purging principle |
| CN108345766A (en) * | 2018-01-11 | 2018-07-31 | 大连理工大学 | A method of porous material microcellular structure is characterized based on imbibition purging process |
| CN108345766B (en) * | 2018-01-11 | 2021-05-18 | 大连理工大学 | Method for characterizing porous material microporous structure based on liquid absorption and gas dispelling processes |
| CN109696380A (en) * | 2019-03-04 | 2019-04-30 | 大连理工大学 | A kind of method and device for evaluating poromerics gas separating property |
| CN109696380B (en) * | 2019-03-04 | 2021-04-16 | 大连理工大学 | Method and device for evaluating gas separation performance of microporous material |
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