CN102313756B - Automatic swelling measuring device and swelling measuring method for coal - Google Patents
Automatic swelling measuring device and swelling measuring method for coal Download PDFInfo
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- CN102313756B CN102313756B CN 201010225203 CN201010225203A CN102313756B CN 102313756 B CN102313756 B CN 102313756B CN 201010225203 CN201010225203 CN 201010225203 CN 201010225203 A CN201010225203 A CN 201010225203A CN 102313756 B CN102313756 B CN 102313756B
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Abstract
The invention relates to an automatic swelling measuring device and a swelling measuring method for coal. The device comprises a measuring container (2), a measurement control instrument (20) and a personal computer (PC) terminal (21), wherein the measurement control instrument (20) is used for outputting a control signal to the measuring device, outputting measurement data and storing the output measurement data to the PC terminal (21); and the PC terminal (21) is used for displaying temperature data and swelling data in the experiment process and a temperature curve and a swelling curve along time variation in real time. By the automatic swelling measuring device, the swelling action of the coal in a solvent can be measured within a wider condition range from normal temperature and pressure to high temperature and pressure, the swelling variation of the coal in the solvent can be measured, and the equilibrium swelling amount and a swelling dynamic process of the coal in the solvent can also be measured. The device has the advantages of simple structure, reliable and safe high-pressure seal, high measurement accuracy, high pressure resistance and the like, is easy to operate, is used for automatic measurement and can be used for displaying the temperature data and the swelling data in the experiment process and the temperature curve and the swelling curve along the time variation in real time on a screen of the PC terminal.
Description
Technical field
The present invention relates to self-operated measuring unit and the method for the swellbility of a kind of automatic measurement coal in solvent, specifically a kind ofly be suitable for estimating coal from the normal temperature and pressure to the High Temperature High Pressure in the wider condition and range, self-operated measuring unit and the measuring method of the swelling behavior of coal in solvent.
Background technology
The research of texture of coal is focus and the most important fundamental research content of coal scientific domain always.The swelling of coal is a kind of critical nature of coal, and the swelling behavior of coal is by the interaction behavior decision between the intermolecular acting force of coal and coal and solvent.The swelling of coal can provide the structural information of more coal, and the swelling technology of coal can also improve the reactivity of coal, provides solvent at the intermolecular displacement behavior of coal.Therefore, the swelling behavior of Study on Coal, the mechanism of action between announcement solvent and the coal molecule realizes that to the characteristic of molecular structure and the coal of Study on Coal the comprehensive processing and utilization of coal and high effect cleaning conversion have very important meaning.
In recent years, the solvent swell technology has become the universal method of Study of The Macromolecular Structure of Coal and variation thereof, and swelling and corresponding research method are used to the interaction behavior between the intermolecular acting force of Study on Coal and coal and solvent.Particularly understand the swelling behavior of coal in solvent, the swelling mechanism aspect of coal is illustrated in the interaction between coal and the solvent, and the Swelling Dynamics research of coal is a kind of effective research method.
The method that the swellbility of measurement coal adopts the earliest is gravimetric method or volumetric method.Gravimetric method is exactly to be interrupted the weight that takes by weighing the swelling sample, obtains the swellbility of coal by the variation of measuring coal dust swelling front and back weight.This method is easily understood, but actual operability is not strong, needs after the measurement to calibrate by deducting the solvent that occupies in the coal hole.Volumetric method is divided into again succusion and centrifuge method (" coal science and technology " that Fan Xiaonan, Liu Xianjie, Zhang Zhongliang deliver, 2004,32 (12): 51-54; Chapter knot soldier, Geling Hill plum, " coal conversion " that Zhou Anning delivers, 2006,29 (2): 1-3; Xiong Chuan, Wang Yonggang, " clean coal technology " that Chen Wei, Liu Hanfang deliver, 2009,16 (2): 53-56), (Wang Zhicai is published in " chemistry of fuel journal " for Cao Meixia, the permanent good fortune of water to develop in addition the method for testing that has the supersonic oscillations method to combine with centrifuge method, 2008,36 (4): 385-390).In above-mentioned various existing methods, succusion repeatability is relatively poor, and centrifuge method is the maximum method of at present domestic and international equilibrium swelling experiments employing.Centrifuge method places coal dust the minor diameter flat based tubes exactly, and centrifugal certain hour on hydro-extractor is measured height of specimen (H
1), then in test tube, adding solvent and stirring, coal sample begins swelling, leaves standstill certain hour (general 24h), and is then centrifugal with identical condition, the height (H after the measurement swelling
2), calculate swelling ratio (Q=H
2/ H
1).Centrifuge method has simply, quick, the advantage that can carry out batch experiment.But, centrifuge method is measured hydro-extractor model and the rotating speed that adopts, the test tube radius, the coal sample amount, the molten ratio of coal all can have influence on the swellbility that records, and highly measure certain error is more or less arranged, particularly for swelling little sample or solvent, may certain influence be arranged to the calculating of measurement and swelling ratio highly.
Along with the development of instrument and equipment and technology, begun to occur to use micro image analysis method (Vladimir Strezov, the John A.Lucas of microscopic, Terry F.Wall, Fuel, 2005,84:1238-1245) and with laser fineness gage measure method (the Deng C R that the characteristics of coal powder distribution obtains the swellbility of coal, Nio T, Sanada Y, et al, Fuel, 1989,68:1134-1138; Cao Min, Gu Xiaohu, Zhang Aiyun, horse Man, coal conversion, 2009,32 (4): 58-60).These methods are subject to the restriction of solvent colourity because instrument is imaging observation, can not observe under the muddy condition of solvent, thereby can not measure there being solute to be dissolved in the solvent situation.
More than these method complex operations, error large, the equilibrium swelling amount of working sample only can not real time record sample time dependent swelling behavior in solvent, can't measure the Swelling Dynamics process of sample.
Particularly, coal is through solvent swell, thereby structure changes its reactivity worth is changed.Impact on Performance of Hydrogenation Liquefaction of Coal is studied many scholars with regard to the swelling behavior of coal, and the swelling pretreatment that shows coal can improve the liquefying conversion rate under the temperate condition.Therefore, the swelling of Study on Coal under the High Temperature High Pressure harsh conditions changes for gentle coal liquefaction condition, improves liquefying conversion rate, thereby exploiting economy, coal liquefaction craft is significant efficiently.
But, more than these methods for the mensuration of the swellbility of coal, can only under normal pressure and lower temperature conditions, carry out, the measurement that changes for the swelling of coal sample under high-temperature and high-pressure conditions is difficulty relatively.At present, also be not found use in the relevant report of the measurement mechanism of the swelling variation of measuring coal under the high-temperature and high-pressure conditions.
Summary of the invention
The purpose of this invention is to provide a kind of swelling self-operated measuring unit and measuring method.This measurement mechanism is applicable to measure coal swelling behavior solvent under from normal temperature and pressure to the High Temperature High Pressure all conditions.This self-operated measuring unit and method both can have been measured the swelling of coal sample in solvent and change, and can measure again equilibrium swelling amount and the Swelling Dynamics process of coal sample in solvent.
The invention provides a kind of swelling self-operated measuring unit of coal, comprise: test container, measuring and controlling instrument and PC terminal, measuring and controlling instrument output control signal is to measurement mechanism, and with measurement data output and be kept in the PC terminal, show in real time temperature and swelling data in the experimentation and time dependent temperature and swelling curve in the PC terminal;
Described test container comprises: loam cake and doffing, and both are fixedly connected with by ring flange; The top of loam cake is fixed with displacement transducer by fixed part, and the end of loam cake links to each other with the sample cylinder by link; The lower end of displacement transducer is provided with measuring staff, and measuring staff passes the through hole of loam cake, link inside, and it is inner to stretch into the sample cylinder;
In the described sample cylinder tested coal sample is housed, above tested coal sample, is provided with compressing tablet;
Described loam cake inside is provided with and is looped around measuring staff cavity on every side, forms the circulating cooling water leg, and the upper and lower end section of cavity is provided with respectively cooling water inlet and coolant outlet;
Be respectively equipped with entrance and exit on the described doffing, be connected with pressurization valve and liquid feeding valve on the entrance, be connected with pressure unit and venting valve in the outlet;
Described doffing is placed in the heating arrangement, and temperature element and electrical heating elements are installed on the heating arrangement;
Described displacement transducer, pressure unit, temperature element and electrical heating elements are electrically connected with measuring and controlling instrument respectively.
In order to make measurement result more accurate, between described loam cake and the doffing, be equipped with seal element between fixed part and the loam cake.
Further, for lock, mutual alignment between fixed connecting part and the sample cylinder, avoid that the relative link of sample cylinder is subjected to displacement in measuring process, the knot port part of described link and sample cylinder is equipped with stay.
Be threaded connection between the lower end of described link and the sample cylinder, be used for adjusting the height of sample cylinder, the measuring staff top of displacement transducer is contacted with compressing tablet, regulate the zero point of displacement transducer.
Described displacement transducer is high pressure resistant linear variable differential transformer (LVDT) formula displacement transducer, and the body of this displacement transducer and measuring staff are the integral type structure; The withstand voltage 35MPa of described displacement transducer, measuring accuracy is 0.05%, and Measurement Resolution is ± 1 μ m, and measurement range is 0～10mm.
The material of described test container is stainless steel.The material of described sample cylinder is stainless steel, is evenly distributed with a plurality of liquid drain holes around the described sample cylinder, and the bottom of sample cylinder is flat and with the sieve plate of porous.
Described heating arrangement is thermostatic bath, and this thermostatic bath comprises thermostatic box, thermostatic box loam cake, electric heating tube, thermal resistance and heating medium; Electric heating tube is connected wire and is connected with measuring and controlling instrument with thermal resistance, this thermostatic bath operating temperature range is 0～250 ℃, is preferably 0～150 ℃, and temperature-controlled precision is ± 0.1 ℃.
Described heating arrangement also can be electric heating cover, electric heating cover comprises electric heating cover urceolus, electric heating cover inner core, electric furnace heating wire heating element and thermopair, wherein the electric furnace heating wire heating element is connected wire and is connected with measuring and controlling instrument with thermopair, the operating temperature range of this electric heating cover is 0～500 ℃, be preferably 100-500 ℃, temperature-controlled precision is ± 0.1 ℃.
The pressure limit that described test container bears is 0～30MPa, and temperature range is 0～500 ℃, and Measurement Resolution is ± 1 μ m.
The present invention also provides a kind of swelling measuring method of coal, and the method adopts the swelling self-operated measuring unit of above-mentioned coal, measures the swelling behavior of coal under various solvent conditions, and the method comprises the steps:
Step 1: open the measuring and controlling instrument power supply, start the PC terminal and move testing software;
Step 2: with the tested coal sample sample cylinder of packing into, measure tested coal sample height (H
0), the stainless steel compressing tablet is placed on the tested coal sample, the sample cylinder is installed on the link of Hi-pot test container upper cover bottom, regulate sample cylinder height, the measuring staff top of displacement transducer is reliably contacted with stainless steel substrates, accurately regulate the zero point of displacement transducer, with stay fixed sample cylinder, loam cake with test container is connected with the test container doffing again, and the test container doffing is placed in the heating arrangement;
Step 3: open the liquid feeding valve, close the liquid feeding valve behind the adding swelling solvent;
Step 4: open the pressurization valve, experimental gas passed in the test container, purge 2-5 time after, be charged to the pressure unit scale and show when force value is experimental pressure, close the pressurization valve, then open circulating condensing water;
Step 5: design temperature is temperature required for experiment, starts to add heat control, makes heating arrangement begin test container is heated;
Step 6: tested coal sample swelling in solvent, promote the measuring staff of displacement transducer to top offset, displacement transducer is the variation of tested coal sample height (Δ H
i) be converted to electric signal, deliver to measuring and controlling instrument and carry out signal processing and analog to digital conversion;
Step 7: the automatic reception of PC terminal is from experimental temperature and the displacement signal data of measuring and controlling instrument, the data that receive are processed calculating and preservation, and on the PC terminal screen, show in real time temperature and swelling altitude information in the experimentation, and automatically show time dependent temperature and swelling height change curve, can obtain swelling height (the Δ H under this experimental temperature
i) and swelling ratio ((Δ H
i+ H
0)/H
0).Swelling reaches after the balance, changes experimental temperature, can measure swelling height and swelling ratio under the different temperatures.
Wherein, the experimental gas in the described step 4 is nitrogen or hydrogen.
The invention provides the swelling measuring method of another kind of coal, the method adopts the swelling self-operated measuring unit of above-mentioned coal, record under the different experiments temperature, and the Swelling Dynamics curve of tested coal sample in solvent, the method comprises the steps:
Step (1): open the measuring and controlling instrument power supply, start the PC terminal and move testing software;
Step (2): with the tested coal sample sample cylinder of packing into, measure tested coal sample height (H
0), the stainless steel compressing tablet is placed on the tested coal sample, the sample cylinder is installed on the link of test container loam cake bottom, regulate sample cylinder height, the measuring staff top of displacement transducer is reliably contacted with stainless steel substrates, accurately regulate the zero point of displacement transducer, with stay fixed sample cylinder, loam cake with test container is connected with the test container doffing again, and the test container doffing is placed in the heating arrangement;
Step (3): design temperature is temperature required for experiment, starts to add heat control, and test container is heated;
Step (4): when temperature reaches design temperature in the container to be tested, open the liquid feeding valve, with preheating or the solvent that is chilled in advance experimental temperature inject fast, close the liquid feeding valve, tested coal sample swelling in solvent promotes the measuring staff of displacement transducer to top offset, and displacement transducer is converted to electric signal to the variation of tested coal sample height (Δ H), deliver to measuring and controlling instrument and carry out signal processing and analog to digital conversion, this moment, tested coal sample height was (H
2=H
1+ Δ H), swelling ratio is (Q=H
2/ H
1);
Step (5): the automatic reception of PC terminal is from the displacement signal data of measuring and controlling instrument, the data that receive are processed calculating and preservation, and on the PC terminal screen, show in real time swelling height and swelling ratio in the experimentation, and automatically show time dependent swelling height change curve, swelling reaches after the balance, can record under this experimental temperature the Swelling Dynamics curve of tested coal sample in solvent;
Step (6): change experimental temperature, repeat above step, can record under the different experiments temperature Swelling Dynamics curve of tested coal sample in solvent.
That the swelling self-operated measuring unit of a kind of coal provided by the invention and measuring method have is simple in structure, easy operating, high pressure sealing is reliable and secure, measuring accuracy is high, withstand voltage height, automatic advantages such as measurement.Concrete, the advantage of apparatus of the present invention and method is as follows:
1, this measurement mechanism adopts high voltage bearing stainless steel test container, can be adapted in pressure 0～30MPa, 0～500 ℃ of wider scope of temperature, and the swelling behavior of coal is measured under the various solvent condition;
2, adopt measurement mechanism of the present invention and method both can measure the swelling of coal in solvent and change, can measure again equilibrium swelling amount and the Swelling Dynamics process of coal sample in solvent;
3, in measuring process, the PC terminal gathers experimental temperature and the displacement signal data from measuring and controlling instrument automatically, the data that collect are processed calculating and preservation, and on the PC terminal screen, show in real time the temperature in the experimentation, pressure and swelling data, and time dependent temperature, pressure and swelling curve are realized automatic control and measurement.
Below in conjunction with the drawings and specific embodiments technical scheme of the present invention is described in detail.
Description of drawings
Fig. 1 a and Fig. 1 b are the structural representation of swelling self-operated measuring unit of the present invention, and wherein Fig. 1 a is that heating arrangement is the structural representation of electric heating cover, and Fig. 1 b is that heating arrangement is the structural representation of thermostatic bath;
Fig. 2 is the circuit block diagram of swelling self-operated measuring unit of the present invention;
Fig. 3 be tested coal sample under the 3MPa condition of nitrogen gas of colding pressing from room temperature to 400 ℃ swelling curve;
Fig. 4 is that tested coal sample is at CS
2Equilibrium swelling amount and Swelling Dynamics curve under the middle different temperatures.
Main element description of reference numerals among the figure:
The 1-displacement transducer; The 2-test container; 3-circulating cooling water leg; The 4-fixed part; The 5-loam cake; The 6-doffing; The 7-link; The 8-measuring staff; The 9-cooling water inlet; The 10-coolant outlet; The 11-compressing tablet; The 12-stay; 13-sample cylinder; The 14-solvent; The tested coal sample of 15-; The 16-valve that pressurizes; 17-liquid feeding valve; The 18-air release; The 19-pressure unit; The 20-measuring and controlling instrument; The 21-PC terminal; The 22-electric heating cover; 23-electric heating cover urceolus; 24-electric heating cover inner core; The 25-thermopair; 26-electric furnace heating wire heating element; The 27-thermostatic bath; The 28-thermostatic box; 29-thermostatic box loam cake; The 30-electric heating tube; The 31-thermal resistance.
Embodiment
Below in conjunction with embodiment the specific embodiment of the present invention is done further and to be described in detail.
Embodiment one
Fig. 1 a is the structural representation of swelling self-operated measuring unit of the present invention.As shown in Figure 1a, be the embodiment one of the swelling self-operated measuring unit of coal of the present invention, the heating arrangement in this device is electric heating cover.The swelling self-operated measuring unit of coal comprises: test container 2, measuring and controlling instrument 20 and PC terminal 21, measuring and controlling instrument 20 output control signals are to measurement mechanism, and with measurement data output and be kept in the PC terminal 21, in PC terminal 21 real-time temperature and the swelling data that show in the experimentation, and time dependent temperature and swelling curve; Described test container 2 comprises: loam cake 5 and doffing 6, and both are fixedly connected with by ring flange; The top of loam cake 5 is fixed with displacement transducer 1 by fixed part 4, and the end of loam cake 5 links to each other with sample cylinder 13 by link 7; The lower end of displacement transducer 1 is provided with measuring staff 8, and measuring staff 8 passes the through hole of loam cake 5, link 7 inside, stretches into sample cylinder 13 inside; Tested coal sample 15 is housed in the described sample cylinder 13, above tested coal sample 15, is provided with compressing tablet 11; Described loam cake 5 inside are provided with and are looped around measuring staff 8 cavity on every side, form the circulating cooling water leg, and the upper and lower end section of cavity is provided with respectively cooling water inlet 9 and coolant outlet 10; Be respectively equipped with entrance and exit on the described doffing 6, be connected with pressurization valve 16 and liquid feeding valve 17 on the entrance, be connected with pressure unit 19 and venting valve 18 in the outlet; Described doffing 6 is placed in the heating arrangement, and temperature element and electrical heating elements are installed on the heating arrangement; Described displacement transducer 1, pressure unit 19, temperature element and electrical heating elements are electrically connected with measuring and controlling instrument 20 respectively.
In order to make measurement result more accurate, between described loam cake 5 and the doffing 6, be equipped with seal element between fixed part 4 and the loam cake 5.The knot port part of described link 7 and sample cylinder 13 is equipped with stay 12, is used for the mutual alignment between locking, fixed connecting part 7 and the sample cylinder 13, avoids that sample cylinder 13 relative links 7 are subjected to displacement in measuring process.
Be threaded connection between the lower end of described link 7 and the sample cylinder 13, be used for adjusting the height of sample cylinder 13, measuring staff 8 tops of displacement transducer 1 are contacted with compressing tablet 11, regulate the zero point of displacement transducer 1.Described displacement transducer 1 is high pressure resistant linear variable differential transformer (LVDT) formula displacement transducer, and the body of this displacement transducer 1 and measuring staff 8 are the integral type structure; Described displacement transducer 1 withstand voltage 35MPa, measuring accuracy is 0.05%, and Measurement Resolution is ± 1 μ m, and measurement range is 0～10mm.
The material of described test container 2 and sample cylinder 13 is stainless steel, and is evenly distributed with a plurality of liquid drain holes around the described sample cylinder 13, and the bottom of sample cylinder 13 is flat and with the sieve plate of porous.
In the present embodiment, described heating arrangement is electric heating cover 22, electric heating cover 22 comprises electric heating cover urceolus 23, electric heating cover inner core 24, electric furnace heating wire heating element 26 and thermopair 25, wherein electric furnace heating wire heating element 26 is connected with thermopair and is connected with measuring and controlling instrument 20 by wire, the operating temperature range of this electric heating cover is 0～500 ℃, be preferably 100-500 ℃, temperature-controlled precision is ± 0.1 ℃.The temperature control of electric heating cover 22 is by the temperature of measuring and controlling instrument 20 by thermopair 25 measurement electric heating covers 22, and the thereof using PID control technology is controlled electric furnace heating wire heating element 26 and realized electric heating cover 22 is carried out temperature control.Displacement transducer 1 is connected with measuring and controlling instrument 20 by shielded cable.Measuring and controlling instrument 20 is connected with PC terminal 21 by RS232 communication wire.
Fig. 2 is the circuit block diagram of swelling self-operated measuring unit of the present invention, and such as Fig. 2 and in conjunction with shown in Fig. 1 a, the swelling measuring method of the coal of present embodiment may further comprise the steps:
Step 1: open measuring and controlling instrument 20 power supplys, start PC terminal 21 and move testing software;
Step 2: with the tested coal sample 15 sample cylinder 13 of packing into, concussion evenly makes surface level, measures tested coal sample height H
0Stainless steel compressing tablet 11 is placed on the tested coal sample 15, sample cylinder 13 is installed on the link 7 of loam cake 5 bottoms of test container, regulate the height of sample cylinder 13, the top of the measuring staff 8 of displacement transducer 1 is reliably contacted with stainless steel compressing tablet 11, accurately regulate the zero point of displacement transducer, with stay 12 fixed sample cylinders 13, again the loam cake 5 of test container is connected connection with the test container doffing, test container doffing 6 is placed in the electric heating cover 22;
Step 3: open liquid feeding valve 17, close liquid feeding valve 17 behind the adding solvent 14;
Step 4: open pressurization valve 16, experimental gas (nitrogen, hydrogen etc.) is passed into test container 2 inside, purge 3 times, be charged to experimental pressure, pressure unit 19 is used for measuring Hi-pot test container 2 internal pressures, close pressurization valve 16, open recirculated cooling water, 9 pass into chilled water to circulating cooling water leg 3 from the cooling water inlet;
Step 5: design temperature is temperature required for experiment on measuring and controlling instrument 20, starts to add heat control, makes electric heating cover 22 begin test container 2 is heated;
Step 6: tested coal sample 15 swelling in solvent 14, promote the measuring staff 8 of displacement transducer 1 to top offset, displacement transducer 1 is converted to electric signal to the variation (Δ H) of tested coal sample 15 height, delivers to measuring and controlling instrument 20 and carries out signal processing and analog to digital conversion;
Step 7: 21 automatic receptions of PC terminal are from the experimental temperature of measuring and controlling instrument 20, pressure and displacement signal data, the data that receive are processed calculating and preservation, and on the PC terminal screen, show in real time the temperature in the experimentation, pressure and swelling altitude information, and automatically show time dependent temperature and swelling change curve.Swelling reaches after the balance, changes experimental temperature, can measure the swelling change curve under the different temperatures.
Fig. 3 be tested coal sample under the 3MPa condition of nitrogen gas of colding pressing from room temperature to 400 ℃ swelling curve.As shown in Figure 3, swelling curve is the result show, when swelling temperature is lower than 300 ℃, the swelling height change value Δ H of coal sample is along with the rising of the prolongation of swelling time and swelling temperature and increase, when swelling temperature reaches more than 350 ℃, the swelling height change value Δ H of coal sample begins to reduce on the contrary, and this trend is especially remarkable under 400 ℃ swelling temperature.This should be dissolved in the solvent with hydrocarbon partial in the coal under the higher temperature and in the coal gasification of part volatile matter relevant.
Embodiment two
Fig. 1 b is the structural representation of swelling self-operated measuring unit of the present invention.Shown in Fig. 1 b, be the embodiment two of the swelling self-operated measuring unit of coal of the present invention, the heating arrangement in this device is thermostatic bath.Structure broadly similar among the structure of present embodiment and the embodiment one, from different among the embodiment one be that described heating arrangement is thermostatic bath 27, this thermostatic bath 27 comprises thermostatic box 28, thermostatic box loam cake 29, electric heating tube 30, thermal resistance 31 and heating medium; Electric heating tube 30 is connected with thermal resistance and is connected with measuring and controlling instrument 20 by wire, and these thermostatic bath 27 operating temperature ranges are 0～250 ℃, are preferably 0～150 ℃, and temperature-controlled precision is ± 0.1 ℃.
The temperature control of thermostatic bath 27 is by the temperature of measuring and controlling instrument 20 by thermal resistance 31 measurement thermostatic baths 27 inside, and the thereof using PID control technology is controlled 30 pairs of thermostatic baths of electric heating tube 27 and carried out temperature control.Displacement transducer 1 is connected with measuring and controlling instrument 20 by shielded cable.Measuring and controlling instrument 5 is connected with PC terminal 21 by RS232 communication wire.
The swelling measuring method of the coal in the present embodiment may further comprise the steps:
Step (1): open measuring and controlling instrument 20 power supplys, start PC terminal 21 and move testing software;
Step (2): with the tested coal sample 15 sample cylinder 13 of packing into, concussion evenly makes surface level, measures tested coal sample 15 height H
0Stainless steel compressing tablet 11 is placed on the tested coal sample 15, sample cylinder 13 is installed on the link 7 of loam cake 5 bottoms of test container, regulate the height of sample cylinder 13, the top of the measuring staff 8 of displacement transducer 1 is reliably contacted with stainless steel substrates 11, accurately regulate the zero point of displacement transducer, with stay 12 fixed sample cylinders 13, again the loam cake 5 of test container is connected connection with the test container doffing, test container doffing 6 is placed in the thermostatic bath 27;
Step (3): design temperature is temperature required for experiment on measuring and controlling instrument 20, starts to add heat control, and thermostatic bath 27 is heated;
Step (4): treat that thermostatic bath 27 temperature arrive design temperature, open liquid feeding valve 17, with preheating or the solvent 14 that is chilled in advance experimental temperature inject fast, close liquid feeding valve 17, tested coal sample 15 swelling in solvent 14 promotes the measuring staff 8 of displacement transducer 1 to top offset, and displacement transducer 1 is converted to electric signal to the changes delta H of tested coal sample 15 height, deliver to measuring and controlling instrument 20 and carry out signal processing and analog to digital conversion, this moment, tested coal sample 15 highly was H
2=H
1+ Δ H, swelling ratio are Q=H
2/ H
1
Step (5): 21 automatic receptions of PC terminal are from the experimental temperature of measuring and controlling instrument 20, pressure and displacement signal data, the data that receive are processed calculating and preservation, and on the PC terminal screen, show in real time swelling height and swelling ratio data in the experimentation, and automatically show time dependent swelling height change curve.Swelling reaches after the balance, and experiment finishes, and can record under this experimental temperature the Swelling Dynamics curve of tested coal sample 15 in solvent 14;
Step (6): change experimental temperature, repeat above experiment, can record under the different experiments temperature Swelling Dynamics curve of coal sample in solvent.
Fig. 4 is that tested coal sample is at CS
2Equilibrium swelling amount and Swelling Dynamics curve under the middle different temperatures.As shown in Figure 4, wherein, Fig. 4 a be coal sample respectively under the temperature conditions of 25 ℃, 30 ℃, 35 ℃ and 40 ℃ at CS
2The Swelling Dynamics curve of swelling in the time of 1440 minutes in the solvent, Fig. 4 b are the front 10 minutes partial enlarged drawings of Swelling Dynamics curve among Fig. 4 a.Can find out that such as Fig. 4 a, Fig. 4 b under 25 ℃, 30 ℃, 35 ℃ and 40 ℃ of swelling temperature conditions, coal sample is at CS
2Swelling reached swelling equilibrium in the solvent in front 180 minutes, and after this, along with the prolongation of swelling time, swelling ratio Q remains unchanged substantially.
Below described embodiment of the present invention in detail, can do a lot of improvement and variation obviously for a person skilled in the art and can not deviate from essence spirit of the present invention.All these changes and improvements are all within protection scope of the present invention.
Claims (15)
1. the swelling self-operated measuring unit of a coal, it is characterized in that, comprise: test container (2), measuring and controlling instrument (20) and PC terminal (21), measuring and controlling instrument (20) output control signal is to measurement mechanism, and with measurement data output and be kept in the PC terminal (21), show in real time temperature and swelling data in the experimentation and time dependent temperature and swelling curve in PC terminal (21);
Described test container (2) comprising: loam cake (5) and doffing (6), and both are fixedly connected with by ring flange; The top of loam cake (5) is fixed with displacement transducer (1) by fixed part (4), and the end of loam cake (5) links to each other with sample cylinder (13) by link (7); The lower end of displacement transducer (1) is provided with measuring staff (8), and measuring staff (8) passes loam cake (5), the inner through hole of link (7), stretches into sample cylinder (13) inside;
Tested coal sample (15) is housed in the described sample cylinder (13), is provided with compressing tablet (11) in tested coal sample (15) top;
Described loam cake (5) inside is provided with and is looped around measuring staff (8) cavity on every side, forms the circulating cooling water leg, and the upper and lower end section of cavity is provided with respectively cooling water inlet (9) and coolant outlet (10);
Described doffing is respectively equipped with entrance and exit on (6), is connected with pressurization valve (16) and liquid feeding valve (17) on the entrance, is connected with pressure unit (19) and venting valve (18) in the outlet;
Described doffing (6) is placed in the heating arrangement, and temperature element and electrical heating elements are installed on the heating arrangement;
Described displacement transducer (1), pressure unit (19), temperature element and electrical heating elements are electrically connected with measuring and controlling instrument (20) respectively.
2. the swelling self-operated measuring unit of coal as claimed in claim 1 is characterized in that, between described loam cake (5) and the doffing (6), be equipped with seal element between fixed part (4) and the loam cake (5).
3. the swelling self-operated measuring unit of coal as claimed in claim 1, it is characterized in that, the interface position of described link (7) and sample cylinder (13) is equipped with stay (12), be used for the mutual alignment between locking, fixed connecting part (7) and the sample cylinder (13), avoid that the relative link of sample cylinder (13) is subjected to displacement in measuring process.
4. the swelling self-operated measuring unit of coal as claimed in claim 1, it is characterized in that, be threaded connection between the lower end of described link (7) and the sample cylinder (13), be used for adjusting the height of sample cylinder (13), measuring staff (8) top of displacement transducer (1) is contacted with compressing tablet (11), regulate the zero point of displacement transducer (1).
5. the swelling self-operated measuring unit of coal as claimed in claim 1, it is characterized in that, described displacement transducer (1) is high pressure resistant linear variable differential transformer (LVDT) formula displacement transducer, and the body of this displacement transducer (1) and measuring staff (8) are the integral type structure; The withstand voltage 35MPa of described displacement transducer (1), measuring accuracy is 0.05%, and Measurement Resolution is ± 1 μ m, and measurement range is 0～10mm.
6. the swelling self-operated measuring unit of coal as claimed in claim 1 is characterized in that, the material of described test container (2) is stainless steel.
7. the swelling self-operated measuring unit of coal as claimed in claim 1, it is characterized in that, the material of described sample cylinder (13) is stainless steel, and described sample cylinder (13) is evenly distributed with a plurality of liquid drain holes on every side, and the bottom of sample cylinder (13) is flat and with the sieve plate of porous.
8. the swelling self-operated measuring unit of coal as claimed in claim 1, it is characterized in that, described heating arrangement is thermostatic bath (27), and this thermostatic bath (27) comprises thermostatic box (28), thermostatic box loam cake (29), electric heating tube (30), thermal resistance (31) and heating medium; Electric heating tube (30) is connected 31 with thermal resistance) be connected with measuring and controlling instrument (20) by wire, this thermostatic bath (27) operating temperature range is 0～250 ℃, temperature-controlled precision is ± 0.1 ℃.
9. the swelling self-operated measuring unit of coal as claimed in claim 8 is characterized in that, this thermostatic bath (27) operating temperature range is 0～150 ℃.
10. the swelling self-operated measuring unit of coal as claimed in claim 1, it is characterized in that, described heating arrangement is electric heating cover (22), electric heating cover (22) comprises electric heating cover urceolus (23), electric heating cover inner core (24), electric furnace heating wire heating element (26) and thermopair (25), wherein electric furnace heating wire heating element (26) is connected 25 with thermopair) be connected with measuring and controlling instrument (20) by wire, the operating temperature range of this electric heating cover is 0～500 ℃, and temperature-controlled precision is ± 0.1 ℃.
11. the swelling self-operated measuring unit of coal as claimed in claim 10 is characterized in that, the operating temperature range of described electric heating cover is 100-500 ℃,
12. the swelling self-operated measuring unit of coal as claimed in claim 1 is characterized in that the pressure limit that described test container bears is 0～30MPa, temperature range is 0～500 ℃, and Measurement Resolution is ± 1 μ m.
13. the swelling measuring method of a coal, the method adopts the swelling self-operated measuring unit such as each described coal of claim 1-12, measures the swelling behavior of coal under various solvent conditions, it is characterized in that the method comprises the steps:
Step 1: open measuring and controlling instrument (20) power supply, start PC terminal (21) and move testing software;
Step 2: with tested coal sample (15) the sample cylinder (13) of packing into, measure tested coal sample (15) height H
0Compressing tablet (11) is placed on the tested coal sample (15), sample cylinder (13) is installed on the link (7) of loam cake (5) bottom of Hi-pot test container (2), regulate sample cylinder (13) highly, measuring staff (8) top of displacement transducer (1) is reliably contacted with compressing tablet (11), accurately regulate the zero point of displacement transducer (1), with stay (12) fixed sample cylinder (13), again the loam cake (5) of test container (2) is connected 2 with test container) doffing (6) connect, the doffing (6) of test container (2) is placed in the heating arrangement;
Step 3: open liquid feeding valve (17), close liquid feeding valve (16) behind the adding solvent (14);
Step 4: open pressurization valve (16), experimental gas is passed in the test container (2), purge 2-5 time after, be charged to pressure unit (19) scale and show when force value is experimental pressure, close pressurization valve (16), then open circulating condensing water;
Step 5: design temperature is temperature required for experiment, starts to add heat control, makes heating arrangement begin test container is heated;
Step 6: tested coal sample (15) swelling in solvent, promote the measuring staff (8) of displacement transducer (1) to top offset, displacement transducer (1) is the changes delta H of tested coal sample (15) height
iBe converted to electric signal, deliver to measuring and controlling instrument (20) and carry out signal processing and analog to digital conversion;
Step 7: PC terminal (21) automatic reception is from experimental temperature and the displacement signal data of measuring and controlling instrument (20), the data that receive are processed calculating and preservation, and on PC terminal (21) screen, show in real time temperature and swelling altitude information in the experimentation, and automatically show time dependent temperature and swelling height change curve, can obtain the swelling height Δ H under this experimental temperature
iAnd swelling ratio (Δ H
i+ H
0)/H
0Swelling reaches after the balance, changes experimental temperature, can measure swelling height and swelling ratio under the different temperatures.
14. the swelling measuring method of coal as claimed in claim 13 is characterized in that, the experimental gas in the described step 4 is nitrogen or hydrogen.
15. the swelling measuring method of a coal, the method adopts the swelling self-operated measuring unit such as each described coal of claim 1-12, records under the different experiments temperature Swelling Dynamics curve of coal sample in solvent, it is characterized in that the method comprises the steps:
Step (1): open measuring and controlling instrument (20) power supply, start PC terminal (21) and move testing software;
Step (2): with tested coal sample (15) the sample cylinder (13) of packing into, measure tested coal sample height H
0Stainless compressing tablet (11) is placed on the tested coal sample (15), sample cylinder (13) is installed on the link (7) of loam cake (5) bottom of test container (2), regulate sample cylinder (13) highly, measuring staff (8) top of displacement transducer (1) is reliably contacted with stainless compressing tablet (11), accurately regulate the zero point of displacement transducer (1), with stay (12) fixed sample cylinder (13), again the loam cake (5) of test container (2) is connected 2 with test container) doffing (6) connect, the doffing (6) of test container (2) is placed in the heating arrangement;
Step (3): design temperature is temperature required for experiment, starts to add heat control, and test container is heated;
Step (4): when the interior temperature of container to be tested (2) reaches design temperature, open liquid feeding valve (17), with preheating or the solvent (14) that is chilled in advance experimental temperature inject fast, close liquid feeding valve (17), tested coal sample (15) is swelling in solvent (14), promote the measuring staff (8) of displacement transducer (1) to top offset, displacement transducer (1) is converted to electric signal to the changes delta H of tested coal sample (15) height, deliver to measuring and controlling instrument (20) and carry out signal processing and analog to digital conversion, tested coal sample this moment (15) highly is H
2=H
1+ Δ H, swelling ratio are Q=H
2/ H
1
Step (5): PC terminal (21) automatic reception is from the displacement signal data of measuring and controlling instrument (20), the data that receive are processed calculating and preservation, and on PC terminal (21) screen, show in real time swelling height and swelling ratio in the experimentation, and automatically show time dependent swelling height change curve, swelling reaches after the balance, can record under this experimental temperature the Swelling Dynamics curve of tested coal sample (15) in solvent (14);
Step (6): change experimental temperature, repeat above step, can record under the different experiments temperature Swelling Dynamics curve of tested coal sample (15) in solvent (14).
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| CN103822936A (en) * | 2014-03-05 | 2014-05-28 | 叶俊 | Molding sand and core sand high-temperature property detection instrument and molding sand and core sand high-temperature property detection method |
| CN104833732B (en) * | 2015-02-13 | 2016-11-16 | 新疆大学 | The assay method of coal solubility parameter |
| CN105349163A (en) * | 2015-10-23 | 2016-02-24 | 北京中科诚毅科技发展有限公司 | On-line detection and control method and apparatus thereof for swelling degree of coal |
| CN107860677A (en) * | 2017-10-23 | 2018-03-30 | 合肥国轩高科动力能源有限公司 | Testing device and testing method for detecting swelling degree of lithium battery material |
| CN108169417B (en) * | 2017-12-13 | 2020-05-22 | 中国工程物理研究院化工材料研究所 | Intelligent dynamic swelling degree testing device and testing method |
| CN109883878A (en) * | 2019-03-05 | 2019-06-14 | 重庆大学 | A kind of water bath with thermostatic control fire damp desorption measurement device and its measuring method |
| CN111965090B (en) * | 2020-09-15 | 2023-08-18 | 天津市捷威动力工业有限公司 | Measurement device and characterization method for swelling characteristics of high polymer for lithium battery |
| CN114924033A (en) * | 2022-04-07 | 2022-08-19 | 中国科学院广州地球化学研究所 | Micro temperature control swelling tester and use method thereof |
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Address after: 101407 No.1, south 2nd Yueyuan street, C District, Yanqi Economic Development Zone, Huairou District, Beijing Patentee after: Zhongke synthetic oil Technology Co.,Ltd. Address before: 101407 No.1, south 2nd Yueyuan street, C District, Yanqi Economic Development Zone, Huairou District, Beijing Patentee before: SYNFUELS CHINA TECHNOLOGY Co.,Ltd. |