CN101819170B - Non-integrated variable volume high-pressure phase balance measuring device - Google Patents
Non-integrated variable volume high-pressure phase balance measuring device Download PDFInfo
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- CN101819170B CN101819170B CN2010101734625A CN201010173462A CN101819170B CN 101819170 B CN101819170 B CN 101819170B CN 2010101734625 A CN2010101734625 A CN 2010101734625A CN 201010173462 A CN201010173462 A CN 201010173462A CN 101819170 B CN101819170 B CN 101819170B
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Abstract
The invention discloses a non-integrated variable volume high-pressure phase balance measuring device, which belongs to the technical field of chemical engineering. The measuring device consists of an air bottle, a filter, a cold trap, a high-pressure injection pump, a needle valve, a fixed volume high-pressure visible phase balance kettle, a tee joint, an adjustable volume pressure reduction container, an air release valve and an oven. The fixed volume high-pressure visible phase balance kettle and the pressure reduction container are connected by using the tee joint; the adjustable volume non-visual pressure reduction container has a pump head plunger piston structure of a high-pressure plunger piston pump or is a pressure reduction container; an outlet is plugged by a plunger piston pump head and a stainless steel plug, and an inlet is provided with a cutting sleeve joint which is connected with the high-pressure visible phase balance kettle; and the pressure reduction container is provided with an adjusting screw, and the lower end of the adjusting screw is provided with a universal joint which is connected with a piston. The measuring device has the advantages of making full use of a fixed volume phase balance pool and adjusting the pressure of the whole system through the externally connected container. The operation is time-saving and convenient, the total manufacturing cost of the device is low, and the sealing requirement is easily met.
Description
Technical field
The invention belongs to technical field of chemical engineering, relate to a kind of improved device of high pressure phase balance studies, the visual still that weighs mutually of fixed volume is modified into the variable-volume measurement mechanism that balances each other.
Background technology
Study on Phase Equilibrium relates to various aspects such as distillation, extraction, dissolving, recrystallization, purification and metallographic examination at present, for research and production chemical, chemical industry extremely profound significance is arranged.And the high pressure visable still that balances each other is that research thermodynamics balances each other, and the key instrument of observing reaction under high pressure.Observing wherein a kind of important method of high pressure phase balance is static method; To prepare certain density material in advance and put into equilibrium still; Change pressure or temperature then gradually; Occur or disappear until observing a certain the beginning mutually, pressure, temperature and the known material concentration of this moment promptly constitute the frontier point of a phase.Near critical point, it is the most reliable, the method that also is best suited for.But existing Instrument structure is too in complicacy, and cost is high.The fixed volume still that balances each other, cost is lower, uses the column type form more.But detection time is long, and for researcher's experience, responsible degree is had relatively high expectations.
Chinese patent CN 101021519A discloses a kind of phase balance determining device of high pressure visable adjustable volume; Volume that can online adjusting high pressure equilibrium still; And have visual window, research is convenient, but the price of withstand voltage glass own is higher; And the visual window that this equilibrium still uses is long bar shaped, and this has just improved the overall cost of equilibrium still; The hermetically-sealed construction of this equilibrium still is also complicated on the other hand.
Xu of Nanjing University of Technology DeAGE etc. has been set up the two circulation phase equilibrium experiment determinators of a cover vapour-liquid, and has adopted magnetic force ebullator circulation stream-liquid two-phase flow body, the online sample analysis sample of six-way valve.(Xu Meiqian, Qian Renyuan.The two devices that balance each other that circulate of Nanjing University of Technology's journal (natural science edition) vapour-liquid.2006，28(5)：76-78。) device is complicated, inconvenient operation.
Summary of the invention
The object of the present invention is to provide a kind of variable-volume high pressure phase balance studies device of non-Unitary, it is higher to solve the present variable-volume apparatus cost that balances each other, the problem of seal complex.
Technical scheme of the present invention is: the concrete structure of this device mainly is made up of gas cylinder 1, filtrator 2, cold-trap 3, high pressure syringe pump 4, needle-valve 6, fixed volume high pressure phase equilibrium still 8, threeway and adjustable volume pressure reduction vessel 12, atmospheric valve 11, baking oven 13.The present invention designs the ingenious fixed volume still that balances each other that utilized, and only need add a piston type pressure reduction vessel, can carry out the variable-volume research that balances each other.The fixed volume still that balances each other is connected with threeway with the non-visual pressure reduction vessel of an adjustable volume, changes system pressure through the volume of regulating non-visual pressure reduction vessel.The visual still that balances each other of fixed volume can have been bought from market, and its volume can change according to customer requirements, and cost is relatively low.And pressure reduction vessel has two kinds of methods to realize, a kind of is the pump head piston structure that utilizes high-pressure plunger pump, the pressure reduction vessel that a kind of the present invention of being designs.
The high-pressure plunger pump pump head that can be used as one of pressure reduction vessel generally is a double plunger, so add a plug on will be at one end, and adds a cutting ferrule joint on the other end, is used for that the balance each other outlet of still is connected with high pressure visable.Adjustable volume is relevant with the stroke of plunger.
The structure of adjustable volume pressure reduction vessel is made up of cavity, handwheel, end cap, piston rod, piston ring and piston, air intake opening, evacuation port.Be connected with the 1.25mm coarse plain thread between piston rod and the end cap; The end cap pipe thread is left-handed, adopts the coarse thread of pitch 2mm; One end of piston rod is welded with handwheel, and the other end is a universal knot, links to each other with piston ring through universal knot, can drive piston to move up and down; And piston is made up of piston ring and piston, is respectively the piston ring first half, piston ring Lower Half, the piston first half, piston Lower Half, all adopts oat tail groove structure to connect between them, and material is for filling graphite.
Effect of the present invention and benefit are to have made full use of the fixed volume still that balances each other, and connect the pressure that container is regulated whole system outward through one.The fixed volume still that balances each other is used for placing material, observes phase-state change, and comes the regulation system volume with connecting pressure reduction vessel outward, change pressure.With respect to traditional static method, reduced the balance detection time greatly, alleviated operator's burden.The overall cost of device is lower, and seal request reaches easily.
Description of drawings
Fig. 1 is the balance each other schematic flow sheet of still phase balance determining of non-Unitary high pressure variable-volume.
Among the figure: 1 dioxide bottle; 2 filtrators; 3 cold-traps; 4 high pressure syringe pumps; 5 surge tanks; 6 needle-valves; 7 magnetic stirring apparatuss; The 8 high pressure visables still that balances each other; 9 thermopairs; 10 tensimeters; 11 atmospheric valves; 12 pressure reduction vessels; 13 baking ovens.
Fig. 2 is the pressure reduction vessel structural representation.
Among the figure: 14 pressure reduction vessel cavitys; 15 piston body the latter halfs; 16 piston body the first half; The related piston ring the latter half of 17 bars; The related piston the first half of 18 bars; 19 end caps; 20 piston rods; 21 handwheels; 22 air intake openings; 23 evacuation ports; 24 chucks.
Fig. 3 is the related piston ring the first half of bar front view.
Fig. 4 is the related piston ring the first half of bar vertical view.
Fig. 5 is the related piston ring the latter half of bar front view.
Fig. 6 is the related piston ring the latter half of bar vertical view.
Fig. 7 is piston the first half front view.
Fig. 8 is piston the first half vertical view.
Fig. 9 is piston the latter half front view.
Figure 10 is piston the latter half vertical view.
Figure 11 is piston rod construction figure.
Figure 12 is a piston rod A-A sectional view shown in Figure 11.
Figure 13 is the end cap front view.
Figure 14 is the end cap vertical view.
Embodiment
Below in conjunction with technical scheme and accompanying drawing and concrete embodiment technical scheme of the present invention is done further to describe.
Apparatus of the present invention mainly are made up of balance each other still 8, thermopair 9, tensimeter 10, atmospheric valve 11, pressure reduction vessel 12, baking oven 13 of dioxide bottle 1, filtrator 2, cold-trap 3, high pressure syringe pump 4, surge tank 5, needle-valve 6, magnetic stirring apparatus 7, fixed volume high pressure visable.Fixed volume high pressure visable balance each other still 8 and pressure reduction vessel 12 connect with a threeway; The non-visual pressure reduction vessel of adjustable volume is the pump head piston structure or the pressure reduction vessel of high-pressure plunger pump; The pump head of ram pump adds a stainless steel plug exit is blocked, and inflow point adds a cutting ferrule joint, is connected with the high pressure visable still that balances each other; Pressure reduction vessel has an adjusting screw mandrel as piston rod, and the end cap on cylindrical shell top is connected with the adjusting screw mandrel through screw thread, and regulating the screw mandrel lower end is a universal knot, is connected with piston.Fig. 2 has provided the structural representation of the pressure reduction vessel of the visual kettle device that balances each other of high pressure variable-volume provided by the invention.As shown in Figure 2, pressure reduction vessel is by pressure reduction vessel cavity 14, piston body the latter half 15, piston body the first half 16, the related piston ring the latter half 17 of bar; The related piston ring the first half 18 of bar, end cap 19, piston rod 20, handwheel 21, air intake opening 22, evacuation port 23, chuck 24 is formed.Be connected hand wheel pole and piston rod welding between piston rod and the end cap with the 1.25mm coarse plain thread.The end cap pipe thread is left-handed, adopts the coarse thread of pitch 2mm.Between piston and piston ring, and link to each other with oat tail groove structure between the piston body.
The regulating piston bar drives piston and moves, thereby changes the volume of cylindrical shell.The maximum working pressure (MOP) of pressure reduction vessel is 35MPa, and working temperature is 0～60 ℃.
Embodiment 1
The mensuration of CO2 critical point.At first material is put into the fixed volume still that balances each other, the plunger of pressure reduction vessel is pushed into the bottom, according to connecting each device shown in the accompanying drawing 1; Open atmospheric valve 11 and needle-valve 6 then, open gas cylinder low pressure emptying three times, close atmospheric valve 11; Be driven into fixed volume to CO2 with high-pressure plunger pump and balance each other in the still, make pressure reach 8.50MPa, temperature is controlled at 32 ℃ by baking oven.After treating thermal equilibrium,, drive piston and move, change the volume of cylindrical shell 1, pressure is reduced to about 7.30MPa from 8.50MPa through regulating piston bar 7.Can observe CO2 from form and become muddiness by clear; And, when making the smaller volume of cavity, can make pressure come back to 8.50MPa again when promoting piston rod, can be observed CO2 and recover the clear state again this moment.Open atmospheric valve 11 pressure releases.
Embodiment 2
Surfactant A OT, i.e. two (2-ethylhexyl) succinate sodium sulfonate ethanolic solution and supercritical CO 2 phase balance determinings.With 3.74m10.0861molL
-1The AOT ethanolic solution be placed on fixed volume together with stirrer and balance each other in the still, add 1.58ml ethanol again, add water 0.38ml.Be connected into the system of balancing each other.The pressure reduction vessel piston rod is pushed into the bottom.Temperature is controlled at 35 ℃ with baking oven, and squeezing into CO2 is 12MPa up to pressure, stirs until observe the potpourri clear that becomes from form.This moment, the regulating piston bar increased the volume of cavity 1, occurred vaporific muddiness suddenly until the fixed volume still top of balancing each other, and the pressure of writing down this moment is 10.22MPa.And promote piston rod forward the volume of cavity 1 is reduced, system is recovered clear again.The pulled backwards piston vaporific muddiness occurs up to system once more, three times so repeatedly, obtains 10.32,10.28 cloud points of this system of averaging 35 ℃ that promptly obtain the time respectively and presses 10.27MPa.
Claims (2)
1. non-integrated variable volume high-pressure phase balance measuring device; Form by the balance each other non-visual pressure reduction vessel of still, threeway and adjustable volume, atmospheric valve, baking oven of gas cylinder, filtrator, cold-trap, high pressure syringe pump, needle-valve, fixed volume high pressure visable, it is characterized in that:
A. gas cylinder (1) is connected through pipeline with filtrator (2); Filtrator (2) is connected through pipeline with cold-trap (3); Cold-trap (3) is connected through pipeline with high pressure syringe pump (4), and high pressure syringe pump (4) is connected through pipeline with surge tank (5), and surge tank (5) is connected through pipeline with needle-valve (6); The inlet connector tube that the discharge pipe of needle-valve (6) and fixed volume high pressure visable balance each other on the still (8) is connected; The fixed volume high pressure visable balances each other and connects thermopair (9) on the still (8), and the balance each other outlet of still (8) of fixed volume high pressure visable is connected with tensimeter (10), fixed volume high pressure visable balance each other still (8) and the non-visual pressure reduction vessel of adjustable volume (12); Connect with a threeway, connect an atmospheric valve (11) in the threeway;
B. the non-visual pressure reduction vessel of adjustable volume is the pump head piston structure or the pressure reduction vessel of high-pressure plunger pump;
C. the pump head of ram pump adds a stainless steel plug exit is blocked, and inflow point adds a cutting ferrule joint, is connected with the high pressure visable still that balances each other;
D. the non-visual pressure reduction vessel of adjustable volume has an adjusting screw mandrel as piston rod, and the end cap on cylindrical shell top is connected with the adjusting screw mandrel through screw thread, and regulating the screw mandrel lower end is a universal knot, is connected with piston.
2. a kind of non-integrated variable volume high-pressure phase balance measuring device according to claim 1; It is characterized in that: the piston of the non-visual pressure reduction vessel of adjustable volume wherein; Form by piston ring and piston; Be respectively the piston ring first half, piston ring Lower Half, the piston first half, piston Lower Half, all adopt oat tail groove structure to connect between them, material is for filling graphite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101734625A CN101819170B (en) | 2010-05-13 | 2010-05-13 | Non-integrated variable volume high-pressure phase balance measuring device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101734625A CN101819170B (en) | 2010-05-13 | 2010-05-13 | Non-integrated variable volume high-pressure phase balance measuring device |
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| Publication Number | Publication Date |
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| CN101819170A CN101819170A (en) | 2010-09-01 |
| CN101819170B true CN101819170B (en) | 2012-05-16 |
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| CN2010101734625A Expired - Fee Related CN101819170B (en) | 2010-05-13 | 2010-05-13 | Non-integrated variable volume high-pressure phase balance measuring device |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105865963B (en) * | 2016-03-29 | 2018-06-05 | 中国石油大学(华东) | A kind of supercritical carbon dioxide balances each other instrument and its application method |
| CN107727805B (en) * | 2017-10-18 | 2021-06-08 | 中石化炼化工程（集团）股份有限公司 | High-temperature high-pressure gas-liquid phase balance testing device and method |
| CN109630401B (en) * | 2018-11-16 | 2022-11-25 | 泰州博英生物科技有限公司 | Syringe pump for micro-fluidic device |
| CN113123767A (en) * | 2019-12-27 | 2021-07-16 | 中国石油天然气股份有限公司 | Oil-gas periodic huff-puff simulation system and method |
| CN111879736B (en) * | 2020-07-31 | 2022-11-15 | 西南石油大学 | Device and method for determining solid-phase deposition conditions of crude oil in high-temperature ultrahigh-pressure oil reservoir |
| CN114425179B (en) * | 2020-09-02 | 2023-07-11 | 中国石油化工股份有限公司 | Phase balance measuring and separating device and application method thereof |
| CN114279890B (en) * | 2021-12-24 | 2024-06-07 | 青岛科技大学 | System and method for measuring liquid volume under high pressure |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101021519A (en) * | 2007-03-15 | 2007-08-22 | 上海交通大学 | High pressure visable adjustable volume phase balance determining device |
| CN101699274A (en) * | 2009-10-23 | 2010-04-28 | 中国科学院武汉岩土力学研究所 | Testing device for natural gas hydrate phase equilibrium in marine sediment and method thereof |
-
2010
- 2010-05-13 CN CN2010101734625A patent/CN101819170B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101021519A (en) * | 2007-03-15 | 2007-08-22 | 上海交通大学 | High pressure visable adjustable volume phase balance determining device |
| CN101699274A (en) * | 2009-10-23 | 2010-04-28 | 中国科学院武汉岩土力学研究所 | Testing device for natural gas hydrate phase equilibrium in marine sediment and method thereof |
Non-Patent Citations (3)
| Title |
|---|
| JP特开平7-167768A 1995.07.04 |
| 徐美倩等.汽液双循环相平衡测定装置.《南京工业大学学报》.2006,第28卷(第5期),76-78. * |
| 邱祖民.汽液相平衡测定的研究进展.《江西科学》.1996,第14卷(第4期),254-258. * |
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