阅读说明：本技术 测定粘稠物质沸点的试验装置及其用途 (Test device for measuring boiling point of viscous substance and application thereof ) 是由 吴保意 王双全 郭璐 于 2019-04-04 设计创作，主要内容包括：本发明涉及一种测定粘稠物质沸点的试验装置及其用途,主要解决现有技术中测试结果不准确的问题。本发明通过采用一种测定粘稠物质沸点的试验装置,包括低温模块、高温模块、测试管、压力传感器,低温模块正中部为制冷器,制冷器两侧为测试管座孔,制冷器上方为贮液池,贮液池与测试管座孔上部连通；高温模块为沸点测试模块,正中部为加热器,测试管座孔设置在制冷器和高温模块上,测试管上部有抽真空部件,抽真空部件上有真空泵管接入孔,真空泵管接入孔与测试管内部连通,压力传感器为椎体形,插在测试管上方的技术方案较好地解决了上述问题,可用于测定粘稠物质沸点的试验中。(The invention relates to a test device for measuring the boiling point of a viscous substance and application thereof, and mainly solves the problem of inaccurate test result in the prior art. The invention adopts a test device for measuring the boiling point of viscous substances, which comprises a low-temperature module, a high-temperature module, a test tube and a pressure sensor, wherein a refrigerator is arranged in the middle of the low-temperature module, test tube seat holes are formed in two sides of the refrigerator, a liquid storage tank is arranged above the refrigerator, and the liquid storage tank is communicated with the upper part of the test tube seat holes; the high temperature module is boiling point test module, and the heater is just middle part, and the test tube seat hole sets up on refrigerator and high temperature module, and there is the evacuation part test tube upper portion, has the vacuum pump pipe access hole on the evacuation part, and vacuum pump pipe access hole and test tube inside intercommunication, pressure sensor are centrum shape, insert the technical scheme who glues the pipe top and solved above-mentioned problem betterly, can be used to the experiment of survey ropy material boiling point.)

1. A test device for measuring the boiling point of viscous materials comprises a low-temperature module, a high-temperature module, a test tube and a pressure sensor, wherein a refrigerator is arranged in the middle of the low-temperature module, test tube seat holes are formed in two sides of the refrigerator, a liquid storage tank is arranged above the refrigerator, and the liquid storage tank is communicated with the upper part of the test tube seat holes; the high-temperature module is a boiling point test module, the middle part of the high-temperature module is a heater, the interior of the heater is divided into two parts, two different temperatures can be respectively controlled, and the temperature stability of the two parts can be ensured; the test tube seat hole is arranged on the refrigerator and the high-temperature module, and silicone oil needs to be added into the test tube seat hole during testing; the upper portion of the test tube is provided with a vacuumizing part, the vacuumizing part is provided with a vacuum pump tube access hole, the vacuum pump tube access hole is communicated with the inside of the test tube, the pressure sensor is in a cone shape, the diameter of the upper portion of the vacuum pump tube access hole is larger than that of the lower portion of the vacuum pump tube access hole, the upper portion of the vacuum pump tube access hole is inserted above the test tube, the inside of the pressure sensor is hollow, the side portion of the lower portion of the vacuum pump tube access hole is provided.

2. The test apparatus for determining the boiling point of a viscous material according to claim 1, wherein in the test for determining the boiling point of a viscous material, the characteristic that the saturated vapor pressure of the viscous material is small under a low temperature condition is utilized to perform air tightness detection on the test system under the low temperature condition, then the test system is placed at a constant temperature under the test temperature, the saturated vapor pressure of the sample at the boiling temperature is detected by vacuumizing the system and performing data processing, a constant A, B is obtained by two sets of the temperature and the pressure at the boiling temperature and the relationship lgP between the boiling point T and the pressure P, and finally the boiling point of the sample under the atmospheric pressure of the test environment is reversely pushed according to the atmospheric pressure of the test environment.

3. The test device for measuring the boiling point of the viscous substance according to claim 1, wherein the temperature control range of the low-temperature module is-20 ℃ to 0 ℃, and the temperature precision is as follows: plus or minus 0.1 ℃; the temperature control range of the high-temperature module is 30-150 ℃.

4. The apparatus as claimed in claim 1, wherein the two holes are provided on the refrigerator and the high temperature module, and a proper amount of silicone oil is added to the holes to make the tubes heated uniformly.

5. The apparatus for testing boiling point of viscous material according to claim 1, wherein the test tubes are made of glass, and have two shapes, the shape of the test tubes is identical to that of a common test tube, the ratio of the length of the part below the vacuum-pumping part to the total length is 1:1-1.4, and the internal volumes of the two test tubes are identical and need to be calibrated.

6. The test device for measuring the boiling point of the viscous material according to claim 1, wherein the pressure sensors are made of stainless steel, have two conical shapes, have a pressure measurement range of 0 to 100kPa and a precision of +/-1 Pa, and have a ratio of the diameter of the upper part to the diameter of the lower part of 1:0.2 to 0.6.

7. The apparatus as claimed in claim 1, wherein the pressure sensor is inserted into the test tube during the test, the test tube is connected to the pressure sensor and inserted into the hole of the test tube, the low temperature module, the high temperature module and the pressure sensor are connected to the test software, and the software controls the temperature of the low temperature module and the high temperature module and monitors the pressure of the pressure sensor in real time.

8. The apparatus for testing boiling point of viscous material according to claim 1, wherein the apparatus is used in a fume hood where the air velocity is 0.5 m/s or less, and the exhaust system is adapted to absorb toxic fumes.

9. The test device for determining the boiling point of a viscous material according to claim 6, wherein the ratio of the diameter of the upper portion to the diameter of the lower portion is 1:0.3 to 0.5.

10. An apparatus for measuring the boiling point of a viscous material according to any one of claims 1 to 9, which is used in a test for measuring the boiling point of a viscous material.

Technical Field

The invention relates to a test device for measuring the boiling point of a viscous substance and application thereof.

Background

Boiling point is an important parameter for assessing the volatility of a chemical substance. The domestic and foreign determination of the boiling point of liquid substances mainly refers to GB/T616-2006 general method for determining the boiling point of chemical reagents, OECD chemical test criterion 103 boiling point, EC440-2008A.2 boiling point and other test standards, the corresponding test devices mainly comprise a distillation device, a photoelectric tube detection test device and the like, and are mainly applied to easily flowing and low-boiling-point substances, however, for the measurement of the boiling point of viscous substances, the existing test device has certain defects, the distillation device generally adopts an alcohol lamp for heating or electric heating, the heating rate is not easy to control, the heating is not uniform, meanwhile, the photoelectric tube detection test device is not easy to observe, so that the test result is not accurate, and the aperture of the glass tube is too small, the invention relates to a test device for measuring the boiling point of a viscous substance by vacuum stability, which has the defects of difficult sample application and great defects.

The invention meets the relevant technical requirements in terms of boiling point measurement. At present, according to the conditions of literature retrieval and market investigation, no related institution designs a similar test method for the boiling point according to a vacuum stability measurement method in China, and the method has important guiding significance for measuring the boiling point of a viscous substance.

Disclosure of Invention

One of the technical problems to be solved by the invention is the problem of inaccurate test result in the prior art, and the invention provides a new test device for measuring the boiling point of the viscous substance, which has the advantage of accurate test result. The second technical problem to be solved by the present invention is to provide an application of the testing device for measuring the boiling point of the viscous material corresponding to the first technical problem.

In order to solve one of the problems, the technical scheme adopted by the invention is as follows: a test device for measuring the boiling point of viscous materials comprises a low-temperature module, a high-temperature module, a test tube and a pressure sensor, wherein a refrigerator is arranged in the middle of the low-temperature module, test tube seat holes are formed in two sides of the refrigerator, a liquid storage tank is arranged above the refrigerator, and the liquid storage tank is communicated with the upper part of the test tube seat holes; the high-temperature module is a boiling point test module, the middle part of the high-temperature module is a heater, the interior of the heater is divided into two parts, two different temperatures can be respectively controlled, and the temperature stability of the two parts can be ensured; the test tube seat hole is arranged on the refrigerator and the high-temperature module, and silicone oil needs to be added into the test tube seat hole during testing; the upper portion of the test tube is provided with a vacuumizing part, the vacuumizing part is provided with a vacuum pump tube access hole, the vacuum pump tube access hole is communicated with the inside of the test tube, the pressure sensor is in a cone shape, the diameter of the upper portion of the vacuum pump tube access hole is larger than that of the lower portion of the vacuum pump tube access hole, the upper portion of the vacuum pump tube access hole is inserted above the test tube, the inside of the pressure sensor is hollow, the side portion of the lower portion of the vacuum pump tube access hole is provided.

In the above technical solution, preferably, in the test for measuring the boiling point of the viscous substance, the characteristic that the saturated vapor pressure of the viscous substance is small under a low temperature condition is utilized to perform air tightness detection on the test system under the low temperature condition, then the test system is placed at a constant temperature under the test temperature, the saturated vapor pressure of the sample at the boiling temperature is detected by performing vacuum pumping and data processing on the system, a constant A, B is obtained by two sets of temperature and pressure at the boiling time and the relationship lgP between the boiling point T and the pressure P being a + a/T, and finally the boiling point of the sample under the atmospheric pressure of the test environment is reversely deduced according to the atmospheric pressure of the test environment.

In the above technical scheme, preferably, the temperature control range of the low-temperature module is-20 ℃ to 0 ℃, and the temperature precision is as follows: plus or minus 0.1 ℃; the temperature control range of the high-temperature module is 30-150 ℃.

In the above technical scheme, preferably, the test tube seat holes are arranged on the refrigerator and the high temperature module, and each test tube seat hole is two.

In the above technical scheme, preferably, the test tubes are made of glass, the two test tubes are in total, the shapes of the test tubes are consistent with those of common test tubes, the ratio of the length of the part below the vacuumizing part to the total length is 1:1-1.4, the internal volumes of the two test tubes are consistent, and the two test tubes need to be calibrated.

In the above technical solution, preferably, the pressure sensors are made of stainless steel, and have a conical shape, a pressure test range is 0 to 100kPa, an accuracy is ± 1pa, and a ratio of an upper diameter to a lower diameter is 1:0.2 to 0.6, more preferably 1:0.3 to 0.5.

In the above technical scheme, preferably, during testing, the pressure sensor is inserted on the test tube, then the test tube is communicated with the pressure sensor and is inserted in the hole of the test tube seat, the low-temperature module, the high-temperature module and the pressure sensor are all connected with test software, the software controls the temperature of the low-temperature module and the temperature of the high-temperature module, and meanwhile, the pressure of the pressure sensor is monitored in real time.

In the above solution, preferably, the device is used in a fume hood where the air flow rate is 0.5 m/s or less, and the exhaust system is adapted to absorb toxic fumes.

In order to solve the second problem, the invention adopts the following technical scheme: the application of the test device for measuring the boiling point of the viscous substance is used in the test for measuring the boiling point of the viscous substance.

The boiling point testing device basically stays in the distillation device and the photoelectric tube testing device, but the two devices have certain defects for testing the viscous substance, and the flash point testing of the viscous substance is often involved in daily production, detection and scientific research. The invention relates to a test method for measuring and evaluating the boiling point of a chemical substance through vacuum stability, which is very novel in test principle. Compared with the traditional distillation device, the invention solves the problems that the heating rate can not be controlled, the sample is not heated uniformly, the reading of the glass thermometer is not easy to observe, and the like. Compared with the traditional photoelectric tube detection device, the invention solves the problems of difficult sample addition, easy bubble generation, easy bumping and the like. The data of the invention is recorded by software, calculated by software and calculated accurately, thereby avoiding the error introduced by artificial reading and obtaining better technical effect.

Drawings

FIG. 1 is a schematic flow diagram of the apparatus of the present invention.

In fig. 1, 1 refrigerator 2 test tube socket hole, 3 test tube, 4 reservoir, 5 pressure sensor, 6 data line, 7 heater.

The present invention will be further illustrated by the following examples, but is not limited to these examples.

Detailed Description

[ example 1 ]

The invention is realized by the following technical scheme: and (3) performing air tightness detection on the test system under the low-temperature condition by utilizing the characteristic that the saturated vapor pressure of the viscous substance is small under the low-temperature condition. And then placing the test system at a constant temperature, vacuumizing the system and processing data to detect the saturated vapor pressure of the sample at the temperature when the sample is boiled, and obtaining constants A and B by two groups of temperature and pressure when the sample is boiled and the relation lgP between the boiling point and the pressure, namely A + B/T. And finally, reversely deducing the boiling point of the sample under the atmospheric pressure of the test environment according to the atmospheric pressure of the test environment.

The device of the invention consists of a low-temperature module, a high-temperature module, a test tube and a pressure sensor, as shown in figure 1, the functions and the connections of the specific components are as follows:

1. a low-temperature module: the temperature control range is-20 ℃ to 0 ℃, and the temperature precision is as follows: the positive middle part of the refrigerator is a refrigerator, the module is refrigerated, when the air tightness is detected, the test tube is maintained at the target temperature, two test tube seat holes are arranged at the two sides of the refrigerator, a liquid storage tank is arranged above the refrigerator, and the liquid storage tank is communicated with the upper part of the test tube seat hole; the low-temperature module has the main functions of vacuumizing the test system under the low-temperature condition by utilizing the characteristic that the saturated vapor pressure of a viscous substance is small under the low-temperature condition and detecting the air tightness of the device.

2. A high-temperature module: the high-temperature module is a boiling point test module, the temperature control range is 30-150 ℃, the heater is arranged in the middle, the interior of the high-temperature module is divided into two parts, two different temperatures can be controlled respectively, and the temperature stability of the two parts can be ensured.

3. Testing the tube seat hole: the test tube seat holes are arranged on the low-temperature module and the high-temperature module, the number of the test tube seat holes is two, the aperture is 20mm, the depth is 150mm, and during testing, a proper amount of silicon oil needs to be added into the test tube seat holes to enable the test tubes to be heated uniformly.

4. Testing tubes: the test tubes are made of glass and are respectively numbered 1 and 2, the appearance of the test tube is basically consistent with that of a common test tube, the outer diameter is 18mm, the wall thickness is 2mm, the total length is 160mm, the inner volume of the two test tubes is consistent with that of a vacuum part, and the test tubes need to be calibrated. The upper part of the test tube is provided with a vacuumizing part, the vacuumizing part is provided with a vacuum pump tube connection hole, and the vacuum pump tube connection hole is communicated with the inside of the test tube.

5. A pressure sensor: the pressure sensors are made of stainless steel, are respectively numbered A and B, are conical, have a pressure testing range of 0-100 kPa, have the precision of +/-1 pa, have the diameter of 20mm at the upper part and the diameter of 15mm at the lower part, are inserted above the testing tube, are hollow inside, have a suction hole with the diameter of 2mm at the lower side part, and can align to a vacuum pump pipe connection hole of a vacuumizing part on the testing tube when being inserted on the testing tube;

the invention needs to design a set of corresponding test software which has the functions required by the test software, and 1) the temperature of the low-temperature module and the high-temperature module can be accurately controlled; 2) the air tightness of the test system can be effectively detected; 3) the numerical value of the pressure in the test tube can be recorded in real time; 4) the measured data can be simply processed.

[ example 2 ]

A test device for determining the boiling point of viscous materials, as shown in FIG. 1, is used in a fume hood having an air flow rate of 0.5 m/s or less, and the exhaust system is adapted to absorb toxic fumes, and then the test is performed according to the following steps:

(1) preparation before experiment

Preparing a test sample, placing the sample at a designated place, starting a test instrument, a computer and test software, adding a proper amount of liquid silicone oil into the test tube seat holes of the low-temperature module and the high-temperature module, setting the temperature of the low-temperature module to-10 ℃ or lower, and respectively setting two target measurement temperatures (T) of the high-temperature module₁，T₂) And keeping the temperature constant for at least 10 minutes after the temperature reaches the set temperature. A little zeolite was added to test tubes 1 and 2.

(2) And (3) air tightness detection:

adding 4.0mL of sample into the test tubes 1 and 2 respectively by using an injector, coating a thin layer of solid silicone grease on the inner part of the test tube opening and the outer part of the lower end of the pressure sensor, wherein the silicone oil can not block the suction hole on the pressure sensor, inserting the pressure sensor A into the test tube 1, aligning the suction hole of the pressure sensor with the suction hole of the vacuum pump tube of the vacuum pumping part of the test tube, discharging the test tube and the pressure sensor together into the hole of the test tube seat, and simultaneously carrying out the same treatment on the test tube 2. The temperature is kept constant for 30 minutes. And connecting a vacuum pump, respectively vacuumizing the test tubes 1 and 2 until the minimum value is pumped, wherein the pressure is not reduced any more, rotating the pressure sensor by 90 degrees at the moment, connecting and disconnecting the suction inlet of the pressure sensor and the vacuum tube connection hole of the vacuum pumping part of the test tube, and closing the vacuum pump. And opening the air tightness detection on software, detecting the change of the internal pressure of the two test tubes within 1 minute, wherein the pressure increase rate is less than 0.02kPa/min to indicate that the air tightness is good, and meeting the requirement, if the pressure increase rate is more than 0.02kPa/min, indicating that the air tightness is not good, coating silicon oil again, and vacuumizing again until the pressure increase rate is less than 0.02 kPa/min.

(3) Testing

The method comprises the steps of taking out a pressure sensor communicated with a test tube 1 and a test tube 2 from a low-temperature module, inserting the test tube 1 and the test tube 2 into a high-temperature module after the temperature reaches the room temperature, ensuring good air tightness of the test tube in the conversion process, keeping the temperature for at least 30 minutes, starting a test program of test software to vacuumize the test tube 1 and the test tube 2, setting the vacuumizing rate (kPa/s), vacuumizing while recording the change of the internal pressure of the test tube, calculating the change rate of the internal pressure of the test tube through software, and recording the pressure P1 and P2 of the pressure sensor at the moment when the change rate of the internal pressure of the test tube does not change any more (at the moment, the pressure in the tube is the saturated vapor pressure of. Two sets of temperature and pressure data (T) were obtained₁，P₁)，(T₂，P₂)。

(4) Calculation of results

Boiling point versus pressure relationship: lgP ═ a + B/T, where P is the vapor pressure at the surface of the liquid, in kPa; t-thermodynamic temperature at which the solution boils, K; a, B-constant.

By (T)₁，P₁)，(T₂，P₂) Calculating the values of constants A and B in lgP + A/T, and then calculating the values of constants A and B according to the atmospheric pressure P under the environmental conditions₀(manual input system) the boiling point of the sample at ambient conditions was calculated.

(5) Examples of the invention

Taking glycerol as an example, the airtightness detection temperature is set to be-10 ℃, the test temperatures are respectively set to be 100 ℃ (373.15K) and 140 ℃ (413.15K), two groups of temperature and pressure data (373.15K, 4.81kPa) are obtained, 413.15K, 11.75kPa) are introduced into the formula lgP ═ a + B/T to obtain a, B is respectively a ═ 7.68 and B ═ 1492.3, the boiling point of glycerol under the condition of 101.3kPa is obtained by adopting the ambient atmospheric pressure of 101.3kPa to be 284.8 ℃ (557.95K), which is very close to the boiling point of glycerol in the reference document of 290 ℃ (101.3kPa), and the accuracy of the invention is verified.

[ example 3 ]

Using the conditions and procedures described in example 2, taking acetophenone as an example, the airtightness detection temperature was set at-10 ℃, the test temperatures were set at 80 ℃ (353.15K), and 120 ℃ (393.15K), to obtain two sets of temperature and pressure data (353.15K, 3.26kPa), (393.15K, 12.91kPa), and the data were introduced into the formula lgP + a/T to obtain a, B is a 9.46, and B is-2102.2, using the ambient atmospheric pressure of 101.3kPa, to obtain the boiling point of acetophenone under 101.3kPa at 198.2 ℃, which is very close to the boiling point of glycerol 202 ℃ (101.3kPa) in the reference, and the accuracy of the present invention was confirmed.