CN105571984A - High-temperature and high-pressure liquid density measuring device and method - Google Patents
High-temperature and high-pressure liquid density measuring device and method Download PDFInfo
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- CN105571984A CN105571984A CN201610022178.5A CN201610022178A CN105571984A CN 105571984 A CN105571984 A CN 105571984A CN 201610022178 A CN201610022178 A CN 201610022178A CN 105571984 A CN105571984 A CN 105571984A
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N9/04—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity by measuring weight of a known volume of fluids
Abstract
The invention provides a high-temperature and high-pressure liquid density measuring device and method. The system comprises a pressurizing system, a heating system and a measuring system. The pressurizing system comprises a hydraulic test machine, a cylinder and pistons. A sealing box is located between the upper piston and the lower piston. The measuring system comprises a displacement sensor and a pressure sensor. The displacement sensor is connected with a data acquisition card. The pressure sensor is connected with an oil cylinder of the hydraulic test machine and the data acquisition card. The data acquisition card is connected with a control device. The heating system comprises a heating sleeve arranged outside the cylinder. The heating sleeve is connected with a power transformer and a relay. The relay is connected with a temperature controller. The temperature controller is connected with a thermocouple. The measuring range of the high-temperature and high-pressure liquid density measuring device is much larger than that of an existing high-pressure density device, the high-temperature and high-pressure liquid density measuring device is easy to operate, high in precision and good in repeatability, the pressure range of the density of measured liquid is greatly enlarged, the sealing performance and repeatability of the system are improved, and effectiveness and continuity of a measuring result are improved.
Description
Technical field
The invention belongs to liquid key property fields of measurement at extreme pressure and temperature, be specifically related to a kind of measurement mechanism and measuring method of high-temperature high-pressure liquid volume density.
Background technology
Density is a kind of very important physical quantity in the physicochemical property of material, and particularly for liquid, the macro property such as viscosity, refractive index, diffusion of density and liquid is closely related.Therefore, the density parameter of Measurement accuracy liquid under reactiveness and situation of change thereof, for expand different liquids produce and application in life significant.Along with the development of the resources explorations such as marine oil, more and more urgent to the demand of the device measuring fluid density under high-temperature and high-pressure conditions.In addition, in scientific research, the excellent properties that some fluent materials show at high temperature under high pressure, also makes researcher create keen interest to the measurement of fluid density under High Temperature High Pressure and method thereof.But because High Temperature High Pressure belongs to extreme condition, fluent material easily leaks, realize the measurement of fluid density under this extreme condition relatively difficult, corresponding device is also less.
The high-temp. high-pressure PVT test instrument of liquid PVT relation is measured under utility model patent (CN00233404.6) proposes a kind of High Temperature High Pressure, principal feature is that under can carrying out High Temperature High Pressure, PVT measures, but the temperature (room temperature-230 DEG C) be suitable for and pressure limit less (0.1-25MPa), be not suitable for more wide region examination oil density; Utility model patent (CN201653848U) proposes a kind of measurement mechanism and measuring method of high-temperature high pressure oil quality density, mainly improve for High Temperature High Pressure PVT measuring instrument, can realize measuring temperature from 100 DEG C-550 DEG C, pressure is from the density measure of the different liquid-phase products of 0.1MPa-25MPa.But measuring upper limit of pressure is still 25MPa, be not suitable for wider pressure limit examination fluid density, and complex structure, process are loaded down with trivial details.
Summary of the invention
The object of the invention is for above-mentioned the deficiencies in the prior art, propose a kind of high temperature high pressure liquid density measuring equipment and measuring method.
Technical scheme of the present invention is achieved in that a kind of high temperature high pressure liquid density measuring equipment, comprise compression system, heating system and measuring system, described compression system comprises hydraulic test machine, cylinder and piston, seal box is between upper and lower two pistons, seal box is made up of upper cartridge body and lower box body, and upper cartridge body is in lower box body; Described measuring system comprises displacement transducer and pressure transducer, displacement transducer is connected with data collecting card, pressure transducer is connected with hydraulic test Oil cylinder, data collecting card, data collecting card is connected with control device, described heating system comprises the heating jacket be arranged on outside cylinder, heating jacket is connected with power transformer, relay, and relay is connected with temperature controller, and temperature controller is connected with thermopair.
Described seal box is metal or plastic seal box, and described cylinder is carboloy cylinder.
A kind of high temperature high pressure liquid density measuring method, carries out according to following step: testing liquid loads in seal box by (1), and fills completely, takes liquid quality m
0, the record internal diameter of seal box and the degree of depth;
(2) open heating system, cylinder is warming up to predetermined value, holding temperature is stablized;
(3) open compression system supercharging, measuring system is started working simultaneously, gathers force value and shift value curve over time;
(4) calculate supercharging and heat rear fluid density
Wherein, m
0for the initial mass of liquid,
R is the radius of cylinder,
for the initial thickness after liquid sample volume conversion,
S
1the displacement that sample in actual measurement, vertical direction reduces,
S' is the bit shift compensation of systematic error,
for normal temperature and pressure fluid sample density.
Present invention achieves the measurement of fluid density under high-temperature and high-pressure conditions, highest measurement temperature is 500 DEG C, and maximum measurement pressure is 1000MPa, much larger than the measurement range (25MPa) of existing high-density device; And simple to operate, degree of accuracy is high, favorable reproducibility; Device have employed piston cylinder mechanical supercharged, breaches the pressure limit of fluid pressurization, substantially increases the pressure limit measuring fluid density; Adopt polytetrafluoroethylmaterial material as encapsulant, be conducive to sealing and the repeatability of raising system; Measuring system adopts kinetic measurement pattern, improves actual effect and the continuity of measurement result.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is 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 machine, 2. heating systems, 201. heating jackets, 202. thermopairs, 203. relays, 204. power transformers, 205. temperature controllers, 3. measuring system, 301. displacement transducer, 302. data collecting cards, 303. pressure transducers, 304. control device.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not paying the every other embodiment obtained under creative work prerequisite, 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, comprise compression system 1, heating system 2 and measuring system 3, described compression system 1 comprises hydraulic test machine 104, cylinder 103 and piston 102, seal box 101 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 body; Described measuring system 3 comprises displacement transducer 301 and pressure transducer 303, displacement transducer 301 is connected with data collecting card 302, pressure transducer 303 is connected with hydraulic test machine 104 oil cylinder, data collecting card 302, data collecting card 302 is connected with control device 304, described heating system 2 comprises the heating jacket 201 be arranged on outside cylinder 103, heating jacket 201 is connected with power transformer 204, relay 203, relay 203 is connected with temperature controller 205, and temperature controller 205 is connected with thermopair 202.
Wherein, compression system 1 is for receiving fluids and for liquid carrying is for hyperbaric environment; Heating system 2 is for supplying stable hot environment for liquid carrying; Measuring system 3 is for measuring the change of liquid volume in pressurization.
Described seal box 101 is metal or plastic seal box, such as adopts aluminium, copper, teflon or nylon etc., and described cylinder 103 is carboloy cylinder, and drum diameter is 16,20,22 or 26mm.
The hydraulic test machine 104 used in the application is top, two sides hydropress, and maximum working load 2000KN, maximum functional distance is 400mm, and pumping rate is 0.1-10MPa/min, preferred 0.1MPa/min.The resistance wire material of the heating jacket 201 of the resistance-type in heating system 2 can be Aludirome, nickel chromium triangle electrothermal alloy, preferred nickel chromium triangle electrothermal alloy, and peak power is 2500-3000kW.Thermopair 202 is K type probe thermopair, measurement range 0-1300 DEG C; Power transformer 204 is 220V/5kW single 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 controller, sample period 0.5s, fuzzy-adaptation PID control, resolution 1 DEG C, 0.1 DEG C.
Displacement transducer 301 in described measuring system is high precision contact digital displacement sensor and non-contacting Laser Displacement sensor, preferred contact digital displacement sensor, effective range >12mm, resolution >0.1 μm, mechanical response 10Hz; Pressure transducer 303 is digital pressure sensor, resolution <0.01MPa, Best-case Response Time <3ms; Data collecting card 302 is the multiple sensors measurement module that directly can connect all kinds sensor, sample frequency >960Hz, and independently numeral exports and input channel; The measurement mechanism heatproof upper limit is 500 DEG C, and the withstand voltage upper limit is 1000MPa, and control device adopts computing machine.
Thermopair in heating system is positioned at described cylinder top, and for measuring the temperature of cylinder, thermopair and piston lateral separation 3-5cm, be preferably 4cm, fore-and-aft distance 20-30cm, is preferably 25cm.Described measuring system comprises " I " and " T " two pieces of steel crossbeams, is individually fixed in the end of the upper and lower piston of described piston cylinder, for fixing institute displacement sensors.
Time the present invention uses, first liquid is full of in whole seal box 101, then the pressure of compression system is increased to scheduled pressure value; Open heating system, for liquid carries out being warming up to predetermined temperature value, and keep constant; Open measuring system, the pumping rate of setting hydraulic test machine 104 carries out stable pressurization to cylinder, adopt the changing value of data collecting card 302 recorded bit displacement sensor 301 and pressure transducer 303 simultaneously, according to the relation of the quality of liquid under initial environment, volume and displacement and density, the corresponding relation of fluid sample pressure and density at a certain temperature can be set up, be given in measuring tempeature and measure the density value of liquid under pressure.
High temperature high pressure liquid density measuring method of the present invention, carry out according to following step:
(1) testing liquid is loaded in seal box 101, and fill completely, take liquid quality m
0, the record internal diameter of seal box 101 and the degree of depth;
(2) open heating system 2, cylinder 103 is warming up to predetermined value, holding temperature is stablized;
(3) open compression system supercharging, measuring system is started working simultaneously, gathers force value and shift value curve over time;
(4) calculate supercharging and heat rear fluid density
Wherein, m
0for the initial mass of liquid,
R is the radius of cylinder,
for the initial thickness after liquid sample volume conversion,
S
1the displacement that sample in actual measurement, vertical direction reduces,
S' is the bit shift compensation of systematic error,
for normal temperature and pressure fluid sample density.
Present invention achieves the measurement to fluid density under high-temperature and high-pressure conditions, easy to operate, degree of accuracy is high, favorable reproducibility; Compression system adopts drum equipment to seal, and in conjunction with hydraulic test machine, the high pressure range of fluid density ranges up to 1000MPa; Device adopts Resistant heating cover for liquid carrying is for hot environment, and the temperature range of fluid density ranges up to 500 DEG C, and the pressure and temperature measurable range of liquid density measurement device has exceeded existing means of testing.
Embodiment 1
Present embodiments provide a kind of high temperature high pressure liquid density measuring method, this method of testing uses the high temperature high pressure liquid density measuring equipment in Fig. 1 ~ 4 to measure.Wherein, in experimental provision, seal box adopts teflon material; Diameter is selected to be the wimet cylinder of 20cm; Heating jacket selects resistance wire power to be 2500W; K type thermocouple temperature measurement scope 0-1300 DEG C, with piston lateral separation 4cm, fore-and-aft distance is 25cm; Temperature controller resolution 0.1 DEG C; Displacement sensor scope is 12mm, and resolution is 0.1 μm, mechanical response 10Hz; The resolution of digital pressure sensor is 0.01MPa, and Best-case Response Time is 3ms; Data signal acquisition card is multiple sensors measurement module, and sample frequency is 1000Hz; The pumping rate of press selects 0.1MPa/min.Described measuring method comprises the following steps:
Step 1: ultrapure water is loaded in the seal groove 101 of back-off, and be full of completely; In the present embodiment, before high temperature and pressure experiment, first weigh with scale, draw the quality m of liquid under fluid chamber normal temperature and pressure
0.
Step 2: the pressure of described compression system is adjusted to preset pressure value; First hydraulic test machine 104 is opened, regulate oil-feed and oil discharging valve, slowly make the pressure in ram cylinder be increased to 0.2MPa, then close oil-feed and oil discharging valve, this step is reduced in the gap between described cylinder and sample cavity or eliminates, and makes sealing tighter.
Step 3: carry out being warming up to pre-set value to described compression system, and keep stable;
Described heating system is switched on power, sets described temperature controller, regulate described power transformer, described compression system is heated up with certain speed, when temperature rises to setting value, keep temperature-resistant.
Step 4: pressurize to described compression system, opens described measuring system while supercharging;
The control panel of described hydraulic test machine 104 sets required pressurization stages and pumping rate, and described pressurization and pumping rate have mainly been come by the entering of pressure Frequency Converter Control Oil pump electrical machinery, the speed of draining the oil; In the present embodiment, oil pressure pumping rate is 0.10MPa/s, and pressurization is 0.2MPa-40MPa-0MPa; Open described measuring system while supercharging, measure pressure curve and displacement curve by data collecting card 302, and according to the actual effect of described pressure and displacement, provide the corresponding relation of pressure and liquid thickness; And rule of thumb formula calculates the density of liquid liquid at different temperatures and pressures; Described preset temperature can be the series of temperature value of the required multiple temperature spots measured; Above-mentioned pressure is associated with density by following formula by the present invention:
Search ultrapure water initial density at normal temperatures and pressures, and the data such as the initial mass of sample, change in displacement are substituted into above formula, ultrapure water density at different temperatures and pressures can be measured.
The density measurement of ultrapure 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, within 1%, differs less with standard value, and the precision of high-tension measurement is higher.
Table 1
In addition, the corresponding relation of ultrapure water provided by the present invention pressure and density 27 DEG C time, experimentally value carries out matching, also can set up the water equation of state under high pressure; Therefore, the measurement that a kind of high temperature high pressure liquid density measuring method can be used for the liquid equation of state is embodiments provided.
Liquid in the embodiment of the present invention is ultrapure water, and described liquid also can be other liquid that the field such as oil, chemical industry needs density measurement.
Embodiment 2
Identical with step with the experimental technique of described embodiment 1, the present embodiment measures the density value of ultrapure water when temperature is 50 DEG C under different pressures, and compares with standard value.
Table 2 is 50 DEG C of ultrapure waters density value at various pressures and the absolute mean deviation with standard value.The absolute mean deviation of high-tension measurement result and standard value, within 1%, differs less with standard value, illustrates that in the present invention, high temperature high pressure liquid density measuring equipment is more stable under high temperature.
Table 2
Embodiment 3
Identical with step with the experimental technique of described embodiment 1, the present embodiment measures the density value of ultrapure water when temperature is 80 DEG C under different pressures, and compares with standard value.
Table 3
Table 3 is 80 DEG C of ultrapure waters density value at various pressures and the absolute mean deviation of standard value, the absolute mean deviation of measured value and standard value is within 1%, with standard value relatively, under showing High Temperature High Pressure, the high temperature high pressure liquid density measuring method in the present invention is reliable.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. a high temperature high pressure liquid density measuring equipment, comprise compression system (1), heating system (2) and measuring system (3), it is characterized in that: described compression system (1) comprises hydraulic test machine (104), cylinder (103) and piston (102), seal box (101) 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 body, described measuring system comprises displacement transducer (301) and pressure transducer (303), displacement transducer (301) is connected with data collecting card (302), pressure transducer (303) and hydraulic test machine (104) oil cylinder, data collecting card (302) is connected, data collecting card (302) is connected with control device (304), described heating system (2) comprises and is arranged on cylinder (103) heating jacket outward (201), heating jacket (201) and power transformer (204), relay (203) is connected, relay (203) is connected with temperature controller (205), temperature controller (205) is connected with thermopair (202).
2. high temperature high pressure liquid density measurement system according to claim 1, is characterized in that: described seal box (101) is metal or plastic seal box, and described cylinder (103) is carboloy cylinder.
3. a high temperature high pressure liquid density measuring method, it is characterized in that carrying out according to following step:
(1) testing liquid is loaded in seal box (101), and fill completely, take liquid quality m
0, record seal box (101) internal diameter and the degree of depth;
(2) open heating system (2), cylinder (103) is warming up to predetermined value, holding temperature is stablized;
(3) open compression system supercharging, measuring system is started working simultaneously, gathers force value and shift value curve over time;
(4) calculate supercharging and heat rear fluid density
Wherein, m
0for the initial mass of liquid,
R is the radius of cylinder,
for the initial thickness after liquid sample volume conversion,
S
1the displacement that sample in actual measurement, vertical direction reduces,
S' is the bit shift compensation of systematic error,
for normal temperature and pressure fluid sample density.
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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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| Application Number | Priority Date | Filing Date | Title |
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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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| CN105571984A true CN105571984A (en) | 2016-05-11 |
| CN105571984B CN105571984B (en) | 2018-02-27 |
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Citations (6)
| 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 |
| JPH1123443A (en) * | 1997-07-07 | 1999-01-29 | Tokyo Keiso Co Ltd | Method and equipment for measuring density of liquid in tank |
| 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 |
-
2016
- 2016-01-14 CN CN201610022178.5A patent/CN105571984B/en active Active
Patent Citations (6)
| 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 |
| JPH1123443A (en) * | 1997-07-07 | 1999-01-29 | Tokyo Keiso Co Ltd | Method and equipment for measuring density of liquid in tank |
| 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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