CN1773289A - Double-isopressing device and application thereof - Google Patents

Double-isopressing device and application thereof Download PDF

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Publication number
CN1773289A
CN1773289A CN 200510061501 CN200510061501A CN1773289A CN 1773289 A CN1773289 A CN 1773289A CN 200510061501 CN200510061501 CN 200510061501 CN 200510061501 A CN200510061501 A CN 200510061501A CN 1773289 A CN1773289 A CN 1773289A
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pressure vessel
double
isostatic pressure
pressure
isostatic
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CN 200510061501
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CN100570367C (en
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郑强
周剑锋
宋义虎
朱姝
徐文武
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The present invention relates to a double - isostatic pressing equipment and its application. Said double isostatic pressing equipment includes external isostatic pressing container and internal isostatic pressing container. The external isotatic container is a closed containing cavity in which an electroheating device and a support are set, the heating cable of electroheating device is led out from containing cavity and is connected with a temperature control instrument, on the support an internal isostatic pressing container and a CCD camera head are fixed. On the external isostatic pressing container an air intake valve and an exhaust valve are set, and a pressure sensor, a temperature sensor and a displacement sensor also are fixed. The signal lines of pressure sensor, temperature sensor, displacement sensor and CCD camera head are led out from said closed containing cavity, and connected with computer. The internal isostatic pressing container is a transparent one with air inlet, air outlet and slide piece. Said invention also provides its application range.

Description

Double-isopressing device and application thereof
Technical field
The present invention relates to a kind of double-isopressing device and application thereof, in particular for the double-isopressing device of research pressure to the influence of physics or chemical equilibrium, transition process.
Background technology
Pressure is the important state function of all substances, also is the condition and the restraining factors of many reactions of nature and transition process.Reaction of all or transformation all are an equilibrium process in essence, and pressure often makes this balance carry out to the different directions development or with different rates.For some reactions gas-phase reaction different with the product gas molal quantity, often make reaction carry out, and the influence of investigating pressure factor can obtain such as important parameters such as the equilibrium constant, the orders of reaction conversely to the direction that helps generating product by increasing or reducing pressure.Occur in the reaction or the transformation of liquid phase and solid phase fully for some, pressure also can be by exerting one's influence to the effect of infiltration, vapour pressure etc.The influence of research pressure factor almost all has important theory and is worth and engineering significance in any field.But reaction under the high pressure and transformation need be carried out in special high-pressure-resistant vessel usually, and these containers are opaque substantially, this has brought 2 inconvenience at least concerning the researcher: at first be the different reaction needed different materials and the pressure vessel of shape, improved research cost; Next is to observe directly the influence of pressure to some reaction conversion ratio, equilibrium products.
On the other hand, develop in the isostatic pressing technology of field of powder metallurgy and obtained widespread use in fields such as material bonding, powder metallurgy, powder moulding, foundry goods processing.But because common isopressing device often has apparatus expensive, bulky, the isostatic pressing technology particularly popularization of hot isostatic pressing technique still is very limited.Up to the present, even if isostatic pressing technology has application in fields such as chemistry, chemical industry idol, also some simple powder moulding aspects that are confined to seem not enough in the exploration aspect a kind of strong scientific research instrument more, and the thinking of developing its commercial Application simultaneously is still open inadequately.Material universal testing machine, vulcanizing press or high pressure gas storage cylinder etc. are the common equipments of material and chemical engineering experiment chamber, in conjunction with these common tools, often make isostatic pressing technology be able to simple realization.
Summary of the invention
The purpose of this invention is to provide a kind of double-isopressing device.
Another object of the present invention provides apparatus of the present invention is used to study the application process of pressure to the influence of physics or chemical equilibrium, transition process.
Double-isopressing device of the present invention, comprise outer isostatic pressure vessel and interior isostatic pressure vessel, outer isostatic pressure vessel is an airtight cavity volume, be provided with electric heater unit and support in the cavity volume, the heating cable of electric heater unit is drawn cavity volume and is linked to each other with temperature controller, isostatic pressure vessel and CCD camera in being fixed with on the support, isostatic pressure vessel is provided with air intake valve and drain tap outside, and be fixed with pressure transducer, temperature sensor and displacement transducer, pressure transducer, temperature sensor, displacement transducer is drawn airtight cavity volume with the signal wire of CCD camera and is linked to each other with computing machine, interior isostatic pressure vessel is to have into, the transparent vessel of gas outlet and saddle advances, the gas outlet is furnished with stopper.
Apparatus of the present invention are used to study pressure to physics or chemical equilibrium, during the influencing of transition process, to treat that research system puts into isostatic pressure vessel, the physics of initiator system or chemical equilibrium, transition process, stuffing pressure medium in the outside isostatic pressure vessel, it generally is air, gas mediums such as nitrogen, by the material universal testing machine or high-pressure cylinder provides and controlled pressure, by temperature controller and electric heater unit control medium temperature, saddle in the interior isostatic pressure vessel moves freely with the external and internal pressure difference, keep the container internal and external pressure balance, write down the pressure, temperature variation of balance or transition process generation respectively by the pressure and temperature sensor, come the volume change of following response system by the displacement of displacement transducer record saddle, balance or transformation situation in the isostatic pressure vessel in observing by the CCD camera.The output signal of pressure transducer, temperature sensor, displacement transducer and CCD camera is sent to the computer measurement terminal, realized various physics, chemical equilibrium transition process (conversion ratio, the equilibrium constant, the order of reaction that comprise gas-phase reaction, sol-gel transition, swelling equilibrium, change mutually and balance, press to cause seepage flow transformation etc.) the dependent research of pressure.
The present invention is transferred to the transformation under the high pressure or equilibrium process in the normal pressure transparent vessel by double-isopressing device and method and carries out, and has reduced the requirement to high-pressure reaction vessel intensity, thickness, shape and sealing, has reduced research cost; Realized the measurement of small volume change under the pressure condition and the observation directly perceived and the analysis of following reaction of mesohigh or transition process.The present invention can be used for studying the influence of pressure to all kinds of physics or chemical equilibrium, transition process, comprises conversion ratio, the equilibrium constant, the order of reaction of gas-phase reaction, sol-gel transition, and swelling equilibrium changes and balance etc. mutually.
Description of drawings
Fig. 1 is a kind of structural representation of double-isopressing device of the present invention;
Fig. 2 is the another kind of structural representation of double-isopressing device of the present invention;
Fig. 3 is a kind of structural representation of interior isostatic pressure vessel;
Fig. 4 is a kind of structural representation of interior isostatic pressure vessel.
Embodiment
With reference to Fig. 1, Fig. 2, double-isopressing device of the present invention comprises outer isostatic pressure vessel 1 and interior isostatic pressure vessel 10, outer isostatic pressure vessel 1 is an airtight cavity volume, this airtight cavity volume can be as shown in Figure 1, constitute by housing and piston 2, on the surface of contact of piston 2 and inner walls, establish seal 3, perhaps also can be as shown in Figure 2, constitute by housing and top cover 18, establish seal 3 on the surface of contact of top cover and inner walls, seal 3 can be made up of the O RunddichtringO and the sustained ring that are embedded in piston 2 or top cover 18 circumferential slots.In example illustrated in figures 1 and 2, the housing of outer isostatic pressure vessel is formed by base 6 and weldless steel tube thread connection, and RUBBER O RunddichtringO 14 is set on surface of contact, is surrounded by collet 4 outside housing, with control heat radiation and stabilising arrangement temperature.Be provided with electric heater unit 8 and support 9 outside in the cavity volume of isostatic pressure vessel, the heating cable of electric heater unit 8 is drawn cavity volume and is linked to each other with temperature controller 7, isostatic pressure vessel 10 and CCD camera 11 in being fixed with on the support 9, isostatic pressure vessel is provided with air intake valve 12 and drain tap 16 outside, and being fixed with pressure transducer 5, temperature sensor 15 and displacement transducer 13, pressure transducer 5, temperature sensor 1J5, displacement transducer 13 and the signal wire of CCD camera 11 are drawn airtight cavity volume and are linked to each other with computing machine.Interior isostatic pressure vessel 10 can be as shown in Figure 3, be that top is that a kapillary 20, bottom are the transparent vessel of sample chamber, the sample chamber is connected by ground with kapillary, on the sample chamber, be provided with the air intake opening 22 and the gas outlet 23 of band stopper, be provided with saddle 19 in the kapillary and prevent that saddle from slipping into the back-up ring 21 of sample chamber, here, saddle can be the slider of polytetrafluoroethylmaterial material.Perhaps interior isostatic pressure vessel 10 can be a transparent cylinder barrel as shown in Figure 4 also, is provided with saddle 19 in the cylinder barrel, and here, saddle is a piston, and the air intake opening 22 and the gas outlet 23 of band stopper is set on piston, is provided with back-up ring 21 in cylinder barrel.
When apparatus of the present invention are used to study pressure to the influencing of physics or chemical equilibrium, transition process, for double-isopressing device shown in Figure 1, move by material universal testing machine control piston, change pressure medium in the airtight cavity volume, the displacement transducer data are the algebraic sum of saddle displacement in piston displacement and the interior isostatic pressure vessel; For double-isopressing device shown in Figure 2, charge into the gas of different pressures by the high pressure gas cylinder by the air intake valve of outer isostatic pressure vessel, directly regulate pressure medium in the airtight cavity volume, saddle displacement in the isostatic pressure vessel in the displacement transducer data recording.
Embodiment 1: research pressure is for the equilibrium conversion of the influence, particularly gas-phase reaction of physics and chemical equilibrium process and the equilibrium constant etc.
During test, original air in the isostatic pressure vessel in the emptying, under normal pressure, charge into and wait to study the gas-phase reaction system, by heating or initiating agent initiation reaction, saddle in the interior isostatic pressure vessel moves freely with reaction, follow the tracks of reaction by range estimation saddle position change and carry out degree, until arriving balance.Can calculate the reaction conversion ratio and the equilibrium constant under the normal pressure by volume change.Then interior isostatic pressure vessel is put on the support in the outer isostatic pressure vessel, outwards charges into the nitrogen of certain precompression in the isostatic pressure vessel, control the required pressure and temperature condition of reaction indirectly by nitrogen.Provide and controlled pressure by material universal testing machine or high pressure gas cylinder, by temperature controller and electric heater unit control nitrogen temperature, saddle in the interior isostatic pressure vessel moves freely with the external and internal pressure difference, keep the container internal and external pressure balance, write down the pressure, temperature variation of balance or transition process generation respectively by the pressure and temperature sensor, it is constant to keep-up pressure after reaching predetermined pressure, come the volume change of following response system by the displacement of displacement transducer record saddle, observe balance or transformation situation in the interior isostatic pressure vessel, pressure transducer by the CCD camera, temperature sensor, the output signal of displacement transducer and CCD camera is sent to the computer measurement terminal.By recording the reaction conversion ratio and the equilibrium constant under the different pressures, investigate the influence of pressure to the equilibrium conversion and the equilibrium constant.By the environment temperature (nitrogen temperature) of conditioned reaction system, the equilibrium constant under the calculating different temperatures and the energy of activation of balanced reaction.
Embodiment 2: research pressure is to the influence of the gas-phase reaction equilibrium constant and conversion ratio.
During test, after there is air in isostatic pressure vessel Central Plains in the logical nitrogen emptying, to be evacuated in the interior isostatic pressure vessel from the gas outlet of sample chamber or cylinder barrel, saddle will rest on the back-up ring place, inject reacting gas fast and close inlet, outlet from air intake opening then by stopper, this moment displacement transducer record the saddle position promptly corresponding to the initial volume of reactant.Reaction is carried out under normal pressure earlier, by the reaction process and the volume change of range estimation and displacement transducer reading variation tracking system, until arriving balance.Can calculate the reaction conversion ratio and the equilibrium constant under the normal pressure by volume change.Then interior isostatic pressure vessel is put on the support in the outer isostatic pressure vessel, outwards charge into the nitrogen of certain precompression and regulate its pressure in the isostatic pressure vessel by material universal testing machine or high pressure gas cylinder, pressure transducer record pressure changes, by temperature control instrument control electric heater unit nitrogen is heated, and by temperature sensor feedback temperature signal, come the volume change of following response system by the displacement of displacement transducer record saddle, observe balance or transformation situation in the interior isostatic pressure vessel, pressure transducer by the CCD camera, temperature sensor, the output signal of displacement transducer and CCD camera is sent to the computer measurement terminal.By measuring the variation of system cumulative volume under the different pressures, calculating pressure is to the influence of the equilibrium conversion and the equilibrium constant.By the environment temperature (nitrogen temperature) of conditioned reaction system, the equilibrium constant under the calculating different temperatures and the energy of activation of balanced reaction.Present embodiment is applicable to reaction or the transition process faster slightly than embodiment 1.
Embodiment 3: research gas-phase reaction dynamics and pressure are to the influence of reaction kinetics.
During test, earlier interior isostatic pressure vessel is put on the support in the outer isostatic pressure vessel, respectively the air intake opening and the gas outlet of interior isostatic pressure vessel are communicated with the air intake valve and the drain tap of outer isostatic pressure vessel with two sections flexible pipes, interior isostatic pressure vessel and two sections flexible pipes serve as reaction vessel jointly, fill solid foam in the airtight cavity volume of isostatic pressure vessel outside, in airtight cavity volume, charge into the nitrogen of certain precompression, make the free space in the cavity volume be compressed to very little, moving up and down of saddle can significantly change nitrogen pressure in the outer isostatic pressure vessel in the interior isostatic pressure vessel thereby make, and limits being moved further of saddle conversely.From the drain tap of outer isostatic pressure vessel interior isostatic pressure vessel is evacuated, injects reacting gas fast from air intake valve then.Rapid valve-off, initiation reaction, the time dependent signal of reaction system general pressure of pressure transducer output, the time dependent signal of temperature of reaction system of temperature sensor output, the saddle displacement high low signal of displacement transducer output and the picture signal of CCD camera output are sent to the computer measurement terminal, and ask the calculation order of reaction and reaction rate constant by partial pressure.For the situation that original pressure is difficult to determine, can adopt Gu Jinhaimu (Guggenheim) method to handle.By the pressure and temperature condition that conditioned reactions such as material universal testing machine, high pressure gas cylinder and electric heater unit take place, calculate the order of reaction and rate constant under the different situations, investigate pressure and temperature to the gas-phase reaction effect of kinetics.
Embodiment 4: research pressure is for the influence of all kinds of physical conversion and equilibrium process.
(1) change mutually: supposition has the volume that gas-liquid limited under the situation of gas phase existence changes can not influence liquid phase, then can use the influence of double-isopressing device real-time tracing pressure to gas-liquid equilibrium.For the solid-solid phase equilibrium process that takes place at a certain temperature, influence balances each other thereby also available double-isopressing device changes environmental pressure, by the CCD first-class means of making a video recording new phase is observed and is analyzed then.
(2) sol-gel transition: pressure factor can impact some sol-gel transition process.Adopt after the means such as dyeing and can also be in double-isopressing device to investigate with the CCD first-class means of making a video recording.
(3) crystalline phase, transformation of configuration:, may state variation or configuration change take place with external factor such as temperature, pressure for some macromolecular material; Pressure (particularly high pressure) also may cause the crystal formation of some crystalline plastic to change, even generates new crystalline state, and some crystal transition of liquid crystal polymer may be more responsive.By changing of the variation maintenance of other environmental factors, just can utilize double-isopressing device that transformations such as crystalline phase, configuration are intuitively observed with crystalline state.

Claims (8)

1. double-isopressing device, it is characterized in that comprising outer isostatic pressure vessel (1) and interior isostatic pressure vessel (10), outer isostatic pressure vessel (1) is an airtight cavity volume, be provided with electric heater unit (8) and support (9) in the cavity volume, the heating cable of electric heater unit (8) is drawn cavity volume and is linked to each other with temperature controller (7), be fixed with interior isostatic pressure vessel (10) and CCD camera (11) on the support (9), isostatic pressure vessel is provided with air intake valve (12) and drain tap (16) outside, and be fixed with pressure transducer (5), temperature sensor (15) and displacement transducer (13), pressure transducer (5), temperature sensor (15), displacement transducer (13) is drawn airtight cavity volume with the signal wire of CCD camera (11) and is linked to each other with computing machine, interior isostatic pressure vessel (10) is to have air intake opening (22), the transparent vessel of gas outlet (23) and saddle (19) advances, the gas outlet is furnished with stopper.
2. double-isopressing device according to claim 1, the top that it is characterized in that interior isostatic pressure vessel (10) is that kapillary (20), bottom are the sample chamber, the sample chamber is connected by ground with kapillary, and inlet, outlet is arranged on the sample chamber, and saddle (19) is the slider in the kapillary.
3. double-isopressing device according to claim 2 is characterized in that being provided with in sample chamber and kapillary junction and prevents that slider (19) from slipping into the back-up ring (21) of sample chamber.
4. double-isopressing device according to claim 1 is characterized in that interior isostatic pressure vessel (10) is a cylinder barrel, and saddle (19) is the piston in the cylinder barrel, and inlet, outlet is arranged on the piston, is provided with back-up ring (21) in cylinder barrel.
5. double-isopressing device according to claim 1 is characterized in that outer isostatic pressure vessel (1) is made of housing and piston (2), is provided with seal (3) on the surface of contact of piston (2) and inner walls.
6. double-isopressing device according to claim 1 is characterized in that outer isostatic pressure vessel (1) is made of housing and top cover (18), is provided with seal (3) on top cover and inner walls surface of contact.
7. according to claim 5 or 6 described double-isopressing devices, it is characterized in that the housing of outer isostatic pressure vessel is made up of base (6) and weldless steel tube thread connection, and on surface of contact, be provided with RUBBER O RunddichtringO (14) that housing is surrounded by collet (4) outward.
8. double-isopressing device according to claim 1 is characterized in that the application in physics or chemical equilibrium under research pressure, the transition process.
CNB2005100615011A 2005-11-09 2005-11-09 Double-isopressing device and application thereof Expired - Fee Related CN100570367C (en)

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CN100570367C CN100570367C (en) 2009-12-16

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102313756A (en) * 2010-07-09 2012-01-11 中科合成油技术有限公司 Automatic swelling measuring device and swelling measuring method for coal
CN101288934B (en) * 2007-04-16 2012-01-18 浙江三花制冷集团有限公司 Servo press mounting device for monitoring press mounting force and displacement
CN103743863A (en) * 2013-12-18 2014-04-23 工业和信息化部电子第五研究所 Method and device for estimating capability of resisting 'hydrogen poisoning'
CN103837436A (en) * 2012-11-23 2014-06-04 中国科学院理化技术研究所 High-pressure device for testing compressive strength of hollow microspheres under isostatic pressure by air pressure method
CN104343770A (en) * 2014-10-16 2015-02-11 中国工程物理研究院化工材料研究所 Heating device for medium oil in working cylinder of heating isostatic-pressing machine

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101288934B (en) * 2007-04-16 2012-01-18 浙江三花制冷集团有限公司 Servo press mounting device for monitoring press mounting force and displacement
CN102313756A (en) * 2010-07-09 2012-01-11 中科合成油技术有限公司 Automatic swelling measuring device and swelling measuring method for coal
CN102313756B (en) * 2010-07-09 2013-04-17 中科合成油技术有限公司 Automatic swelling measuring device and swelling measuring method for coal
CN103837436A (en) * 2012-11-23 2014-06-04 中国科学院理化技术研究所 High-pressure device for testing compressive strength of hollow microspheres under isostatic pressure by air pressure method
CN103837436B (en) * 2012-11-23 2016-08-10 中国科学院理化技术研究所 High-pressure device for testing compressive strength of hollow microspheres under isostatic pressure by air pressure method
CN103743863A (en) * 2013-12-18 2014-04-23 工业和信息化部电子第五研究所 Method and device for estimating capability of resisting 'hydrogen poisoning'
CN103743863B (en) * 2013-12-18 2015-12-30 工业和信息化部电子第五研究所 The method of anti-" hydrogen the is poisoning " ability of assessment and device thereof
CN104343770A (en) * 2014-10-16 2015-02-11 中国工程物理研究院化工材料研究所 Heating device for medium oil in working cylinder of heating isostatic-pressing machine

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