CN101799451A - Method and device for representing relation of pressure, specific volume and temperature of substance by ultrasonic signals - Google Patents
Method and device for representing relation of pressure, specific volume and temperature of substance by ultrasonic signals Download PDFInfo
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- CN101799451A CN101799451A CN201010128520A CN201010128520A CN101799451A CN 101799451 A CN101799451 A CN 101799451A CN 201010128520 A CN201010128520 A CN 201010128520A CN 201010128520 A CN201010128520 A CN 201010128520A CN 101799451 A CN101799451 A CN 101799451A
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Abstract
The invention discloses a method for testing the relation of the pressure, the specific volume and the temperature of a substance by regulating the volume of a material in a material chamber by a piston and meanwhile testing the pressure and the temperature of the material in the material chamber. The proper position of the material chamber is provided with a probe and can also synchronously test ultrasonic wave signals in the material when being connected with an ultrasonic wave measurement and control system. The corresponding relation of the synchronously acquired two signals can be comparatively analyzed, and thereby, the condensed state problems of a polymer and other fluids can be represented without loss. The device can also carry out on-line representation by installing a pipeline on a runner. The device comprises a mounting plate (1), a fixed bolt (2), a temperature and pressure sensor (3), a material to be measured (4), a piston (5), a piston rod (6), a temperature controlled heating charging barrel (7), an ultrasonic wave probe and ultrasonic wave measurement and control system (8) and a sealing nut (9). A piston drive system can be a manual piston drive system, a power-driven piston drive system or a hydraulic drive piston drive system. The test is suitable for polymers and blending systems thereof, composite material, and other fluids, powders and solids.
Description
Technical field
The invention belongs to material and fluid test technical field, relate to the detection method and the device of a kind of material pressure (P), volume (V), temperature (T) relation, relate in particular to a kind of detection method with the related polymer P of ultrasonic signal-V-T relation.
Background technology
The PVT relation of material, promptly the mutual relationship between the pressure of material (P), volume (V), the temperature (T) as the fundamental property of material, has crucial effect at the aspects such as production, processing and application of material and fluid.
Common PVT detection technique has plunger technology (directly pressurization) and two kinds of confining liquid technology (pressurization indirectly) at present.Directly the testing apparatus of pressurization mainly is made up of several parts such as sample chamber, heating and cooling system, pressurization power system, sensor one-level data acquisition control systems.When test, sample is put into the sample chamber, and, by plunger it is pressurizeed then its upper-lower seal.Its advantage is that its principle is simple, does not introduce any non-sample material, has replaced the liquid medium of a sealing process with sealing gasket or ring, thereby has both guaranteed the impermeability of system, has saved many calibration steps again.The testing apparatus of pressurization has increased confining liquid pressure transmitting medium (being generally mercury) in the sample chamber for direct pressurization indirectly.During test, sample is immersed in the pressure transmitting medium fully, and pressurization power system actuation plunger is pressurizeed to polymer sample indirectly by liquid.The advantage of indirect method has been to introduce the liquid medium of a sealing process, guarantee system's good sealing property, extraneous gas can not invaded in the sample, and adopted pressure transmitting medium can make inside reach higher vacuum tightness, sample is under the hydrostatic pressure state, stressed even.
Adopt the instrument and equipment of above two kinds of technology can only obtain the PVT data of sample, most of producers also can only formulate production technology according to this data result.And influence factor is various in the actual production process, and the state when final output still be can not determine.This just requires not only in test PVT, adopts Dynamic Non-Destruction Measurement such as ultrasound wave directly to characterize wherein condensed state problem, so with opening relationships such as PVT, obtain more material performances and structural information.The present invention has illustrated that ultrasonic signal can directly reflect the PVT characteristic.
Summary of the invention
The object of the invention provides a kind of detection method and device that can be used for material pressure (P), specific volume (V), temperature (T) relation, and simultaneously ultrasonic signal is associated with the PVT data detecting, make this signal results can be used for the online detection of polymer production; Also be convenient to obtain more material information.
Pressure-specific volume-temperature relation testing scheme of the present invention is seen Fig. 1, has adopted the caliberating device of being made up of the measure portion (displacement measurement dial plate, temperature sensor 3, pressure transducer 8, PID temperature controller and pressure controller, ultrasonic probe system) of the running part of actuation plunger 6 motions, the working portion (material storage tube 7, plunger 6, sealing nut 9, well heater) that contains measured object 4 and correlated variables.Raw material 4 is sealed in the material storage tube 7 by sealing nut 9 and plunger piston end 5; By well heater raw material in the material storage tube is heated, its temperature is recorded and is controlled by the PID temperature controller by the thermopair of material storage tube sidewall; Its pressure is recorded by the pressure transducer of material storage tube sidewall; By direct or indirect measurement plunger displacement, multiply by material chamber sectional area and obtain the volume of material of moment, and then calculate specific volume and density etc.Running part can adopt band, chain or motor direct-drive plunger motion and change the material cavity volume.Total system is bound up on the fixed head 1 by bolt 2.
The mounting arrangement of sensor and ultrasonic probe is seen Fig. 2.Two ultrasonic probes 1 and 4 are installed in contraposition in the surface level of pressure transducer 6 and temperature sensor 2 installations, send with ultrasonic signal respectively, accept passage and be connected by signal transmssion line, the ultrasonic signal that sends, accepts filters in the disposal system (see figure 3), computing etc., thereby obtains ultrasound wave transmission speed, attenuation coefficient and the image of material under this PVT state.
On a cross section in material chamber, but pressure and temperature sensor contraposition installation in vertical its direction of 90 °, guarantees to install ultrasound wave point-blank and sends probe and accept probe.Like this, total system is made up of PVT calibration system and ultrasound wave on-line detecting system.Thereby realize PVT and ultrasound wave synchronism detection.
The principle of the characterizing method of this pressure-specific volume-temperature relation is the method by direct pressurization, records the specific volume under different pressures, the temperature, and according to the different ultrasonic signals that obtain under the corresponding conditions of ultrasound wave velocity of propagation in different medium.
The operation steps of off-line test is:
(1) before the test, tested material is carried out pre-treatments such as drying, remove moisture and impurity, in order to avoid produce bad result such as bubble during heating and melting.
(2) connect total system, power-on, chilled water, start-up temperature, pressure and displacement measurement instrument and ultrasonic system, the signal data that normal operation of check and energy rapid extraction need.
(3) ready raw material is added in the material storage tube, the material storage tube temperature is heated to a certain temperature on the material fusing point, and material is pressurizeed, under this temperature, keep certain pressure a period of time, issuable gas is discharged by plunger.Can carry out following experiment after check PVT and the ultrasonic signal data stabilization.
(4) set value in control material storage tube temperature, pressure and the piston displacement, regulate another one and test the 3rd variable, treat the corresponding data group of volume of material in stable back record different temperatures, pressure and the material storage tube.
(5) when carrying out the PVT test, obtain one group of ultrasonic signal, signal is preserved by ultrasonic on-line detecting system with ultrasonic system, and corresponding with corresponding PVT data.Circulation is carried out like this, just obtains the ultrasound wave response of material under certain PVT state.
(6) after experiment finishes, material storage tube is naturally cooled to the temperature that ejects of this kind polymer samples, take off sealing nut, sample is ejected the quality of measuring samples from the material storage tube below.
(7) material PVT data and corresponding ultrasonic signal are handled, mapping or numerical analysis calculate material specific volume (or density) and ultrasound wave transmission speed, attenuation coefficient and phase differential, analyze the corresponding relation of these information.
The method of on-line testing is: in this proving installation material chamber topmost perforate, the form by valve-pipe-valve is connected with runner places such as extruder or injector and head or nozzles.The runner inner fluid is injected this proving installation material chamber fast, behind the shut-off valve, just can carry out above PVT-ultrasound wave synchronism detection, can draw the polymer P VT state in the process.
This method is not only applicable to the online detection of polymer P VT of one-component, is applicable to the polymkeric substance after the modifications such as mixing, filling yet; Also be applicable to other fluid substance such as food, propellant, coal slurry.Processes such as suitable other a lot of materials processings, material transport are measured easy, applied widely.
Specific embodiment one
This example adopts manually operated form to drive leading screw so that drive the motion of piston in the barrel.
As shown in Figure 4, this contrive equipment is made up of rocking handle 1, synchronous pulley 2, displacement measurement dial plate 3, ball-screw 4, material storage tube 5, heating collar 6, ultrasonic probe 7, support 8, tensimeter 9, temperature controller 10, plunger 11, pressure transducer 12, work nut 13, temperature sensor 14 and ultrasound wave on-line measuring device 15.Two ultrasonic probes 7 are installed in the both sides of material storage tube 5 relatively, are with ultrasonic probe to be separately installed with temperature sensor 14 and pressure transducer 12 on 90 ° of directions.
At first use work nut 13 with material storage tube 5 lower end closed, rotation crank 1 drives ball-screw 4 and moves up, make plunger 11 rise on the material storage tube 4 on the plane, regulate 6 pairs of material storage tubes 5 of temperature controller 10 control heating collars and be heated to a certain temperature on tested polymkeric substance (as the polypropylene) fusing point (about 180 ℃).The polypropylene granules that drying is good joins in the material storage tube 5 after treating temperature stabilization, and rotation crank 1 drives ball-screw 4 and move down, and makes plunger 11 drop to material storage tube conical surface lower limb, the record null position.Be rotated further rocking handle 1 and make plunger 11 continue to descend, show certain pressure (about 10MPa), pressure is maintained this numerical value a period of time, and write down plunger decline displacement at any time up to tensimeter 9.
By the time under this temperature (about 180 ℃), when the constant pressure of plunger position still remains on the 10MPa left and right sides, illustrate that exhaust phase finishes.Being rotated further rocking handle 1 pressurizes by the material in 11 pairs of material storage tubes 5 of plunger, under a certain pressure value, read plunger 11 down positions, and by the ultrasound wave waveform signal (respectively reading once under 30MPa, 50MPa, 70MPa, 90MPa, the 100MPa) under ultrasound wave on-line measuring device 15 these temperature of record, the pressure.Rotation crank 1 drives plunger 11 and rises to following a certain position at zero point, and pressure is reduced to about 10MPa, writes down this plunger position, and descends 5 ℃ by the temperature of temperature controller 10 with material storage tube 5.Behind the temperature stabilization, repeat above operation.Plunger position and the ultrasonic signals under one group of different pressures (30MPa, 50MPa, 70MPa, 90MPa, 100MPa) are measured in 5 ℃ of every afterwards declines, are reduced to softening temperature maybe can't continue to measure the time until temperature.
Pressure is maintained lasting cooling about 10MPa, by the time in the material storage tube 5 after the material full solidification, the nut 13 of will working screws off from the below, and rotation crank 1 ejects completely crued material in the material storage tube 5 by plunger 11 from the below, with material metage and the record data that eject.
(180 ℃-115 ℃ of polymer samples (polypropylene) different temperatures have been obtained by this experiment, per 5 ℃ is one at interval), different pressures (30MPa, 50MPa, 70MPa, 90MPa, 100MPa) down density data (drawing) by plunger position, material storage tube volume and example weight conversion and with the ultrasonic velocity data under the condition (by gained after the ultrasound wave waveform signal Processing), polypropylene density is associated with ultrasonic velocity, gets relation as shown in Figure 5.Fig. 5 (1) illustrates the corresponding relation with the polypropylene specific volume-temperature-pressure of this device to test; Fig. 5 (2) illustrates the transmission speed of ultrasound wave in melt under different temperatures and the pressure, and this curve and density polymer-temperature curve are similar; Fig. 5 (3) demonstrates ultrasonic velocity and polypropylene density (inverse of specific volume) has good corresponding relation, aborning can the online ultrasonic signal that records is corresponding with this figure, obtain the PVT state in the actual processing, thus observing and controlling flow liquid process parameter.
Specific embodiment two
This example adopts motor speed measuring rotation turn-screw so that drive the motion of piston in the barrel.
As shown in Figure 6, this contrive equipment is made up of lower installation board 1, support 2, the ultrasonic demarcation of PVT-unit 3, setscrew nut 4, upper mounting plate 5, parts of bearings 6, belt wheel hub 7, big belt wheel (or gear) 8, leading screw 9, belt or chain 10, speed control motor 11, small pulley (or gear) 12, motor supporting seat 13 and ultrasound wave on-line measuring device.Sensor and ultrasonic probe are installed according to Fig. 1,2.
Different with embodiment one, the motor revolution is the steamboat revolution, and bull wheel and the proportional relation of steamboat revolution can converse the leading screw rotational speed by the motor revolution like this, calculates the distance that leading screw vertically moves again, and then calculates the volume in the material cavity.According to the pressure and temperature of test, just can draw the PVT curve.The method of obtaining ultrasonic signal can be carried out the interlock of PVT-ultrasonic signal, the analysis of transient state like this with embodiment one.
Specific embodiment three
This example directly drives piston motion with linear electric motors or oil motor by connecting link.
As shown in Figure 7, this contrive equipment is made up of lower installation board 1, support 2, upper mounting plate 3, linear electric motors or oil motor 4, driving fixed mount 5, No. 6 demarcation of piston rod unit 7, PVT-ultrasound wave letter and ultrasound wave on-line measuring device.Sensor and ultrasonic probe are installed according to Fig. 1,2.
Different with embodiment one and two, linear electric motors or 6 motions of hydraulic cylinder linear drives connecting link, the displacement of energy transient state observing and controlling piston, thus calculate the interior volume of material cavity.According to the pressure and temperature of test, just can draw the PVT curve.The method of obtaining ultrasonic signal can be carried out the interlock of PVT-ultrasonic signal, the analysis of transient state like this with embodiment one.
Description of drawings
Fig. 1 is test philosophy figure used herein
1 installing plate, 2 set bolts, 3 temperature and pressure transducer, 4 tested materials, 5 pistons, 6 piston rods, the heating cylinder of 7 band temperature controls, 8 ultrasonic probes, 9 sealing nuts
Fig. 2 is the mounting arrangement figure of sensor used herein and ultrasonic probe
1 signal sends ultrasonic probe, 2 tested materials, and 3 temperature sensors, 4 signals are accepted ultrasonic probe, the heating cylinder of 5 band temperature controls, 6 pressure transducers
Fig. 3 is a ultrasound wave on-line measuring device pictorial diagram used in the present invention
Fig. 4 is the pictorial diagram of worm drive caliberating device of the present invention
The manual rotating shaft of 1 band tommy bar, the large and small belt wheel or the gear of 2 usefulness belts or chain coupling, the counting scale of 3 band scales, 4 lower end screws connect the leading screw of piston, 5 barrels, 6 heating and cooling systems, 7 ultrasonic probes, 8 support bars, 9 temperature survey tables, 10 pressure measurement tables
Fig. 5 is the legend that concerns of measured polypropylene PVT and ultrasonic velocity
(1) under the different pressures polyacrylic specific volume with variation of temperature
(2) under the different pressures in the polypropylene ultrasonic velocity with variation of temperature
(3) relation of ultrasonic velocity and polypropylene density under the pressure 30MPa
Fig. 6 is the caliberating device synoptic diagram that motor used herein/band or chain transmission drive
1 lower supporting plate, 2 bracing frames, 3PVT-ultrasonic investigation unit, 4 bearing fixed seats, 5 upper backup pads, 6 bearings, 7 big belt wheel or hub of chain wheel, 8 big belt wheel or sprocket wheels, 9 leading screws, 10 belts or chain, 11 install the motor of small pulley or sprocket wheel, 13 motor component mount pads
Fig. 7 directly drives the caliberating device synoptic diagram for linear electric motors used herein or hydraulic cylinder
1 lower supporting plate, 2 bracing frames, 3 upper backup pads, 4 linear electric motors or hydraulic motor system, 5 driver part mount pads, 6 pistons and piston rod, 7PVT-ultrasonic investigation unit
Claims (3)
1. a method and a device that adopts ultrasonic signal to characterize material pressure-specific volume-temperature relation is characterized in that: adopted caliberating device and the ultrasound wave on-line detecting system be made up of the measure portion (displacement measurement dial plate, temperature sensor, pressure transducer, temperature controller and pressure controller, ultrasonic probe system) of the running part of actuation plunger motion, the working portion (material storage tube, plunger, work nut, well heater) that contains measured object and correlated variables.By the method for direct pressurization, record the specific volume under different pressures, the temperature, and according to the different ultrasonic velocities that obtain under the corresponding conditions of ultrasound wave velocity of propagation in different medium.
2. employing ultrasonic signal according to claim 1 characterizes the method and the device of material pressure-specific volume-temperature relation, it is characterized in that: there are one-to-one relationship in ultrasonic velocity and Substance P VT data, and this method is adapted to various polymkeric substance and other fluids, as straight polymer raw material and various modified feedstocks etc.
3. employing ultrasonic signal according to claim 1 characterizes the method and the device of material pressure-specific volume-temperature relation, the PVT characteristic and the ultrasonic signal of direct-on-line test substances flow process, and then study the wherein condensed state problem of complex system.It is characterized in that: the on-tube valve system is directly taken a sample from the runner of equipment such as the extruder of polymer processing, injector on the described material of claim 1 chamber, to take a sample and place this proving installation material chamber to carry out the test of claim 1 and 2, thereby PVT state of material such as characterize polymers and fluid and solid etc.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010128520A CN101799451A (en) | 2010-03-22 | 2010-03-22 | Method and device for representing relation of pressure, specific volume and temperature of substance by ultrasonic signals |
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| CN201010128520A CN101799451A (en) | 2010-03-22 | 2010-03-22 | Method and device for representing relation of pressure, specific volume and temperature of substance by ultrasonic signals |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102589671A (en) * | 2011-01-11 | 2012-07-18 | 中国石油大学(华东) | Sound velocity measurement device for liquid |
| CN102636517A (en) * | 2012-05-17 | 2012-08-15 | 北京化工大学 | Device and method for testing pressure-volume-temperature (PVT) relationship of polymer at high cooling rate |
| CN103006266A (en) * | 2012-12-28 | 2013-04-03 | 汕头市超声仪器研究所有限公司 | Hydraulic ultrasonic probe for elasticity imaging |
| CN103499642A (en) * | 2013-09-25 | 2014-01-08 | 北京化工大学 | Method and device for measuring compression coefficient and expansion coefficient of material on line |
| CN103499514A (en) * | 2013-09-25 | 2014-01-08 | 北京化工大学 | Method and device for testing fluid viscosity on line |
| CN103499639A (en) * | 2013-09-25 | 2014-01-08 | 北京化工大学 | Ultrasonic on-line representing method and device of vulcanizing process |
| CN103512831A (en) * | 2013-07-18 | 2014-01-15 | 北京化工大学 | Method and device for online testing of melt flow index |
| CN106918640A (en) * | 2017-01-18 | 2017-07-04 | 浙江大学 | The ultrasonic in situ characterization apparatus of non-isothermal high shear polymer injection moulding |
| CN108982581A (en) * | 2017-06-02 | 2018-12-11 | 优肯科技股份有限公司 | Measuring equipment for relation between curing degree and specific volume of packaging material |
| CN109521142A (en) * | 2019-01-07 | 2019-03-26 | 大连理工大学 | A kind of device and method for the measurement solid propellant velocity of sound under the conditions of pressure change |
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2010
- 2010-03-22 CN CN201010128520A patent/CN101799451A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102589671A (en) * | 2011-01-11 | 2012-07-18 | 中国石油大学(华东) | Sound velocity measurement device for liquid |
| CN102636517A (en) * | 2012-05-17 | 2012-08-15 | 北京化工大学 | Device and method for testing pressure-volume-temperature (PVT) relationship of polymer at high cooling rate |
| CN102636517B (en) * | 2012-05-17 | 2014-01-01 | 北京化工大学 | Device and method for testing pressure-volume-temperature (PVT) relationship of polymer at high cooling rate |
| CN103006266A (en) * | 2012-12-28 | 2013-04-03 | 汕头市超声仪器研究所有限公司 | Hydraulic ultrasonic probe for elasticity imaging |
| CN103006266B (en) * | 2012-12-28 | 2016-01-13 | 汕头市超声仪器研究所有限公司 | For the hydraulic ultrasonic probe of elastogram |
| CN103512831A (en) * | 2013-07-18 | 2014-01-15 | 北京化工大学 | Method and device for online testing of melt flow index |
| CN103499639A (en) * | 2013-09-25 | 2014-01-08 | 北京化工大学 | Ultrasonic on-line representing method and device of vulcanizing process |
| CN103499514A (en) * | 2013-09-25 | 2014-01-08 | 北京化工大学 | Method and device for testing fluid viscosity on line |
| CN103499642A (en) * | 2013-09-25 | 2014-01-08 | 北京化工大学 | Method and device for measuring compression coefficient and expansion coefficient of material on line |
| CN103499639B (en) * | 2013-09-25 | 2019-05-31 | 北京化工大学 | A kind of online characterizing method of sulfidation ultrasonic wave |
| CN106918640A (en) * | 2017-01-18 | 2017-07-04 | 浙江大学 | The ultrasonic in situ characterization apparatus of non-isothermal high shear polymer injection moulding |
| CN106918640B (en) * | 2017-01-18 | 2019-11-12 | 浙江大学 | The ultrasonic in situ characterization apparatus of non-isothermal high shear polymer injection moulding |
| CN108982581A (en) * | 2017-06-02 | 2018-12-11 | 优肯科技股份有限公司 | Measuring equipment for relation between curing degree and specific volume of packaging material |
| CN109521142A (en) * | 2019-01-07 | 2019-03-26 | 大连理工大学 | A kind of device and method for the measurement solid propellant velocity of sound under the conditions of pressure change |
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Application publication date: 20100811 |