CN107817264B - Automatic inclination point detector by controllable temperature difference method - Google Patents
Automatic inclination point detector by controllable temperature difference method Download PDFInfo
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- CN107817264B CN107817264B CN201711207023.XA CN201711207023A CN107817264B CN 107817264 B CN107817264 B CN 107817264B CN 201711207023 A CN201711207023 A CN 201711207023A CN 107817264 B CN107817264 B CN 107817264B
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- 238000000034 method Methods 0.000 title claims abstract description 21
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 239000003921 oil Substances 0.000 abstract description 68
- 238000001514 detection method Methods 0.000 abstract description 19
- 239000007788 liquid Substances 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 4
- 239000010779 crude oil Substances 0.000 abstract description 2
- 239000000295 fuel oil Substances 0.000 abstract description 2
- 239000010687 lubricating oil Substances 0.000 abstract description 2
- 239000003208 petroleum Substances 0.000 abstract description 2
- 238000009434 installation Methods 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 108010085603 SFLLRNPND Proteins 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 239000003209 petroleum derivative Substances 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001028 reflection method Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/04—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of melting point; of freezing point; of softening point
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Abstract
An automatic inclination point detector using a controllable temperature difference method belongs to the technical field of petroleum pour point automatic detection. The center temperature sensor extends into the oil sample to be measured, and the first temperature sensor and the second temperature sensor are not contacted with the oil sample to be measured. The first micro-heater and the second micro-heater always keep the temperature of the sensor on the oil surface higher than the temperature of the sensor in the oil by more than 2 ℃. At pour point detection, the tube is tilted. If the oil sample flows, the sensor on the liquid surface can touch the oil sample with the temperature lower than the sensor on the liquid surface, and the instantaneous temperature immediately drops by more than 0.5 ℃ in a few seconds. Conversely, if the oil sample does not flow, the instantaneous temperature will not drop suddenly. In other words, if the test tube is inclined and the temperature of the sensor above the oil sample is suddenly changed, it can be judged whether the oil sample flows. The oil sample is in the range of plus 50 ℃ to minus 80 ℃, the detection is sensitive, and the work is extremely reliable. The detector has simple structure and easy installation and debugging; the detection process is irrelevant to oil products. Can be suitable for detecting various oil products such as crude oil, fuel oil, lubricating oil and the like.
Description
Technical Field
The invention relates to an automatic pour point detector by a controllable temperature difference method, which belongs to the technical field of petroleum pour point automatic detection.
Background
Petroleum and petroleum products are known as pour points at the lowest temperature at which they can flow in the low temperature regime.
Pour points were measured by tube tilting according to ISO3016 ASTM D97, IP27, GB/T3535 standard. Currently, pour point automatic detectors are mainly optically detected: such as optical fiber reflection method, high-order photoelectric method, liquid level image pickup method, etc. The disadvantages of these methods are: at lower temperature, the liquid level contracts and is uneven, and the detection effect is affected. In particular, moisture condensation on the detector surface at low temperatures severely affects measurement sensitivity and reliability.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides an automatic inclination point detector by a controllable temperature difference method, and the inclination point detector always keeps the temperature of a sensor on an oil surface to be higher than the temperature of a sensor in oil by more than 2 ℃ in the process of cooling a test tube oil sample. At pour point detection, the tube is tilted. If the oil sample flows, the sensor on the liquid surface will hit the oil sample with a temperature lower than that of the oil sample, and the instant temperature immediately drops by more than 0.5 ℃ within a few seconds. Conversely, if the oil sample does not flow, the instantaneous temperature will not drop suddenly. In other words, if the test tube is inclined and the temperature of the sensor above the oil sample is suddenly changed, whether the oil sample flows or not can be judged, and the key point of the pour point detection of the temperature difference method is that.
The technical scheme adopted by the invention is as follows: an automatic tilting point detector by a controllable temperature difference method comprises a test tube, a cold trap temperature sensor arranged in the cold trap, an oil sample to be detected, the cold trap, a Programmable Logic Controller (PLC) and a refrigerating device, and also comprises a central temperature sensor, a first temperature sensor, a second temperature sensor, a first micro heater and a second micro heater; the test tube is placed in the cold trap, the central temperature sensor penetrates through the test tube plug to extend into an oil sample to be tested in the test tube, the first temperature sensor penetrates through the test tube plug to extend into the test tube near the central temperature sensor, a first micro heater is arranged at the end part of the first temperature sensor, the second temperature sensor penetrates through the test tube plug to extend into the test tube near the inner wall of the test tube, and a second micro heater is arranged at the end part of the second temperature sensor; the first temperature sensor, the first micro heater, the second temperature sensor and the second micro heater are not contacted with the oil sample to be tested in the test tube; the first temperature sensor, the first micro heater, the second temperature sensor, the second micro heater and the cold trap temperature sensor are electrically connected with a programmable controller PLC, and the programmable controller PLC is electrically connected with the printer through the touch screen; the refrigeration device provides cold energy to the cold trap.
The first temperature sensor, the first micro heater and the second temperature sensor are micro platinum resistance temperature sensors.
The beneficial effects of the invention are as follows: the center temperature sensor is stretched into the oil sample to be measured in the test tube by the automatic tilting point detector with the controllable temperature difference method, and the first temperature sensor and the second temperature sensor are not contacted with the oil sample to be measured in the test tube. The first micro-heater and the second micro-heater always keep the temperature of the sensor on the oil surface higher than the temperature of the sensor in the oil by more than 2 ℃. At pour point detection, the tube is tilted. If the oil sample flows, the sensor on the liquid surface can touch the oil sample with the temperature lower than the sensor on the liquid surface, and the instantaneous temperature immediately drops by more than 0.5 ℃ in a few seconds. Conversely, if the oil sample does not flow, the instantaneous temperature will not drop suddenly. In other words, if the test tube is inclined and the temperature of the sensor above the oil sample is suddenly changed, whether the oil sample flows or not can be judged, and the key point of the pour point detection of the temperature difference method is that. The oil sample is detected sensitively and works extremely reliably within the full range of plus 50-minus 80 ℃. The detector body has simple structure and is easy to install and debug; the detection process is irrelevant to the viscosity, color and variety of the oil sample. Can be suitable for detecting various oil products such as crude oil, fuel oil, lubricating oil and the like.
Drawings
FIG. 1 is a schematic diagram of a controllable differential temperature process automatic tip detector.
FIG. 2 is a schematic diagram of the flow of an oil sample when the tube is tilted at an angle of 45 degrees.
FIG. 3 is a schematic diagram of the solidification of an oil sample when the tube is tilted at an angle of 45 degrees.
Fig. 4 is a schematic diagram of oil-like solidification when the tube is tilted at an angle of 90 degrees.
In the figure: 1. the central temperature sensor, 2, the first temperature sensor, 3, the second temperature sensor, 4, the first micro heater, 5, the second micro heater, 6, the test tube, 7, the cold trap temperature sensor, 8, the oil sample that awaits measuring, 9, the cold trap.
Detailed Description
Fig. 1 shows a schematic diagram of a controllable differential-temperature automatic tilt detector. In the figure, the automatic tilting point detector using the controllable temperature difference method comprises a test tube 6, a cold trap temperature sensor 7 arranged in a cold trap 9, an oil sample 8 to be tested, the cold trap 9, a programmable controller PLC, a refrigerating device, a central temperature sensor 1, a first temperature sensor 2, a second temperature sensor 3, a first micro heater 4 and a second micro heater 5. The test tube 6 is placed in the cold trap 9, and in the central temperature sensor 1 passed the test tube stopper and stretched into the test tube 6 the oil sample 8 that awaits measuring, first temperature sensor 2 is close to central temperature sensor 1 and stretches into in the test tube 6 through the test tube stopper to be equipped with first micro-heater 4 at the tip of first temperature sensor 2, second temperature sensor 3 is close to the inner wall of test tube 6 and stretches into in the test tube 6 through the test tube stopper, and is equipped with second micro-heater 5 at the tip of second temperature sensor 3. The first temperature sensor 2, the first micro-heater 4, the second temperature sensor 3 and the second micro-heater 5 do not contact the oil sample 8 to be measured in the test tube 6. The first temperature sensor 2, the first micro heater 4, the second temperature sensor 3, the second micro heater 5 and the cold trap temperature sensor 7 are electrically connected with a programmable controller PLC, and the programmable controller PLC is electrically connected with a printer through a touch screen. The refrigeration device provides cold to the cold trap 9. The first temperature sensor 2, the first micro heater 4 and the second temperature sensor 3 are micro platinum resistance temperature sensors.
By adopting the technical scheme, a pour point test tube is placed in the cold trap, three miniature platinum resistance temperature sensors are arranged in the test tube, one sensor is arranged in the oil sample, and the other two sensors are not contacted with the oil surface. The outer wall of the metal bath is provided with a worm gear and worm transmission mechanism (not shown in the figure), the cold trap drives the test tube to rotate by an angle of 45 degrees and an angle of 90 degrees under the drive of a motor, two micro heaters are arranged in the test tube, the heating power of each micro heater is only 0.25W, and the micro heaters have no influence on the temperature reduction of an oil sample during heating. The main purpose of the micro heater is that the temperature is in the first half of the measuring range of plus 50 ℃ to minus 80 ℃, namely plus 50 ℃ to minus 15 ℃, the heater is heated under the control of an electronic circuit, so that the temperature of three temperature sensors is reduced rapidly under the action of a refrigerator, and simultaneously, the temperature of two sensors on the oil surface is synchronously higher than the instant temperature of an oil sample by 2 ℃ or more than 2 ℃ due to the micro heating effect. Because of the existence of the temperature difference, the inclination detector can sensitively and reliably work within the range.
In the range of the pour point temperature of plus 50 ℃ to minus 80 ℃, the temperature difference detection can be implemented only if the temperature of the oil sample is below minus 15 ℃ and the temperature of the sensor on the oil surface is higher than the temperature of the oil sample by more than 2 ℃. In the first half of the temperature range, the temperature of the air in the test tube is reduced rapidly, and then the temperature is gradually reduced, at the moment, the air temperature is lower than the temperature of the oil sample, then the air temperature is equal to the temperature of the oil sample, the change state cannot be detected by a temperature difference method, and a micro heating plate is arranged for heating, so that two temperature sensors on the oil surface are synchronously higher than the instant temperature of the temperature sensors in the oil by more than 2 ℃, and therefore, in the first half of the measuring range, the detector can also sensitively and reliably work, which is the core of the controllable temperature difference method inclination detector.
The three resistors of the pour point controllable temperature difference detector and the cold trap sensor are connected into a temperature module of a programmable controller PLC, the temperature of the first temperature sensor and the temperature of the second temperature sensor are controlled by the PLC, the temperature of the first temperature sensor and the temperature of the second temperature sensor are higher than 2 ℃ of the central temperature sensor in the oil sample, the programmable controller PLC is connected with a touch screen and a printer, and the cold trap is connected with a refrigerating device. The pour point glass test tube has a thicker inner diameter, and the oil sample near the outer wall of the test tube is solidified firstly and finally at the center position on the oil sample when the temperature is reduced. To prevent detection errors, the pour point has two detection sensors, and the programmable controller PLC judges that the test is finished only when the two detection sensors detect that the oil sample does not flow. When the pour point of the oil sample is actually detected, the pour point temperature is set on the touch screen, for example, minus 36 ℃, when the oil temperature is reduced to minus 36 ℃, the cold trap automatically tilts by 45 degrees (shown in figure 2), and at the moment, as long as any one detection sensor touches the oil sample, the instant temperature will be suddenly changed, so that the oil sample still flows and is not solidified. Then, the programmable controller PLC outputs a signal, the test tube is reset to be vertical, and the next detection point is waited. The temperature of the oil sample is reduced to minus 39 ℃ (interval 3 ℃), the test tube is inclined again for 45 degrees, at the moment, if the temperature of the detection sensor is not suddenly changed (as shown in fig. 3), the oil sample is not flowing, the programmable controller PLC outputs a signal, the test tube is inclined for 90 degrees (as shown in fig. 4), the time is delayed for 5 seconds, after 5 seconds, if the instant temperature of the first temperature sensor is not suddenly changed, the oil sample is thoroughly solidified, and the test is ended. Otherwise, the temperature of the first temperature sensor suddenly changes to indicate that the central oil sample above the oil sample still flows, the test tube is reset, and the next detection point is waited. When the oil temperature was reduced to minus 42 ℃, the above procedure was repeated. And only when the temperature of the first temperature sensor is not suddenly changed, the test is finished, and the printer automatically prints the test result.
Claims (2)
1. The utility model provides an automatic tipping detector with controllable difference in temperature method, it includes test tube (6), sets up cold trap temperature sensor (7) in cold trap (9), await measuring oil appearance (8), cold trap (9), programmable controller PLC and refrigerating plant, characterized by: the device also comprises a central temperature sensor (1), a first temperature sensor (2), a second temperature sensor (3), a first micro heater (4) and a second micro heater (5); the test tube (6) is placed in the cold trap (9), the central temperature sensor (1) penetrates through the test tube plug to extend into an oil sample (8) to be tested in the test tube (6), the first temperature sensor (2) is close to the central temperature sensor (1) and penetrates through the test tube plug to extend into the test tube (6), a first micro heater (4) is arranged at the end part of the first temperature sensor (2), the second temperature sensor (3) is close to the inner wall of the test tube (6) and penetrates through the test tube plug to extend into the test tube (6), and a second micro heater (5) is arranged at the end part of the second temperature sensor (3); the first temperature sensor (2), the first micro heater (4), the second temperature sensor (3) and the second micro heater (5) are not contacted with the oil sample (8) to be detected in the test tube (6); the first temperature sensor (2), the first micro heater (4), the second temperature sensor (3), the second micro heater (5) and the cold trap temperature sensor (7) are electrically connected with a programmable controller PLC, and the programmable controller PLC is electrically connected with a printer through a touch screen; the refrigerating device provides cold energy for the cold trap (9).
2. An automatic inclination detector according to claim 1, characterized by: the first temperature sensor (2) and the second temperature sensor (3) are miniature platinum resistance temperature sensors.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711207023.XA CN107817264B (en) | 2017-11-27 | 2017-11-27 | Automatic inclination point detector by controllable temperature difference method |
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| CN201711207023.XA CN107817264B (en) | 2017-11-27 | 2017-11-27 | Automatic inclination point detector by controllable temperature difference method |
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| CN107817264A CN107817264A (en) | 2018-03-20 |
| CN107817264B true CN107817264B (en) | 2023-10-31 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114563439B (en) * | 2022-04-08 | 2023-11-03 | 北京华科仪科技股份有限公司 | Pour point congeals some measuring device |
| CN114563440B (en) * | 2022-04-08 | 2023-09-12 | 北京华科仪科技股份有限公司 | Pour point measuring method |
| CN118655172B (en) * | 2024-08-22 | 2024-10-25 | 江西省检验检测认证总院工业产品检验检测院 | Pour point and congeal point measuring device |
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