CN105571984B - A kind of high temperature high pressure liquid density measuring equipment and measuring method - Google Patents
A kind of high temperature high pressure liquid density measuring equipment and measuring method Download PDFInfo
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- CN105571984B CN105571984B CN201610022178.5A CN201610022178A CN105571984B CN 105571984 B CN105571984 B CN 105571984B CN 201610022178 A CN201610022178 A CN 201610022178A CN 105571984 B CN105571984 B CN 105571984B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
- G01N9/02—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity by measuring weight of a known volume
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Abstract
The present invention proposes that a kind of high temperature high pressure liquid density measuring equipment and measuring method, including compression system, heating system and measuring system, compression system include hydraulic test machine, cylinder and piston, and seal box is between upper and lower two pistons；Measuring system includes displacement transducer and pressure sensor, displacement transducer is connected with data collecting card, pressure sensor is connected with hydraulic test Oil cylinder, data collecting card, data collecting card is connected with control device, heating system includes the heating mantle being arranged on outside cylinder, heating mantle is connected with power transformer, relay, and relay is connected with temperature controller, and temperature controller is connected with thermocouple.The present invention is much larger than the measurement range of existing high-density device；And it is simple to operate, accuracy is high, favorable reproducibility；Substantially increase the pressure limit of measurement fluid density；Be advantageous to the sealing and repeatability of raising system；Improve the actual effect and continuity of measurement result.
Description
Technical field
The invention belongs to extreme pressure and at a temperature of liquid basic performance fields of measurement, and in particular to a kind of high-temperature high-pressure liquid
The measurement apparatus and measuring method of volume density.
Background technology
Density be material physicochemical properties in a kind of highly important physical quantity, especially for liquid, density with
The macro properties such as the viscosity of liquid, refractive index, diffusion are closely related.Therefore, accurate measurement liquid is under reactiveness
Density parameter and its situation of change, it is significant for expanding application field of the different liquids in production and life.With
The development of the resources explorations such as offshore oil, under high-temperature and high-pressure conditions measure fluid density device demand increasingly
Urgently.In addition, for the excellent properties that in scientific research, some fluent materials are shown at high temperature under high pressure, also cause research
Measurement and its method of the person to fluid density under HTHP generate keen interest.However, because HTHP category is extreme
Condition, fluent material easily leak, and realize that the measurement of fluid density under this extreme condition is relatively difficult, corresponding device
Also it is less.
Utility model patent (CN00233404.6) proposes the high temperature height that liquid PVT relations are determined under a kind of HTHP
Press PVT testers, be mainly characterized by carrying out under HTHP PVT and measure, but applicable temperature (- 230 DEG C of room temperature) and
Pressure limit is smaller (0.1-25MPa), is not suitable for wider range examination oil density；Utility model patent
(CN201653848U) a kind of measurement apparatus and measuring method of high-temperature high pressure oil quality density are proposed, primarily directed to HTHP
PVT measuring instruments are improved, and can realize measurement temperature from 100 DEG C -550 DEG C, different liquid of the pressure from 0.1MPa-25MPa
The density measure of phase product.But measure upper limit of pressure is still 25MPa, it is close wider pressure limit examination liquid is not suitable for
Degree, and it is complicated, process is cumbersome.
The content of the invention
The purpose of the present invention is to be directed to above-mentioned the deficiencies in the prior art, proposes a kind of high temperature high pressure liquid density measuring equipment
And measuring method.
The technical proposal of the invention is realized in this way：A kind of high temperature high pressure liquid density measuring equipment, including compression train
System, heating system and measuring system, the compression system include hydraulic test machine, cylinder and piston, and seal box is in upper and lower two
Between individual piston, seal box is made up of upper cartridge body and lower box body, and upper cartridge body is in lower box body；The measuring system includes displacement
Sensor and pressure sensor, displacement transducer are connected with data collecting card, pressure sensor and hydraulic test Oil cylinder, data
Capture card is connected, and data collecting card is connected with control device, and the heating system includes the heating mantle being arranged on outside cylinder, heating
Set is connected with power transformer, relay, and relay is connected with temperature controller, and temperature controller is connected with thermocouple.
The seal box is metal or plastic seal box, and the cylinder is Talide cylinder.
A kind of high temperature high pressure liquid density measuring method, is carried out as steps described below：(1) testing liquid is loaded close
In jacket, and it is completely filled up, weighs liquid quality m0, record seal box internal diameter and depth；
(2) heating system is opened, cylinder is warming up to predetermined value, maintains temperature stabilization；
(3) compression system supercharging is opened, while measuring system is started working, change of the collection pressure value with shift value with the time
Change curve；
(4) calculate supercharging and heat rear fluid density
Wherein, m0For the initial mass of liquid,
R is the radius of cylinder,
Initial thickness after being converted for liquid sample volume,
S1It is the displacement that sample reduces in actually measuring on vertical direction,
S' is the bit shift compensation of systematic error,
For normal temperature and pressure fluid sample density.
The present invention realizes the measurement of fluid density under high-temperature and high-pressure conditions, and highest measurement temperature is 500 DEG C, maximum measurement
Pressure is 1000MPa, much larger than the measurement range (25MPa) of existing high-density device；And it is simple to operate, accuracy is high,
Favorable reproducibility；Device employs piston cylinder mechanical supercharged, breaches the pressure limit of liquid supercharging, substantially increases measurement
The pressure limit of fluid density；Using polytetrafluoroethylmaterial material as encapsulant, be advantageous to the sealing and again of raising system
Renaturation；Measuring system uses dynamic measurement pattern, improves the actual effect and continuity of measurement result.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the structural representation of the present invention.
Fig. 2 is structure of seal box schematic diagram.
Fig. 3 is heating system structural representation.
Fig. 4 is measuring system structural representation.
Wherein：1. compression system, 101. seal boxes, 102. pistons, 103. cylinders, 104. hydraulic test machines, 2. heating systems
System, 201. heating mantles, 202. thermocouples, 203. relays, 204. power transformers, 205. temperature controllers, 3. measuring systems,
301. displacement transducers, 302. data collecting cards, 303. pressure sensors, 304. control devices.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not paid
Embodiment, belong to the scope of protection of the invention.
As shown in figures 1-4, a kind of high temperature high pressure liquid density measuring equipment, including compression system 1, heating system 2 and survey
Amount system 3, the compression system 1 include hydraulic test machine 104, cylinder 103 and piston 102, and seal box 101 is in upper and lower two
Between piston 102, seal box 101 is made up of upper cartridge body and lower box body, and upper cartridge body is in lower box body；The measuring system 3 is wrapped
Displacement transducer 301 and pressure sensor 303 are included, displacement transducer 301 is connected with data collecting card 302, pressure sensor 303
It is connected with the oil cylinder of hydraulic test machine 104, data collecting card 302, data collecting card 302 is connected with control device 304, the heating
System 2 includes the heating mantle 201 being arranged on outside cylinder 103, and heating mantle 201 is connected with power transformer 204, relay 203, after
Electrical equipment 203 is connected with temperature controller 205, and temperature controller 205 is connected with thermocouple 202.
Wherein, compression system 1 is used to accommodate liquid and provide hyperbaric environment for liquid；Heating system 2 is used to carry for liquid
For stable hot environment；Measuring system 3 is used for the change for measuring liquid volume in pressurization.
The seal box 101 is metal or plastic seal box, such as uses aluminium, copper, polytetrafluoroethylene (PTFE) or nylon etc., institute
It is Talide cylinder, drum diameter 16,20,22 or 26mm to state cylinder 103.
The hydraulic test machine 104 used in the application is that hydraulic press, maximum working load 2000KN, maximum functional are pushed up in two sides
Distance is 400mm, preferably pumping rate 0.1-10MPa/min, 0.1MPa/min.The heating of resistance-type in heating system 2
The resistance wire material of set 201 can be Aludirome, preferably nickel chromium triangle electrothermal alloy, nickel chromium triangle electrothermal alloy, peak power 2500-
3000kW.Thermocouple 202 is K-type probe thermocouple, 0-1300 DEG C of measurement range；Power transformer 204 is that 220V/5kW is single-phase
Transformer；Relay 203 is single-phase solid relay, and direct current control exchanges, load current 40A, load voltage：24-480V/AC.
Temperature controller 205 is RKC type PID digital display temperature controllers, sampling period 0.5s, fuzzy-adaptation PID control, 1 DEG C of resolution ratio, 0.1
℃。
Displacement transducer 301 in the measuring system is high-precision contact digital displacement sensor and contactless swashs
Optical displacement sensor, preferably contact digital displacement sensor, effective range>12mm, resolution ratio>0.1 μm, mechanical response
10Hz；Pressure sensor 303 is digital pressure sensor, resolution ratio<0.01MPa, Best-case Response Time<3ms；Data collecting card
302 be that can be directly connected to the multiple sensors measurement module of all kinds sensor, sample frequency>960Hz, independent is digital defeated
Go out and input channel；The measurement apparatus heatproof upper limit is 500 DEG C, and the pressure-resistant upper limit is 1000MPa, and control device uses computer.
Thermocouple in heating system is located at the cylinder top, and for measuring the temperature of cylinder, thermocouple is horizontal with piston
To distance 3-5cm, preferably 4cm, preferably fore-and-aft distance 20-30cm, 25cm.The measuring system includes " I " and " T " two
Block steel crossbeam, it is individually fixed in the end of the upper and lower piston of the piston cylinder, the displacement sensors for fixing.
When the present invention uses, first liquid is full of in whole seal box 101, then by the pressure increase of compression system
To scheduled pressure value；Heating system is opened, carries out being warming up to predetermined temperature value for liquid, and keep constant；Open measuring system,
The pumping rate of setting hydraulic test machine 104 carries out stablizing pressurization to cylinder, while records displacement using data collecting card 302 and pass
The changing value of sensor 301 and pressure sensor 303, according to the pass of the quality of liquid, volume and displacement and density under initial environment
System, can establish the fluid sample corresponding relation of pressure and density at a certain temperature, be given at measurement temperature and measurement pressure
The density value of lower liquid.
High temperature high pressure liquid density measuring method of the present invention, is carried out as steps described below：
(1) testing liquid is loaded in seal box 101, and be completely filled up, weigh liquid quality m0, record seal box 101
Internal diameter and depth；
(2) heating system 2 is opened, cylinder 103 is warming up to predetermined value, maintains temperature stabilization；
(3) compression system supercharging is opened, while measuring system is started working, change of the collection pressure value with shift value with the time
Change curve；
(4) calculate supercharging and heat rear fluid density
Wherein, m0For the initial mass of liquid,
R is the radius of cylinder,
Initial thickness after being converted for liquid sample volume,
S1It is the displacement that sample reduces in actually measuring on vertical direction,
S' is the bit shift compensation of systematic error,
For normal temperature and pressure fluid sample density.
The present invention realizes the measurement to fluid density under high-temperature and high-pressure conditions, easy to operate, accuracy is high, reappearance
It is good；Compression system is sealed using drum equipment, and combines hydraulic test machine, and the high pressure range of fluid density ranges up to
1000MPa；Device uses Resistant heating set to provide hot environment for liquid, and the temperature range of fluid density ranges up to 500
DEG C, the pressure and temperature measurable range of liquid density measurement device has exceeded existing means of testing.
Embodiment 1
A kind of high temperature high pressure liquid density measuring method is present embodiments provided, the method for testing uses the height in Fig. 1~4
Warm highly pressurised liquid density measuring equipment measures.Wherein, seal box uses polytetrafluoroethylene (PTFE) material in experimental provision；From straight
Footpath is 20cm hard alloy cylinder；Heating mantle is 2500W from resistance wire power；0-1300 DEG C of K-type thermocouple temperature measurement scope,
With piston lateral separation 4cm, fore-and-aft distance 25cm；0.1 DEG C of temperature controller resolution ratio；Displacement sensor scope is
12mm, resolution ratio are 0.1 μm, mechanical response 10Hz；The resolution ratio of digital pressure sensor is 0.01MPa, Best-case Response Time
For 3ms；Data signal acquisition card is multiple sensors measurement module, sample frequency 1000Hz；The pumping rate of press is selected
0.1MPa/min.The measuring method comprises the following steps：
Step 1：Ultra-pure water is loaded in the seal groove 101 of back-off, and be completely filled with；In the present embodiment, in HTHP
Before experiment, first weigh with scale, draw the quality m of liquid under fluid chamber normal temperature and pressure0。
Step 2：The pressure of the compression system is adjusted to preset pressure value；Hydraulic test machine 104 is first turned on, is adjusted
Oil-feed and oil discharging valve, the pressure rise in ram cylinder is slowly set to be then shut off oil-feed and oil discharging valve, this step to 0.2MPa
Suddenly it is that the gap between the cylinder and sample cavity is reduced or eliminated, makes sealing tighter.
Step 3：Carry out being warming up to pre-set value to the compression system, and keep stable；
The heating system is switched on power, sets the temperature controller, adjusts the power transformer, makes described add
Pressure system is heated up with certain speed, and when temperature rises to setting value, keeping temperature is constant.
Step 4：Compression system pressurization is given, opens the measuring system while supercharging；
Required pressurization stages and pumping rate, the supercharging are set on the control panel of the hydraulic test machine 104
Process and pumping rate are mainly by the entering of pressure Frequency Converter Control Oil pump electrical machinery, drain the oil speed to complete；In the present embodiment
Oil pressure pumping rate is 0.10MPa/s, pressurization 0.2MPa-40MPa-0MPa；The measurement system is opened while supercharging
System, pressure curve and displacement curve are measured by data collecting card 302, and according to the pressure and the actual effect of displacement, provided
The corresponding relation of pressure and liquid thickness；And rule of thumb formula calculates the density of liquid liquid at different temperatures and pressures；
The preset temperature can be the series of temperature value of multiple temperature spots of required measurement；The present invention is by following equation by above-mentioned pressure
Power associates with density：
Search ultra-pure water initial density at normal temperatures and pressures, and by the data generation such as the initial mass of sample, change in displacement
Enter above formula, you can the density of measure ultra-pure water at different temperatures and pressures.
The density measurement of ultra-pure water and the absolute mean deviation with standard value under different pressures when table 1 gives 27 DEG C.
The absolute mean deviation of high-tension measurement result and standard value differs smaller within 1%, with standard value, the precision of high-tension measurement compared with
It is high.
Table 1
In addition, ultra-pure water provided by the present invention corresponding relation of pressure and density at 27 DEG C, is carried out according to experiment value
Fitting, can also establish the equation of state of water under high pressure；Therefore, the embodiments of the invention provide a kind of high-temperature high-pressure liquid volume density
Measuring method can be used for the measurement of the liquid equation of state.
Liquid in the embodiment of the present invention is ultra-pure water, and the liquid can also be that the fields such as oil, chemical industry need to measure
Other liquid of density.
Embodiment 2
Identical with the experimental method and step of the embodiment 1, the present embodiment measures ultra-pure water when temperature is 50 DEG C
Density value under different pressures, and compared with standard value.
Table 2 is the 50 DEG C of density values of ultra-pure water at various pressures and the absolute mean deviation with standard value.High-tension measurement
As a result the absolute mean deviation with standard value differs smaller within 1% with standard value, illustrates that high temperature of the present invention is high under high temperature
Press liquid density measuring equipment is more stable.
Table 2
Embodiment 3
Identical with the experimental method and step of the embodiment 1, the present embodiment measures ultra-pure water when temperature is 80 DEG C
Density value under different pressures, and compared with standard value.
Table 3
Table 3 is 80 DEG C of ultra-pure waters density value at various pressures and the absolute mean deviation of standard value, measured value and mark
The absolute mean deviation of quasi- value with standard value relatively, shows under HTHP that the high temperature in the present invention is high within 1%
Press liquid density measuring method is reliable.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (3)
1. a kind of high temperature high pressure liquid density measuring equipment, including compression system (1), heating system (2) and measuring system (3),
It is characterized in that：The compression system (1) includes hydraulic test machine (104), cylinder (103) and piston (102), seal box
(101) it is between upper and lower two pistons (102), seal box (101) is made up of upper cartridge body and lower box body, and upper cartridge body is in lower box
In vivo；The measuring system includes displacement transducer (301) and pressure sensor (303), and displacement transducer (301) is adopted with data
Truck (302) is connected, and pressure sensor (303) is connected with hydraulic test machine (104) oil cylinder, data collecting card (302), and data are adopted
Truck (302) is connected with control device (304), and the heating system (2) includes being arranged on the heating mantle of cylinder (103) outside
(201), heating mantle (201) is connected with power transformer (204), relay (203), relay (203) and temperature controller
(205) it is connected, temperature controller (205) is connected with thermocouple (202)；
Seal box is arranged in cylinder；Thermocouple in heating system is located at the cylinder top, for measuring the temperature of cylinder；
Measuring system includes " I " and " T " two pieces of steel crossbeams, is individually fixed in the end of the upper and lower piston of the piston cylinder, uses
In fixed institute displacement sensors.
2. high temperature high pressure liquid density measuring equipment according to claim 1, it is characterised in that：The seal box (101)
For metal or plastic seal box, the cylinder (103) is Talide cylinder.
3. a kind of high temperature high pressure liquid density measuring method, it is characterised in that carry out as steps described below：(1) by prepare liquid
Body loads in seal box (101), and is completely filled up, and weighs liquid quality m0, record seal box (101) internal diameter and depth；
(2) heating system (2) is opened, cylinder (103) is warming up to predetermined value, maintains temperature stabilization；
(3) compression system supercharging is opened, while measuring system is started working, collection pressure value and shift value change with time song
Line；
(4) calculate supercharging and heat rear fluid density
Wherein, m0For the initial mass of liquid,
R is the radius of cylinder,
Initial thickness after being converted for liquid sample volume,
S1It is the displacement that sample reduces in actually measuring on vertical direction,
S' is the bit shift compensation of systematic error,
For normal temperature and pressure fluid sample density；
Wherein, high temperature high pressure liquid density measuring equipment includes compression system (1), heating system (2) and measuring system (3), institute
Stating compression system (1) includes hydraulic test machine (104), cylinder (103) and piston (102), and seal box (101) is in upper and lower two
Between piston (102), seal box (101) is made up of upper cartridge body and lower box body, and upper cartridge body is in lower box body；The measuring system
Including displacement transducer (301) and pressure sensor (303), displacement transducer (301) is connected with data collecting card (302), pressure
Force snesor (303) is connected with hydraulic test machine (104) oil cylinder, data collecting card (302), data collecting card (302) and control
Device (304) is connected, and the heating system (2) includes being arranged on the heating mantle (201) of cylinder (103) outside, heating mantle (201) with
Power transformer (204), relay (203) are connected, and relay (203) is connected with temperature controller (205), temperature controller
(205) it is connected with thermocouple (202)；
Seal box is arranged in cylinder；Thermocouple in heating system is located at the cylinder top, for measuring the temperature of cylinder；
Measuring system includes " I " and " T " two pieces of steel crossbeams, is individually fixed in the end of the upper and lower piston of the piston cylinder, uses
In fixed institute displacement sensors.
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| CN201610022178.5A CN105571984B (en) | 2016-01-14 | 2016-01-14 | A kind of high temperature high pressure liquid density measuring equipment and measuring method |
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| CN201610022178.5A CN105571984B (en) | 2016-01-14 | 2016-01-14 | A kind of high temperature high pressure liquid density measuring equipment and measuring method |
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| CN105571984B true CN105571984B (en) | 2018-02-27 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4307609A (en) * | 1979-11-29 | 1981-12-29 | Noranda Mines Limited | Liquid density meter |
| US4745807A (en) * | 1986-11-06 | 1988-05-24 | Neill Timothy P O | Density meter for continuous fluid flow |
| CN2428769Y (en) * | 2000-05-19 | 2001-05-02 | 江汉石油学院 | High-temp. high-pressure PVT test instrument |
| CN2884196Y (en) * | 2005-11-21 | 2007-03-28 | 西南石油学院 | High-temp. and high-pressure drilling fluid density testing device |
| CN202562823U (en) * | 2012-04-25 | 2012-11-28 | 中国石油化工股份有限公司 | Compressible fluid high-temperature high-pressure density test system |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3176323B2 (en) * | 1997-07-07 | 2001-06-18 | 東京計装株式会社 | Method and apparatus for measuring density of liquid in tank |
-
2016
- 2016-01-14 CN CN201610022178.5A patent/CN105571984B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4307609A (en) * | 1979-11-29 | 1981-12-29 | Noranda Mines Limited | Liquid density meter |
| US4745807A (en) * | 1986-11-06 | 1988-05-24 | Neill Timothy P O | Density meter for continuous fluid flow |
| CN2428769Y (en) * | 2000-05-19 | 2001-05-02 | 江汉石油学院 | High-temp. high-pressure PVT test instrument |
| CN2884196Y (en) * | 2005-11-21 | 2007-03-28 | 西南石油学院 | High-temp. and high-pressure drilling fluid density testing device |
| CN202562823U (en) * | 2012-04-25 | 2012-11-28 | 中国石油化工股份有限公司 | Compressible fluid high-temperature high-pressure density test system |
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