CN110530689A - A kind of preparation method and device of aging sample, senile experiment method - Google Patents

A kind of preparation method and device of aging sample, senile experiment method Download PDF

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Publication number
CN110530689A
CN110530689A CN201910626191.5A CN201910626191A CN110530689A CN 110530689 A CN110530689 A CN 110530689A CN 201910626191 A CN201910626191 A CN 201910626191A CN 110530689 A CN110530689 A CN 110530689A
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CN
China
Prior art keywords
aging
plastic container
deformable plastic
soft deformable
bag body
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CN201910626191.5A
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Chinese (zh)
Inventor
孔昭柯
孙林涛
王熙
时志兴
白兆非
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China Petroleum and Chemical Corp
China Petrochemical Corp
Exploration and Development Research Institute of Sinopec Henan Oilfield Branch Co
Original Assignee
China Petrochemical Corp
Exploration and Development Research Institute of Sinopec Henan Oilfield Branch Co
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Application filed by China Petrochemical Corp, Exploration and Development Research Institute of Sinopec Henan Oilfield Branch Co filed Critical China Petrochemical Corp
Priority to CN201910626191.5A priority Critical patent/CN110530689A/en
Publication of CN110530689A publication Critical patent/CN110530689A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Biological Materials (AREA)

Abstract

The present invention relates to a kind of preparation method of aging sample and device, senile experiment methods.1) preparation method of the aging sample is the following steps are included: vacuumize deoxygenation: vacuumizing to a soft deformable plastic container, soft deformable plastic container deforms under the action of negative pressure, and the air in container intracavity is discharged;2) fluid injection: after vacuumizing deoxygenation, liquid to be aging is pressed into soft deformable plastic container, sealing.The preparation method of aging sample provided by the invention, using soft deformable plastic container replace ampoule bottle realize the preparation of aging sample, it can be achieved that the anaerobic of liquid to be aging saves, experiments verify that, can be used for senile experiment.Soft deformable plastic container is reusable, compared with ampoule bottle aging sample, greatly reduces preparation cost.

Description

A kind of preparation method and device of aging sample, senile experiment method
Technical field
The invention belongs to the Evaluation of Thermal Stability fields of polymer, and in particular to a kind of preparation method and dress of aging sample It sets, senile experiment method.
Background technique
Driving the long-term thermal stability of agent in the evaluation of tertiary oil recovery Chemical Screening is a key parameter, is carrying out drive agent at present It is the method using SY/T5862-2008 mostly when prepared by long-term thermal stability laboratory sample.When heat stability testing, test first Then chemical flooding agent to be measured is dispensed into 5 ampoule bottles, and ampoule bottle is connected to pumping by the apparent viscosity of chemical flooding agent to be measured On blank pipe converges, manifold will be evacuated together with being put into cold-trap after ampoule bottle freezing, connect with evacuator, after evacuation, thaw at RT; After repeated freezing, evacuation, operation of thawing, nitrogen is poured into manifold and ampoule bottle to atmospheric pressure, cuts device sealing with flame envelope After carry out senile experiment.
Thermal stability experimental evaluation is that chemical flooding agent is kept after a certain period of time under the conditions of anaerobic, high temperature (such as 75 DEG C) Viscosity retention ratio, keeping chemical flooding agent to test under anaerobic can just make experimental result have certain representative meaning.In order to It is further simplified the anaerobic conveying of chemical flooding agent, saves, notification number is that the utility model patent of CN204841532U discloses one Kind isolation air prepares the device of liquid to be aging, can realize the anaerobic conveying of mixed liquor using the device, save.The anaerobic is defeated The method for sending mixed liquor is to inject mixed liquor after vacuumizing to ampoule bottle, then carries out the sealing of ampoule bottle.
Thermal stability experiment belongs to long-term, continuity experiment, and the liquid to be aging in ampoule bottle is once opening and using, to old Changing liquid can touch air, in liquid and ampoule bottle itself to be aging can not all continue to use, thus cause hot steady Anaerobic conveying need to be repeated when qualitative experiment, save operation, not only experimentation is cumbersome, low efficiency, and ampoule bottle etc. is real The consumption for testing material is also larger.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of aging sample, high with the preparation cost for solving aging sample The problem of.
Second object of the present invention is to provide a kind of device for being used to prepare aging sample, to solve aging sample The high problem of preparation cost.
Third object of the present invention is to provide a kind of senile experiment method, with solve the experiment of existing aging method at The problem of this height, low efficiency.
To achieve the above object, technical solution used by the preparation method of aging sample of the invention is:
A kind of preparation method of aging sample, comprising the following steps:
1) it vacuumizes deoxygenation: a soft deformable plastic container is vacuumized, soft deformable plastic container is negative The lower deformation of pressure effect, the air in container intracavity is discharged;
2) fluid injection: after vacuumizing deoxygenation, liquid to be aging is pressed into soft deformable plastic container, sealing.
The preparation method of aging sample provided by the invention replaces ampoule bottle to realize old using soft deformable plastic container Change the preparation of sample, it can be achieved that the anaerobic of liquid to be aging saves, experiments verify that, it can be used for senile experiment.It is soft deformable Plastic containers are reusable, compared with ampoule bottle aging sample, greatly reduce preparation cost.
To further decrease sample cost, it is preferred that the soft deformable plastic container is blood bag, and blood bag includes bag body It is connected with one end of the communicating pipe being arranged in bag body, communicating pipe with bag body inner cavity, the other end is connected to extension on the outside of bag body Pipe extends the pipe clamp that opening or closed communication pipe are provided on one end to bag body outside.
The technical solution used by the device of aging sample that is used to prepare of the invention is:
A kind of device being used to prepare aging sample, including soft deformable plastic container, soft deformable plastic container It deforms under the action of negative pressure and the air in container intracavity is discharged;
Wet tank to be aging;
Vacuum-pumping pipeline, one end of vacuum-pumping pipeline are connected with soft deformable plastic container, and the opening of the other end is to take out Vacuum port;
Fluid injection pipeline connects wet tank to be aging and soft deformable plastic container;
Valve, be respectively arranged at vacuum-pumping pipeline and liquid injection pipe road or vacuum-pumping pipeline, fluid injection pipeline be used for it is soft The connected one end of matter deformable plastic container is connected after merging with soft deformable plastic container, and valve is arranged at merging, with Control vacuum-pumping pipeline, the opening or closing of fluid injection pipeline;
Gas access is squeezed, is set on wet tank to be aging, for being passed through extruding gas to wet tank to be aging, Liquid to be aging to be pressed into the inner cavity of soft deformable plastic container by fluid injection pipeline.
Provided by the present invention for preparing the device of aging sample, can facilitate by liquid anaerobic to be aging be delivered to it is soft can In deformable plastic container, the manufacturing cost of aging sample preparation is reduced.
To further decrease manufacturing cost, it is preferred that the soft deformable plastic container is blood bag, and blood bag includes bag body It is connected with one end of the communicating pipe being arranged in bag body, communicating pipe with bag body inner cavity, the other end is connected to extension on the outside of bag body Pipe extends the pipe clamp that opening or closed communication pipe are provided on one end to bag body outside.
Technical solution used by senile experiment method of the invention is:
A kind of senile experiment method, comprising the following steps:
1) it vacuumizes deoxygenation: a soft deformable plastic container is vacuumized, soft deformable plastic container is negative The lower deformation of pressure effect, the air in container intracavity is discharged;
2) fluid injection: after vacuumizing deoxygenation, liquid to be aging is pressed into soft deformable plastic container, sealing;
3) it tests: the soft deformable plastic container being sealed is subjected to senile experiment.
Liquid to be aging is packed into soft deformable plastic container by senile experiment method of the invention, is then carried out old Change experiment, soft deformable plastic container is reusable, has saved the use of the experiment consumptive material such as ampoule bottle, reduces aging reality Test cost.
To further increase senile experiment efficiency, it is preferred that, will be soft after senile experiment reaches setting time in step 3) Liquid in matter deformable plastic container avoids air from entering by detection requirement discharge, discharge process, seal later it is soft can Deformable plastic container, continues senile experiment.The operation realizes the liquid in deformable plastic container and examines in different agings The continuous anaerobic surveyed in the period uses, compared with prior art, time saving and energy saving, improves conventional efficient, reduces experimental cost.
To further decrease experimental cost, it is preferred that the soft deformable plastic container is blood bag, and blood bag includes bag body It is connected with one end of the communicating pipe being arranged in bag body, communicating pipe with bag body inner cavity, the other end is connected to extension on the outside of bag body Pipe extends the pipe clamp that opening or closed communication pipe are provided on one end to bag body outside.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the Installation practice for being used to prepare aging sample of the invention;
In figure, 1- vacuum pump, 2- drying tower, 3- buffer container, the soft deformable plastic container of 4-, 5- liquid storage to be aging Tank, 6- triple valve, 7- gas source, 8- vacuum meter.
Specific embodiment
Embodiments of the present invention are described further with reference to the accompanying drawing.
The specific embodiment of the device for being used to prepare aging sample of the invention, as shown in Figure 1, including vacuum pump 1, dry Device, buffer container 3, soft deformable plastic container 4, wet tank to be aging 5, gas source 7.
Soft deformable plastic container 4 is finished product blood bag, including bag body and and communicating pipe for being arranged in bag body, communicating pipe One end be connected with bag body inner cavity, the other end extends on the outside of bag body, and communicating pipe is arranged to extending on the outside of bag body on one end There is the pipe clamp (not shown in figure 1) of opening or closed communication pipe.Bag body includes the forward and backward plastic foil being oppositely arranged, forward and backward plastics The surrounding sealing of film is into a single integrated structure.
Communicating pipe is connected with the first valve port of triple valve 6, and the second valve port of triple valve 6 is stored up by pipeline and liquid to be aging Tank 5 is connected, and the third valve port of triple valve 6 is connected by pipeline with vacuum pump 1.
The outlet being connected on wet tank 5 to be aging with the second valve port is the liquid outlet for liquid to be aging discharge, to old Change and is additionally provided with the extruding gas access being connected with gas source 7 on wet tank 5.Gas source 7 is High Purity Nitrogen airbag.
Vacuum meter 8, drying device and buffer container 3 are provided in the connecting pipeline of vacuum pump 1 and third valve.Dry dress It is set to the drying tower 2 being sequentially connected.Buffer container 3 is surge flask.
Pipeline between vacuum pump 1 and the communicating pipe of bag body forms vacuum-pumping pipeline, wet tank 5 to be aging and bag body Pipeline between communicating pipe forms fluid injection pipeline.
The course of work of apparatus above is as follows: the first valve port of adjustment triple valve 6 first is connected to third valve port, is vacuumized Pipeline connection (the first valve port, the second valve port interface channel accordingly close), open vacuum pump 1 finished product blood bag is vacuumized;It takes out After vacuum, the front and back plastic foil of finished product blood bag, which is bonded to each other, is completely exhausted out the gas in bag, then adjusts the first of triple valve 6 Valve port is connected to the second valve port, fluid injection pipeline connection (the first valve port, third valve port interface channel accordingly close), by gas source 7 It is passed through extruding gas into wet tank 5 to be aging, squeezes gas for the liquid to be aging in wet tank 5 to be aging by going out liquid Mouth discharge, then enter in finished product blood bag (height of adjustable liquid outlet is higher than inlet to facilitate liquid to be discharged) through inlet, After the completion of liquid conveying to be aging, the communicating pipe in finished product blood bag is clamped with pipe clamp, liquid to be aging can be made in anaerobic item It is saved under part.
Valve can be set at the liquid outlet of wet tank 5 to be aging, before conveying liquid to be aging, valve is closed, The air in the connecting pipeline of the second valve port and inlet is shifted to vacuum-pumping pipeline under the action of negative pressure at this time, then by adjusting Triple valve and vacuum extract the air in fluid injection pipeline out.
The occasion using liquid to be aging is being needed, the pipe clamp on the communicating pipe of finished product blood bag is being unclamped, is being measured as needed The liquid to be aging in it is squeezed out, the actual volume in finished product blood bag accordingly compresses, it then proceedes to be clamped communicating pipe with pipe clamp, Can continue that the liquid to be aging in finished product blood bag is kept to be in anaerobic state.
The embodiment of senile experiment method of the invention, using the device for being used to prepare aging sample above, including it is following Step:
1) it vacuumizes deoxygenation: finished product blood bag is vacuumized, forward and backward plastic foil mutually pastes finished product blood bag under the action of negative pressure Tightly, the air in its inner cavity is discharged.
2) fluid injection: chemical flooding agent to be measured indentation is vacuumized in the finished product blood bag after deoxygenation and (is pressed into 350ml chemistry to be measured altogether Drive agent), the communicating pipe in finished product blood bag is clamped with pipe clamp.
3) it tests: the finished product blood bag being sealed is subjected to senile experiment at 80 DEG C.After senile experiment 1d, by finished product blood bag On pipe clamp unclamp, squeeze out 15ml chemical flooding agent to be measured, detect and record its apparent viscosity.Senile experiment 5d, 10d, 20d, After 30d, 40d, 45d, chemical flooding agent to be measured is squeezed out by same operation, detects and records its apparent viscosity.
During the above senile experiment, part liquid may be remained in the outside pipeline section of pipe clamp clamped position on communicating pipe Body, the partially liq are contacted with air, can squeeze out in time the partially liq, to avoid may be to follow-up test bring not It is good influence (can also next time test before, using the partially liq as waste liquid discharge, with the liquid of extrusion intracavitary out of bag body into Row test).
Comparative example
The chemical flooding agent thermal stability experimental method of comparative example conveys the device and the basic phase of embodiment of liquid to be aging Together, difference is only that, replaces finished product blood bag using ampoule bottle, is the practical new of CN204841532U with specific reference to Authorization Notice No. The related content of type patent disclosure;After ampoule bottle heat sealing, senile experiment is carried out at identical conditions.
The experimental result of the thermal stability experimental method of embodiment and comparative example is investigated, it is specific as shown in table 1.
The Comparative result of 1 differing thermal stabilities experimental method of table
As shown in Table 1, the ampoule bottle method of the experimental result of the method for embodiment and comparative example is almost the same, To drive the thermal stability of agent for evaluating chemical.But the method for embodiment realizes the continuous use of liquid to be aging, which save The anaerobic transmission process repeatedly of liquid to be aging, has saved the dosage of ampoule bottle, has reduced experimental cost.
The above experimental method is suitable for temperature in 80 DEG C of sample aging experiments below.Temperature is too high, in senile experiment mistake Cheng Zhongshui (solvent) will become gaseous state, and blood bag is caused to expand as balloon, and volume increases, so that aged samples do not have representative Property.
The specific embodiment of the preparation method of aging sample of the invention, the step with the embodiment of above-mentioned senile experiment method Rapid 1) -2) identical, this will not be detailed here.

Claims (7)

1. a kind of preparation method of aging sample, which comprises the following steps:
1) it vacuumizes deoxygenation: a soft deformable plastic container is vacuumized, soft deformable plastic container is made in negative pressure With lower deformation, the air in container intracavity is discharged;
2) fluid injection: after vacuumizing deoxygenation, liquid to be aging is pressed into soft deformable plastic container, sealing.
2. the preparation method of aging sample as described in claim 1, which is characterized in that described soft deformable in step 2) Plastic containers are blood bag, and blood bag includes bag body and communicating pipe for being arranged in bag body, and one end of communicating pipe is connected with bag body inner cavity Logical, for the other end to extending on the outside of bag body, communicating pipe is provided with opening or closed communication pipe to extending on the outside of bag body on one end Pipe clamp.
3. a kind of device for being used to prepare aging sample, which is characterized in that soft deformable including soft deformable plastic container Plastic containers deform under the action of negative pressure and the air in container intracavity are discharged;
Wet tank to be aging;
Vacuum-pumping pipeline, one end of vacuum-pumping pipeline are connected with soft deformable plastic container, and the opening of the other end is to vacuumize Mouthful;
Fluid injection pipeline connects wet tank to be aging and soft deformable plastic container;
Valve, be respectively arranged at vacuum-pumping pipeline and liquid injection pipe road or vacuum-pumping pipeline, fluid injection pipeline be used for it is soft can The connected one end of deformable plastic container is connected after merging with soft deformable plastic container, and valve is arranged at merging, with control Vacuum-pumping pipeline, the opening or closing of fluid injection pipeline;
Gas access is squeezed, is set on wet tank to be aging, it, will for being passed through extruding gas to wet tank to be aging Liquid to be aging is pressed into the inner cavity of soft deformable plastic container by fluid injection pipeline.
4. being used to prepare the device of aging sample as claimed in claim 3, which is characterized in that the soft deformable plastic holds Device is blood bag, and blood bag includes bag body and communicating pipe for being arranged in bag body, and one end of communicating pipe is connected with bag body inner cavity, another It holds to extension on the outside of bag body, communicating pipe extends the pipe clamp for being provided with opening or closed communication pipe on one end to bag body outside.
5. a kind of senile experiment method, which comprises the following steps:
1) it vacuumizes deoxygenation: a soft deformable plastic container is vacuumized, soft deformable plastic container is made in negative pressure With lower deformation, the air in container intracavity is discharged;
2) fluid injection: after vacuumizing deoxygenation, liquid to be aging is pressed into soft deformable plastic container, sealing;
3) it tests: the soft deformable plastic container being sealed is subjected to senile experiment.
6. senile experiment method as claimed in claim 5, which is characterized in that in step 3), senile experiment reaches setting time Afterwards, by the liquid in soft deformable plastic container by detection requirement discharge, discharge process avoids air from entering, seals later Soft deformable plastic container, continues senile experiment.
7. such as senile experiment method described in claim 5 or 6, which is characterized in that the soft deformable plastic container is blood Bag, blood bag include bag body and communicating pipe for being arranged in bag body, and one end of communicating pipe is connected with bag body inner cavity, and the other end is to bag External side extends, and communicating pipe extends the pipe clamp that opening or closed communication pipe are provided on one end to bag body outside.
CN201910626191.5A 2019-07-11 2019-07-11 A kind of preparation method and device of aging sample, senile experiment method Pending CN110530689A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040166583A1 (en) * 2001-06-12 2004-08-26 Antoine De Gaulle Method for determining and monitoring ageing of blood bags
CN202105182U (en) * 2011-06-15 2012-01-11 孟祥远 Liquid medicine in soft bag with optimal curative effect
CN204841532U (en) * 2015-06-16 2015-12-09 中国石油化工股份有限公司 Device that mixes liquid is prepared to isolated air
CN206832642U (en) * 2017-02-17 2018-01-02 中国石油天然气股份有限公司 Asphalt binder long-term ageing simulation test device
CN107664652A (en) * 2017-08-01 2018-02-06 哈尔滨哈普电气技术有限责任公司 A kind of dynamic aging tester device and method of work

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040166583A1 (en) * 2001-06-12 2004-08-26 Antoine De Gaulle Method for determining and monitoring ageing of blood bags
CN202105182U (en) * 2011-06-15 2012-01-11 孟祥远 Liquid medicine in soft bag with optimal curative effect
CN204841532U (en) * 2015-06-16 2015-12-09 中国石油化工股份有限公司 Device that mixes liquid is prepared to isolated air
CN206832642U (en) * 2017-02-17 2018-01-02 中国石油天然气股份有限公司 Asphalt binder long-term ageing simulation test device
CN107664652A (en) * 2017-08-01 2018-02-06 哈尔滨哈普电气技术有限责任公司 A kind of dynamic aging tester device and method of work

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