CN104833613A - Capillary tube orifice mold and method for measuring rheological characteristics of polymer under ultrasonic vibration condition - Google Patents
Capillary tube orifice mold and method for measuring rheological characteristics of polymer under ultrasonic vibration condition Download PDFInfo
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Abstract
The invention discloses a capillary tube orifice mold and a method for measuring rheological characteristics of a polymer under an ultrasonic vibration condition. The capillary tube orifice mold comprises an ultrasonic generator, an amplitude-change pole, a transducer, a fixing ring, a heating coil, a charging barrel, a capillary tube, a control device and the like, wherein the fixing ring is fixedly arranged at the upper part of a support rod; a seal ring is fixedly arranged at the lower part of the support rod to form a fixing frame; the fixing frame is fixedly arranged at the top of the charging barrel; a heat insulating layer is assembled on the contact surface of the charging barrel and the seal ring; the heating coil sleeves the outer side of the charging barrel; the amplitude-change pole penetrates through the fixing ring and the seal ring and extends out of the charging barrel; the transducer is connected with the amplitude-change pole; the transducer is connected with the ultrasonic generator through a lead; a radiator sleeves the amplitude-change pole; the seal ring sleeves the contact surface of the amplitude-change pole and the seal ring; the capillary tube is assembled in the charging barrel; and the signal output ends of a charging barrel temperature sensor, a melt pressure sensor and a melt temperature sensor arranged in the charging barrel are connected with the control device. According to the capillary tube orifice mold, the apparent viscosity of the polymer under ultrasonic vibration with different frequencies and power can be measured.
Description
Technical field
The present invention is a kind of capillary die and method of measuring polymeric rheology characteristic under ultrasonic vibration condition, belongs to and measures the capillary die of polymeric rheology characteristic and the innovative technology of method under ultrasonic vibration condition.
Background technology
Since nineteen fifties, when finding to utilize static ultrasound process polymer melt, rheological effect has occurred, ultrasonic assistant expressing technique has been used to the viscosity reducing polymkeric substance, thus improves the processing characteristics of polymkeric substance.In the past few decades, extensive research application high-power ultrasonic process polymer melt, has facilitated several application: the devulcanization of ultrasonic wave added expressing technique and static ultrasound ripple process polymer melt rubber; Strengthen the blended compatibilization of incompatible polymer; Recently for the preparation of the nano composite material of polymkeric substance.
Ultrasound wave is in the maximally related application of Polymer Processing.First, for improving the processing characteristics of polymkeric substance, as improved the mobility of polymkeric substance, especially improve the surfaceness of extrusion profile.In order to reduce polymkeric substance in extrusion molding, or the viscosity when injection moulding, research relates to and add ultrasonic vibration in mechanized equipment, mould mostly, thus promotes the decline of polymer flowability, and improves the appearance of extrudate.Secondly, for devulcanization of rubber effect.From the nineties in 20th century, toppling over plastic garbage has become a serious environmental problem.Under this background, ultrasonic technology is used to process rubber-based waste material (as doughnut, hose) that is natural or synthesis, and plastic garbage is recycled by ultrasound wave sulfur removal technology, can replace traditional practice of dumping rubbish.The sulfur removal technology that one does not relate to the Continuous maching rubber of chemical substance treatment is have studied Isayev first time in 1993.This technique is by using high-power ultrasonic to destroy the elastic body of sulfuration and the chemical bond of other thermoset plastic polymers, and such plastic garbage just can be reprocessed by the way as undressed rubber, then through over cure, reshaping.Recently, ultrasound wave is for the preparation of polymer blend and polymer nanocomposites.Large power supersonic is used for polymer blending, filling material is disperseed equably in thermoplastics, promotes that coblended interface produces chemical reaction, improve the compatibility between two incompatible polymers, with compared with ultrasonic process, the mechanical property of these polymkeric substance can be improved.
Along with new material, the development of new technology, ultrasound wave is widely used in polymer processing field, but also quite lacks for measuring the instrument of polymeric rheology performance under ul-trasonic irradiation.At present, capillary type flow graph, rotor-type flow graph, mixing type torque rheometer, oscillation mode flow graph that the instrument of polymeric rheology characteristic is main or traditional is measured.Except oscillation mode flow graph has except the feature of vibration, other several features all not having vibration, but oscillation mode flow graph also cannot characterize the rheology characteristic of ultrasonic vibration.Because the development of capillary type flow graph is the most ripe, the most typical, simple to operate, measure accurately, measurement range is wide, can not only measure the shear viscosity of material, can also by the research to extrusion, the elastic behavior of material is discussed, thus on the basis of capillary type flow graph, add ultrasound wave vibration, develop a kind of capillary rheometer being suitable for the measurement polymeric rheology characteristic of ultrasound wave vibration, there is engineering practical value widely.
Summary of the invention
The object of the invention is to consider the problems referred to above and a kind of capillary die measuring polymeric rheology characteristic under ultrasonic vibration condition is provided.The present invention can measure under the ultrasonic vibration of different frequency and different capacity, the apparent viscosity of polymkeric substance.
Another object of the present invention is to provide a kind of method measuring polymeric rheology characteristic under ultrasonic vibration condition.The present invention is simple to operate, and measuring accuracy is high, convenient and practical.The present invention, by the research of extrusion under the ultrasonic vibration effect to different frequency and different capacity, discusses the elastic behavior after ultrasound wave vibration of material.
Technical scheme of the present invention is: the capillary die of polymeric rheology characteristic under measurement ultrasonic vibration condition of the present invention, includes ultrasonic generator, ultrasonic transformer, transducer, set collar, support bar, heating radiator, O-ring seal, sealing ring, heat insulation layer, heater coil, barrel, kapillary, barrel temperature sensor, melt force sensor, melt temperature sensor, control device, set collar is fixed on the top of support bar, fixed mount is formed at the bottom that sealing ring is fixed on support bar, fixed mount is fixed on the top of barrel, heat insulation layer is installed on the surface of contact of barrel and sealing ring, heater coil is sleeved on the outside of barrel, ultrasonic transformer stretches out in barrel through set collar and sealing ring, and transducer is fixed on fixed mount, and transducer is connected with ultrasonic transformer, and transducer is connected with ultrasonic generator by wire, form ultrasonic wave oscillation portion, radiator muff-joint is on ultrasonic transformer, and O-ring seal is enclosed within the surface of contact between ultrasonic transformer and sealing ring, kapillary is installed in barrel, barrel temperature sensor, melt force sensor, melt temperature sensor is installed in barrel, barrel temperature sensor, melt force sensor, the signal output part of melt temperature sensor is connected with control device.
The present invention measures the measuring method of the capillary die of polymeric rheology characteristic under ultrasonic vibration condition, comprises the steps:
1) ultrasound wave vibration-rheological mouth mould is contained on torque rheometer by torque rheometer interface group forms vertical ultrasonic-wave Vibration Torque flow graph;
2) control device is according to the temperature of material requirement setting barrel, and by heater coil to equipment preheating;
3) material reaches design temperature, and by the screw extrusion apparatus of torque rheometer material melts, melt is squeezed into ultrasound wave vibration-rheological instrument mouth mould by the position of torque rheometer interface, and by Capillary Flow out;
4) torque rheometer screw speed is set by control device, that is to say the shear rate to material, open ultrasonic generator simultaneously, setting ultrasonic power and frequency;
5) monitor capillary die by control device, when temperature, pressure, shear rate tend towards stability, get the material that the unit interval flows out from kapillary, and weigh up its weight, the flow of unit interval can be drawn;
6) repeat the 4th and the 5th step, gather different data;
7) analyzing and processing is carried out to data, thus draw the rheological characteristics of polymer melt.
The present invention is in order to solve the measurement problem of the rheological characteristics of polymkeric substance under ultrasound wave effect of vibration, design a kind of capillary die measuring the lower polymeric rheology characteristic of ultrasound wave vibration, by to the adjustment to ultrasonic frequency and power of ultrasonic generator and control device thereof, and to the isoparametric mensuration of temperature, pressure and flow, reach the object obtaining polymeric rheology characteristic under different frequency and different capacity ultrasonic vibration.The present invention designs ingenious, function admirable, convenient and practical.It is simple to operate that the present invention measures the method for polymeric rheology characteristic under ultrasonic vibration condition, can measure under the ultrasonic vibration of different frequency and different capacity, the apparent viscosity of polymkeric substance.The present invention by the research of extrusion under the ultrasonic vibration effect to different frequency and different capacity, can also discuss the elastic behavior after ultrasound wave vibration of material.
Accompanying drawing explanation
Fig. 1 is the structural representation of the axial section of vertical ultrasonic-wave vibration-rheological mouth mould of the present invention;
Fig. 2 is the schematic layout pattern of ultrasonic generator of the present invention and control device;
Fig. 3 is the T-T sectional view in Fig. 1;
Fig. 4 is the structural representation of the axial section of horizontal ultrasound wave vibration-rheological mouth mould of the present invention;
Fig. 5 is the T-T sectional view in Fig. 4.
Embodiment
Embodiment:
As shown in Figure 1, under measurement ultrasonic vibration condition of the present invention, the capillary die of polymeric rheology characteristic, includes ultrasonic generator 1 to structural representation of the present invention, ultrasonic transformer 2, transducer 3, set collar 4, support bar 5, heating radiator 6, O-ring seal 7, sealing ring 8, heat insulation layer 9, heater coil 10, barrel 11, kapillary 12, barrel temperature sensor 13, melt force sensor 14, melt temperature sensor 16, control device 17, set collar 4 is fixed on the top of support bar 5, fixed mount is formed at the bottom that sealing ring 8 is fixed on support bar 5, fixed mount is fixed on the top of barrel 11, heat insulation layer 9 is installed in barrel 11 with on the surface of contact of sealing ring 8, heater coil 10 is sleeved on the outside of barrel 11, ultrasonic transformer 2 stretches out in barrel 11 through set collar 4 and sealing ring 8, and transducer 3 is fixed on fixed mount, transducer 3 is connected with ultrasonic transformer 2, and transducer 3 is connected with ultrasonic generator 1 by wire, form ultrasonic wave oscillation portion, heating radiator 6 is enclosed within ultrasonic transformer 2, and O-ring seal 7 is enclosed within the surface of contact between ultrasonic transformer 2 and sealing ring 8, kapillary 12 is installed in barrel 11, barrel temperature sensor 13, melt force sensor 14, melt temperature sensor 16 is installed in barrel 11, barrel temperature sensor 13, melt force sensor 14, the signal output part of melt temperature sensor 16 is connected with control device 17.
Above-mentioned barrel temperature sensor 13, melt force sensor 14, melt temperature sensor 16 are installed in barrel 11 and mutually vertically become in the threaded hole of an angle of 90 degrees.Leave certain gap between above-mentioned ultrasonic transformer 2 and sealing ring 8, avoid ultrasonic transformer 2 and Metal Contact, thus protection ultrasonic transformer, and guarantee that ultrasonic unit normally works.Meanwhile, be conducive to O-ring seal 7 to seal it.
The axis of above-mentioned ultrasonic transformer 2, transducer 3 and the axis coaxle of kapillary 12, form vertical ultrasonic-wave vibration-rheological mouth mould, barrel 11 is provided with torque rheometer interface 15-1, the external torque rheometer of torque rheometer interface 15-1 or extruder.As shown in Figure 1,3.
In addition, the axis of above-mentioned ultrasonic transformer 2, transducer 3 can also make the axes normal with kapillary 12, forms horizontal ultrasound wave vibration-rheological mouth mould, the axle center of barrel 11 is equiped with plunger 15-2.As shown in Figure 4,5.Horizontal ultrasound wave vibration-rheological mouth mould is similar to vertical ultrasonic-wave vibration-rheological mouth mould, and only horizontal ultrasound wave vibration-rheological mouth mould is assembled by plunger 15-2 and traditional capillary type flow graph, forms horizontal ultrasound wave vibration-rheological instrument.And vertical ultrasonic-wave vibration-rheological mouth mould forms vertical ultrasonic-wave Vibration Torque flow graph in the external extruder of torque rheometer interface 15-1, torque rheometer assembling.In addition, this flow graph also by controlling the speed of feed U of plunger 15-1, can be used alone.
Above-mentioned ultrasonic transformer 2 forms ultrasonic vibrator with transducer 3, and heat insulation layer 9 can greatly reduce hot-fluid to ultrasonic vibrator transmission.Meanwhile, heating radiator 6 on ultrasonic transformer 2 overlaps, heating radiator 6 water flowing is carried out carrying out water-cooling to ultrasonic transformer 2.Guarantee that ultrasonic vibrator works under normal working temperature.When ultrasonic vibrator exceeds critical temperature, ultrasonic generator automatic alarm, and stop sending out ripple.
Barrel temperature monitored by above-mentioned barrel temperature sensor 13; Melt force sensor 14 monitors melt pressure, melt temperature sensor 16 monitors melt temperature.Temperature sensor and pressure transducer are all adopt thin thread connected mode to be tightened against barrel 11.
Kapillary 12 adopts thin thread connected mode to be tightened against barrel 11, and the length-diameter ratio that replaceable one-tenth is different, thus Bagley correction is carried out to pressure gradient.
In the present embodiment, above-mentioned control device 17 is computing machines.
In the present embodiment, above-mentioned ultrasonic transformer 2 is connected with transducer 3 by screw thread.
In the present embodiment, above-mentioned transducer 3 is fixed on fixed mount with hexagon socket head cap screw.
The axis of above-mentioned ultrasonic transformer 2, transducer 3 and the axis coaxle of kapillary 12 in the present embodiment, form vertical ultrasonic-wave vibration-rheological mouth mould.
In the present embodiment, above-mentioned fixed mount is screwed on barrel 11.
Be fixed on the top of support bar 5 in the present embodiment with hexagon socket head cap screw in above-mentioned set collar 4, fixed mount is formed at sealing ring 8 bottom that hexagon socket head cap screw is fixed on support bar 5.
The measuring method of vertical ultrasonic-wave vibration-rheological mouth mould of the present invention, comprises the steps:
1) as shown in Figure 1, 2, 3, ultrasound wave vibration-rheological mouth mould is assembled on torque rheometer by the helicitic texture that torque rheometer interface 15-1 makes forms vertical ultrasonic-wave Vibration Torque flow graph;
2) control device is according to the temperature of material requirement setting barrel 11, and by heater coil 10 pairs of equipment preheatings;
3) material reaches design temperature, and by the screw extrusion apparatus of torque rheometer material melts, melt is squeezed into ultrasound wave vibration-rheological instrument mouth mould by the position at torque rheometer interface 15-1 place, and flows out by kapillary 12;
4) torque rheometer screw speed is set by control device, that is to say the shear rate to material, open ultrasonic generator 1 simultaneously, setting ultrasonic power and frequency;
5) monitor capillary die by control device, when temperature, pressure, shear rate tend towards stability, get the material that the unit interval flows out from kapillary 12, and weigh up its weight, the flow of unit interval can be drawn;
6) repeat the 4th and the 5th step, gather different data;
7) analyzing and processing is carried out to data, thus draw the rheological characteristics of polymer melt.
This flow graph ultrasonic generator is all adjustable in certain limit with its control device ultrasonic frequency, power and amplitude.
The measuring method of the present invention's horizontal ultrasound wave vibration-rheological mouth mould, as shown in Figure 4, by the control of control device 17, according to material requirement setting barrel temperature, and to the equipment preheating regular hour, then material is loaded barrel, compacting be incubated the regular hour.Then the speed U(constant speed of plunger 15-2 is controlled) make it to travel forward, melt extrusion kapillary.In addition, other steps are substantially the same with the measuring method of vertical ultrasonic-wave vibration-rheological mouth mould.
The present invention by the adjustment to ultrasonic frequency and power of ultrasonic generator and control device thereof, and to the isoparametric mensuration of temperature, pressure and flow, reaches the object obtaining polymeric rheology characteristic under different frequency and different capacity ultrasonic vibration.The present invention can measure under the ultrasonic vibration of different frequency and different capacity, the apparent viscosity of polymkeric substance.
Claims (10)
1. measure a capillary die for polymeric rheology characteristic under ultrasonic vibration condition, it is characterized in that including ultrasonic generator, ultrasonic transformer, transducer, set collar, support bar, heating radiator, O-ring seal, sealing ring, heat insulation layer, heater coil, barrel, kapillary, barrel temperature sensor, melt force sensor, melt temperature sensor, control device, set collar is fixed on the top of support bar, fixed mount is formed at the bottom that sealing ring is fixed on support bar, fixed mount is fixed on the top of barrel, heat insulation layer is installed on the surface of contact of barrel and sealing ring, heater coil is sleeved on the outside of barrel, ultrasonic transformer stretches out in barrel through set collar and sealing ring, and transducer is fixed on fixed mount, and transducer is connected with ultrasonic transformer, and transducer is connected with ultrasonic generator by wire, form ultrasonic wave oscillation portion, radiator muff-joint is on ultrasonic transformer, and O-ring seal is enclosed within the surface of contact between ultrasonic transformer and sealing ring, kapillary is installed in barrel, barrel temperature sensor, melt force sensor, melt temperature sensor is installed in barrel, barrel temperature sensor, melt force sensor, the signal output part of melt temperature sensor is connected with control device.
2. the capillary die of polymeric rheology characteristic under measurement ultrasonic vibration condition according to claim 1, is characterized in that above-mentioned barrel temperature sensor, melt force sensor, melt temperature sensor are installed in barrel and mutually vertically become in the threaded hole of an angle of 90 degrees.
3. the capillary die of polymeric rheology characteristic under measurement ultrasonic vibration condition according to claim 1, it is characterized in that the axis of above-mentioned ultrasonic transformer, transducer and the axis coaxle of kapillary, form vertical ultrasonic-wave vibration-rheological mouth mould, barrel is provided with torque rheometer interface, and torque rheometer interface can external torque rheometer or extruder.
4. the capillary die of polymeric rheology characteristic under measurement ultrasonic vibration condition according to claim 1, it is characterized in that the axis of above-mentioned ultrasonic transformer, transducer and the axes normal of kapillary, form horizontal ultrasound wave vibration-rheological mouth mould, the axle center of barrel is equiped with plunger.
5. under the measurement ultrasonic vibration condition according to any one of Claims 1-4, the capillary die of polymeric rheology characteristic, is characterized in that above-mentioned control device is computing machine.
6. the capillary die of polymeric rheology characteristic under measurement ultrasonic vibration condition according to claim 5, is characterized in that above-mentioned ultrasonic transformer is connected with transducer 3 by screw thread.
7. the capillary die of polymeric rheology characteristic under measurement ultrasonic vibration condition according to claim 6, is characterized in that above-mentioned transducer hexagon socket head cap screw is fixed on fixed mount.
8. the capillary die of polymeric rheology characteristic under measurement ultrasonic vibration condition according to claim 7, is characterized in that above-mentioned fixed mount is screwed on barrel.
9. the capillary die of polymeric rheology characteristic under measurement ultrasonic vibration condition according to claim 5, it is characterized in that above-mentioned set collar hexagon socket head cap screw is fixed on the top of support bar 5, fixed mount is formed at the bottom that sealing ring hexagon socket head cap screw is fixed on support bar.
10. measure a measuring method for the capillary die of polymeric rheology characteristic under ultrasonic vibration condition, it is characterized in that comprising the steps:
1) ultrasound wave vibration-rheological mouth mould is contained on torque rheometer by torque rheometer interface group forms vertical ultrasonic-wave Vibration Torque flow graph;
2) control device is according to the temperature of material requirement setting barrel, and by heater coil to equipment preheating;
3) material reaches design temperature, and by the screw extrusion apparatus of torque rheometer material melts, melt is squeezed into ultrasound wave vibration-rheological instrument mouth mould by the position of torque rheometer interface, and by Capillary Flow out;
4) torque rheometer screw speed is set by control device, that is to say the shear rate to material, open ultrasonic generator simultaneously, setting ultrasonic power and frequency;
5) monitor capillary die by control device, when temperature, pressure, shear rate tend towards stability, get the material that the unit interval flows out from kapillary, and weigh up its weight, the flow of unit interval can be drawn;
6) repeat the 4th and the 5th step, gather different data;
7) analyzing and processing is carried out to data, thus draw the rheological characteristics of polymer melt.
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Cited By (6)
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| CN105547920A (en) * | 2015-12-10 | 2016-05-04 | 北京理工大学 | Right-angle type mould used for torque rheological testing |
| CN105928829A (en) * | 2016-04-29 | 2016-09-07 | 西南石油大学 | Experiment device for monitoring high-speed shearing stability of polymer molecule on line |
| CN106092823A (en) * | 2016-07-27 | 2016-11-09 | 西南石油大学 | A kind of continuous assessment high-temperature, high pressure fluid viscosity and the experimental provision of shear stability |
| WO2019184403A1 (en) * | 2018-03-30 | 2019-10-03 | 四川大学 | Rotating extrusion rheometer and rheology measurement method capable of simultaneously measuring polymer pressure/shearing rheology |
| CN110595947A (en) * | 2019-08-14 | 2019-12-20 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | Method for testing vibration rheological property of cement mortar |
| CN114633448A (en) * | 2022-03-16 | 2022-06-17 | 浙江大学 | Testing machine with wide-frequency amplitude vibration test/rheological measurement integrated function |
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| CN110595947A (en) * | 2019-08-14 | 2019-12-20 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | Method for testing vibration rheological property of cement mortar |
| CN114633448A (en) * | 2022-03-16 | 2022-06-17 | 浙江大学 | Testing machine with wide-frequency amplitude vibration test/rheological measurement integrated function |
| CN114633448B (en) * | 2022-03-16 | 2022-11-08 | 浙江大学 | Testing machine with wide-frequency amplitude vibration test/rheological measurement integrated function |
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