CN113740376B - Quantitative sample injection device and method for converting normal-temperature gaseous substances into low-temperature liquid - Google Patents
Quantitative sample injection device and method for converting normal-temperature gaseous substances into low-temperature liquid Download PDFInfo
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- CN113740376B CN113740376B CN202010466247.8A CN202010466247A CN113740376B CN 113740376 B CN113740376 B CN 113740376B CN 202010466247 A CN202010466247 A CN 202010466247A CN 113740376 B CN113740376 B CN 113740376B
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- 239000007788 liquid Substances 0.000 title claims abstract description 57
- 238000002347 injection Methods 0.000 title claims abstract description 32
- 239000007924 injection Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000000126 substance Substances 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 138
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000012360 testing method Methods 0.000 claims abstract description 51
- 238000001816 cooling Methods 0.000 claims abstract description 47
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 35
- 239000010959 steel Substances 0.000 claims abstract description 35
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 27
- 238000009835 boiling Methods 0.000 claims abstract description 13
- 238000005259 measurement Methods 0.000 claims abstract description 9
- 239000012071 phase Substances 0.000 claims description 71
- 238000009413 insulation Methods 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 9
- 239000012774 insulation material Substances 0.000 claims description 7
- 230000008859 change Effects 0.000 claims description 6
- 239000011344 liquid material Substances 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 239000007792 gaseous phase Substances 0.000 claims 1
- 239000007789 gas Substances 0.000 abstract description 27
- 238000006243 chemical reaction Methods 0.000 abstract description 15
- 230000008569 process Effects 0.000 abstract description 15
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000004880 explosion Methods 0.000 abstract description 3
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 238000001311 chemical methods and process Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 2
- -1 methylene ester Chemical class 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000012994 industrial processing Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- BLLFVUPNHCTMSV-UHFFFAOYSA-N methyl nitrite Chemical compound CON=O BLLFVUPNHCTMSV-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005502 peroxidation Methods 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
Classifications
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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
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C5/00—Methods or apparatus for filling containers with liquefied, solidified, or compressed gases under pressures
- F17C5/02—Methods or apparatus for filling containers with liquefied, solidified, or compressed gases under pressures for filling with liquefied gases
- F17C5/04—Methods or apparatus for filling containers with liquefied, solidified, or compressed gases under pressures for filling with liquefied gases requiring the use of refrigeration, e.g. filling with helium or hydrogen
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01G—WEIGHING
- G01G13/00—Weighing apparatus with automatic feed or discharge for weighing-out batches of material
- G01G13/16—Means for automatically discharging weigh receptacles under control of the weighing mechanism
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention discloses a quantitative sample injection device and a sample injection method for converting normal-temperature gaseous substances into low-temperature liquid, and relates to the technical field of petrochemical engineering safety production. The problems that gas-phase materials with boiling points close to normal temperature are difficult to achieve material proportioning pressure required by chemical reaction in a sample injection process in an adiabatic calorimetric test process, cannot be uniformly mixed with other materials, and have explosion safety hazards in pressurizing feeding are solved. The sample injection device comprises a nitrogen steel cylinder, a gas phase material steel cylinder, a buffer tank, a pressure piston device, an electronic scale, a low-temperature cooling circulation device and an adiabatic calorimetric test device, wherein the gas phase material entering the buffer tank is cooled through the low-temperature cooling circulation device and is converted into a liquid state; recording the mass of the gas-phase material which enters into the pressure piston device and is converted into liquid state through an electronic scale; and the electronic scale is recorded with sufficient materials through the adiabatic quantity and heat testing device for measurement. The invention can improve the accuracy of the adiabatic calorimetric test result participated by the gas-phase material.
Description
Technical Field
The invention relates to the technical field of petrochemical engineering safety production, in particular to a quantitative sample injection device and a sample injection method for converting normal-temperature gaseous substances into low-temperature liquid.
Background
In the petrochemical industry, many chemical product production processes involve process reactions that are highly exothermic, such as decomposition, polymerization, nitration, oxidation, peroxidation, and the like. If the conditions are controlled improperly or misoperation occurs in the production process, the heat in the reactor is easy to accumulate, and the reaction is out of control. Therefore, intensive research on the thermal runaway process of exothermic reactions is required in the process design and development stages, and the thermal runaway mechanism of the exothermic reaction runaway process is studied, so that the most effective safety control measures are proposed to ensure the safety of the production process.
At present, aiming at the thermal safety research of the chemical reaction process, the thermal runaway process of the chemical reaction can be monitored in the whole process, and the testing method of the thermal runaway parameters under the extreme conditions in the thermal runaway process can be obtained, and the thermal insulation thermal testing method is generally adopted by students at home and abroad. The testing method can test the thermal runaway process of single-phase, two-phase and even three-phase chemical reactions to obtain relevant thermal runaway parameters, and is a testing method which is comprehensive and has the testing result closest to the actual working condition. But the quantitative sample injection problem of gas phase materials with boiling points close to normal temperature in the two-phase and three-phase reaction process is always a difficult problem which bothers students at home and abroad, such as 1-butene, methylene ester, liquid ammonia and the like. Because the boiling point is close to normal temperature, the outlet pressure of the pressure-resistant steel cylinder for storing the materials is generally the saturated vapor pressure of the materials under the normal temperature condition, and in the adiabatic test sample injection process, the pressure-resistant steel cylinder is directly used for sample injection, and the pressure which can only be added to the saturated vapor pressure of the materials under the normal temperature condition at most is generally difficult to reach the pressure of the material proportion required in the chemical reaction process. Meanwhile, materials are converted into gas state in the process of entering the heat insulation test system from the liquid state in the pressure-resistant steel cylinder to the outlet, quantitative material entering the heat insulation test system and uniform mixing with other materials can be influenced, deviation of material proportion is caused, and the heat insulation heat test result is inconsistent with the actual working condition. In addition, in industrial production and pilot scale process, accessible industrial processing device such as pressure boost or cooling carries out continuous feeding after the pretreatment to the material, and laboratory level's adiabatic heat test process is intermittent type reaction process, can only once only with the material start reaction after all adding, can not carry out the reaction through continuous feeding's mode, greatly increased quantitative sampling's degree of difficulty. Particularly, the materials which are inflammable and explosive under normal temperature conditions, such as 1-butene, methylene ester and the like, can bring potential safety hazards of explosion when being fed in a pressurizing mode. Therefore, it is very necessary to design an adiabatic calorimetric quantitative sample injection method for converting a material having a boiling point close to normal temperature and being in a gas phase at normal temperature into a low-temperature liquid.
Disclosure of Invention
The invention aims to provide a quantitative sample injection device for converting normal-temperature gaseous substances into low-temperature liquid, which can solve the problems that the gas-phase materials with the boiling point close to normal temperature are difficult to achieve the material proportioning pressure required by chemical reaction in the adiabatic calorimetric test process, cannot be uniformly mixed with other materials, and have explosion safety hazards in pressurizing feeding.
The technical problems to be overcome by the invention are mainly as follows:
1) How to build a device for converting the liquid low-temperature gas phase material in the pressure-resistant steel cylinder into a gas state through a pressure reducing valve, then collecting again, performing low-temperature treatment, and then converting the gas phase material into a liquid state again;
2) How to build a device for quantitatively weighing the liquid gas phase material after low-temperature treatment so as to ensure the accuracy of quantitative sample injection;
3) And a device for safely and effectively adding the liquid gas phase material subjected to low-temperature treatment into an adiabatic calorimetric test system.
In order to overcome the technical problems, the invention adopts the following technical scheme:
The quantitative sample injection device comprises a nitrogen steel cylinder, a gas phase material steel cylinder, a buffer tank, a pressure piston device, an electronic scale, a low-temperature cooling circulation device, an adiabatic calorimetric test device, related pipelines and valves, wherein the gas phase material entering the buffer tank is cooled by the low-temperature cooling circulation device and is converted into a liquid state; the mass of the gas phase material which enters and is converted into liquid state and enters the pressure piston device is recorded through the electronic scale.
Further, the heat insulation calorimetric test device is used for measuring the materials which are sufficient to record by the electronic scale.
Further preferably, the buffer tank comprises a tank wall and a tank body, wherein a cooling coil and a heat insulation material are arranged in the tank wall, and the cooling coil is communicated with the low-temperature cooling circulation device so as to form a cooling circulation for the tank body.
Preferably, the tank body is connected with a first pipeline, a second pipeline and a third pipeline, wherein the first pipeline is connected with the gas-phase material steel cylinder, gas-phase materials are conveyed into the tank body through the first pipeline, the second pipeline is connected with a vacuum pump, a vacuum-pumping pipeline valve is connected to the second pipeline, and the tank body is vacuumized through the vacuum pump; the third pipeline is connected with the pressure piston device and is used for conveying liquid materials formed after being cooled by the low-temperature cooling circulation device to the pressure piston device.
Preferably, the electronic scale is located below the pressure piston device, the pressure piston device comprises a piston chamber and a piston pull rod, the piston pull rod horizontally reciprocates in the piston chamber, a handle is arranged at the end part of the piston pull rod far away from the piston chamber, and the handle is pulled to draw the material which is converted into a liquid state in the buffer tank into the pressure piston device.
Preferably, the piston chamber is connected to the nitrogen steel cylinder through a fourth pipeline connected with the piston chamber, a fifth pipeline is connected between the piston chamber and the adiabatic calorimetric test device, and the electronic scale records sufficient materials and is sent to the adiabatic calorimetric test device for measurement through the fifth pipeline.
Preferably, the insulation amount measuring device includes a calorimeter tank provided with a calorimeter tank temperature sensor and a calorimeter tank pressure sensor.
Preferably, the buffer tank is provided with a material pressure sensor, a tank wall temperature sensor and a material temperature sensor.
Preferably, the periphery of the piston chamber is covered by the heat insulation material.
Preferably, valves are arranged on the first pipeline, the second pipeline, the third pipeline, the fourth pipeline and the fifth pipeline.
Preferably, a coil pipe for cooling and lowering the temperature of the material is also arranged on the outer wall of the piston chamber, and the coil pipe is connected with the low-temperature cooling circulation device to form a cooling circulation.
The second object of the invention is to provide a quantitative sample injection method for converting normal temperature gaseous substances into low temperature liquid, which comprises the steps of firstly performing low temperature cooling treatment on the gaseous substances with boiling point close to normal temperature provided by a pressure-resistant steel cylinder, adding the gaseous substances into a pressure piston device which is subjected to low temperature cooling treatment and pressure resistance and can weigh mass through a pipeline provided with a heat preservation layer after the gaseous substances are completely converted into liquid, and quantitatively, accurately and safely adding the liquid substances into an adiabatic calorimetric test system by means of the pressure piston device.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
The quantitative sample injection method for converting normal temperature gaseous matter into low temperature liquid includes the steps of:
S1, firstly detecting the air tightness of the device, and after the air tightness is detected to be qualified, feeding gas-phase materials into a buffer tank;
s2, starting a low-temperature cooling circulation device, and cooling the buffer tank until the temperature in the buffer tank is lower than the boiling point temperature of the gas-phase material by at least 10 ℃, wherein the gas-phase material in the buffer tank is completely converted into a liquid state;
S3, starting the electronic scale and the pressure piston device, pumping all the gas-phase materials which are converted into liquid in the buffer tank into the pressure piston device by controlling a piston pull rod and a handle of the pressure piston device, and recording the mass change of the electronic scale;
and S4, stopping material entering when the record of the electronic scale reaches a certain quality, inputting nitrogen into the pressure piston device, recording through the electronic scale, and sending the material therein into the adiabatic heat testing device for measurement by controlling the nitrogen pressure in the pressure piston device.
Further preferably, in step S4, after the materials in the pressure piston device are all sent to the adiabatic heat testing device, the nitrogen pressure in the pressure piston device is released to normal pressure.
Compared with the prior art, the invention has the following beneficial technical effects:
(1) The quantitative sample injection device for the adiabatic calorimetric test for converting the gas-phase material into the low-temperature liquid can convert the liquid low-temperature gas-phase material in the pressure-resistant steel cylinder into the gas state through the pressure reducing valve, then collect the gas state again and perform low-temperature treatment, quantitatively weigh the liquid gas-phase material subjected to the low-temperature treatment, safely and effectively add the liquid gas-phase material into the adiabatic calorimetric test system, and improve the accuracy of the adiabatic calorimetric test result participated in by the gas-phase material.
(2) According to the adiabatic calorimetric test quantitative sample injection method for converting gas-phase materials into low-temperature liquid, the gas-phase materials with boiling points close to normal temperature provided by the pressure-resistant steel cylinders are subjected to low-temperature cooling treatment firstly, after the materials are completely converted into liquid states, the liquid-phase materials are added into a pressure piston device which is subjected to low-temperature cooling treatment and pressure resistance and can weigh the mass through a pipeline provided with a heat preservation layer, and the liquid-phase materials are quantitatively, accurately and safely added into an adiabatic calorimetric test system by means of the pressure piston device.
(3) According to the invention, the thermal runaway adiabatic heat test of methyl nitrite decomposition and butene-1 polymerization reaction is carried out successively, and the materials can be effectively and accurately quantitatively added into the adiabatic heat test device after being cooled.
(4) The device and the method are particularly suitable for scientific research institutions, universities, enterprises and design units engaged in the safety of chemical processes and the safety of chemical processes, especially the safety study of chemical reaction thermal runaway, and have considerable application and popularization values in the scientific research institutions, universities, enterprises and design units engaged in the safety of the chemical processes and the safety of the chemical processes along with the gradual perfection of the process safety control technology of petrochemical production enterprises in China.
Drawings
The invention is described in detail below with reference to the attached drawing figures:
FIG. 1 is a schematic structural diagram of a quantitative sample injection device for converting normal-temperature gaseous substances into low-temperature liquid;
FIG. 2 is a schematic structural view of a surge tank;
FIG. 3 is a schematic view of a pressure piston apparatus;
In the figure: 1-nitrogen steel cylinder, 2-gas phase material steel cylinder, 3-nitrogen steel cylinder pressure reducing valve, 4-gas phase material steel cylinder pressure reducing valve, 5-pressure sensor, 6-vacuumizing pipeline valve, 7-vacuum pump, 8-buffer tank, 9-low temperature cooling circulation device, 10-pressure piston device nitrogen feeding pipeline valve, 11-electronic scale, 12-pressure piston device, 13-pressure piston device gas phase material feeding pipeline valve, 14-adiabatic calorimeter system feeding pipeline valve, 15-adiabatic calorimeter, 16-calorimeter tank temperature sensor, 17-calorimeter tank pressure sensor, 18-material temperature sensor, 19-heat insulation material, 20-cooling coil pipe, 21-material pressure sensor, 22-tank wall temperature sensor, 23-handle, 24-piston pull rod, 25-internal heat insulation material and 26-internal cooling coil pipe.
Detailed Description
The invention provides a quantitative sample injection device and a sample injection method for converting normal-temperature gaseous substances into low-temperature liquid, and in order to make the advantages and the technical scheme of the invention clearer and more definite, the invention is described in detail below with reference to specific embodiments.
As shown in fig. 1, the quantitative sample injection device for converting normal-temperature gaseous substances into low-temperature liquid comprises a nitrogen steel cylinder 1, a gas-phase material steel cylinder 2, a vacuum pump 7, a buffer tank 8, a low-temperature cooling circulation device 9, an electronic scale 11, a pressure piston device 12, an adiabatic calorimetric test device 15 and related valves, wherein the related valves comprise a nitrogen steel cylinder pressure reducing valve 3, a gas-phase material steel cylinder pressure reducing valve 4, a vacuumizing pipeline valve 6, a pressure piston device nitrogen feed pipeline valve 10, a pressure piston device gas-phase material feed pipeline valve 13 and an adiabatic calorimetric test system feed pipeline valve 14.
As shown in fig. 2, the specific structure of the buffer tank 8 comprises a tank wall and a tank body, a cooling coil 20 and a heat insulation material 19 are arranged in the tank wall, the cooling coil 20 is communicated with a low-temperature cooling circulation device, so as to form a cold circulation to the tank body, the tank body is connected with a material temperature sensor 18 and a material pressure sensor 21 for respectively monitoring the temperature and the pressure of the material in the tank body, and a tank wall temperature sensor 22 is arranged on the tank wall and used for monitoring the temperature of the tank wall. The tank wall of the buffer tank is cooled by the low-temperature cooling circulation device, so that the gas phase in the buffer tank is converted into the liquid phase.
Further, a first pipeline, a second pipeline and a third pipeline are connected to the tank body, wherein the first pipeline is connected with a gas-phase material steel bottle, gas-phase materials are conveyed into the tank body through the first pipeline, a pressure sensor 5 is arranged on the first pipeline, the second pipeline is connected with a vacuum pump, a vacuumizing pipeline valve 6 is connected to the second pipeline, and the tank body is vacuumized through the vacuum pump; the third pipeline is connected with the pressure piston device and is used for conveying the liquid material formed after being cooled by the low-temperature cooling circulation device to the pressure piston device. Corresponding valves are arranged on the corresponding pipelines to control the device, such as a gas-phase material steel cylinder pressure reducing valve 4 is arranged on a first pipeline, and a pressure piston device gas-phase material feeding pipeline valve 13 is arranged on a third pipeline.
As shown in fig. 3, the electronic scale is located below the pressure piston device, the pressure piston device comprises a piston chamber and a piston pull rod 24, the piston pull rod 24 horizontally reciprocates in the piston chamber, a handle 23 is arranged at the end of the piston pull rod far away from the piston chamber, and the handle is pulled to control the material which is converted into liquid in the buffer tank to be pumped into the pressure piston device.
For controlling the temperature of the material in the pressure piston device, an inner insulation 25 is preferably wrapped around the piston chamber, and an inner cooling coil 26 is provided between the piston chamber and the inner insulation.
The piston chamber is connected to the nitrogen steel cylinder through a fourth pipeline connected with the piston chamber, a fifth pipeline is connected between the piston chamber and the adiabatic calorimetric test device, and the electronic scale records sufficient materials and sends the materials into the adiabatic test device for measurement through the fifth pipeline.
The insulation amount measuring device includes a calorimeter tank, a calorimeter tank temperature sensor 16, and a calorimeter tank pressure sensor 17.
The surge tank of the present invention is preferably made of a pressure-resistant metal material.
The quantitative sample injection method for converting normal-temperature gaseous substances into low-temperature liquid is described in detail below, and the quantitative sample injection device is adopted, and comprises the following steps:
Firstly, detecting the air tightness of the device, and after the air tightness is detected to be qualified, feeding gas-phase materials into a buffer tank;
Secondly, starting a low-temperature cooling circulation device to cool the buffer tank until the temperature in the buffer tank is lower than the boiling point temperature of the gas-phase material by at least 10 ℃, and completely converting the gas-phase material in the buffer tank into a liquid state;
Thirdly, starting the electronic scale and the pressure piston device, pumping all the gas-phase materials which are converted into liquid state in the buffer tank into the pressure piston device by controlling a piston pull rod and a handle of the pressure piston device, and recording the mass change of the electronic scale;
And fourthly, stopping feeding materials when the record of the electronic scale reaches a certain quality, inputting nitrogen into the pressure piston device, recording by the electronic scale, and feeding the materials into the adiabatic heat testing device for measurement by controlling the nitrogen pressure in the pressure piston device.
The sample injection method of the device of the invention is further described below with reference to specific examples.
Example 1:
firstly, vacuumizing a buffer tank until the reading of a pressure sensor is unchanged, closing a valve of a vacuum pump pipeline, performing air tightness detection, opening a pressure-resistant valve switch of a gas-phase material pressure-resistant steel cylinder after the detection is qualified, pumping low-temperature liquid gas-phase material in the pressure-resistant steel cylinder into the buffer tank by means of negative pressure in a buffer until the reading of the pressure sensor of the buffer tank is unchanged, and closing the pressure-resistant valve switch;
Starting a low-temperature cooling circulation device to cool the buffer tank until the temperature of a temperature sensor in the buffer tank is at least 10 ℃ below the boiling point temperature of the gas-phase material, so as to ensure that the gas-phase material in the buffer tank is completely converted into a liquid state;
Starting the electronic scale and the pressure piston device, pumping all the gas phase materials which are converted into liquid state in the buffer tank into the pressure piston device by controlling a piston pull rod and a handle of the pressure piston device, and recording the mass change of the electronic scale;
When the electronic scale records that certain quality is achieved, stopping material entering, then inputting nitrogen into the pressure piston device, recording through the electronic scale, and sending the material therein into the adiabatic heat testing device for measurement by controlling the nitrogen pressure in the pressure piston device.
Example 2:
firstly, vacuumizing a buffer tank until the reading of a pressure sensor is unchanged, closing a valve of a vacuum pump pipeline, performing air tightness detection, opening a pressure-resistant valve switch of a gas-phase material pressure-resistant steel cylinder after the detection is qualified, pumping low-temperature liquid gas-phase material in the pressure-resistant steel cylinder into the buffer tank by means of negative pressure in a buffer until the reading of the pressure sensor of the buffer tank is unchanged, and closing the pressure-resistant valve switch;
Starting a low-temperature cooling circulation device to cool the buffer tank until the temperature of a temperature sensor in the buffer tank is at least 10 ℃ below the boiling point temperature of the gas-phase material, so as to ensure that the gas-phase material in the buffer tank is completely converted into a liquid state;
after all the gas phase materials in the buffer tank are converted into liquid, the valve switches of the feed pipeline of the electronic balance and the pressure piston device are opened, a piston pull rod handle of the pressure piston device which is made of pressure-resistant metal materials, sealed and provided with a cooling coil pipe and a heat-insulating filling material in the tank wall is pulled, and the handle can control the gas phase materials which are all converted into liquid in the buffer tank to be pumped into the pressure piston device, so that the mass change of the electronic balance is recorded. If the quality of the low-temperature gas phase material extracted at one time is not less than the material quantity required by the adiabatic heat test, repeating the operation for a plurality of times until the material quality meets the material quantity required by the adiabatic heat test;
When the electronic scale records that certain quality is achieved, stopping material entering, then inputting nitrogen into the pressure piston device, recording through the electronic scale, and sending the material therein into the adiabatic heat testing device for measurement by controlling the nitrogen pressure in the pressure piston device.
Example 3:
firstly, vacuumizing a buffer tank until the reading of a pressure sensor is unchanged, closing a valve of a vacuum pump pipeline, performing air tightness detection, opening a pressure-resistant valve switch of a gas-phase material pressure-resistant steel cylinder after the detection is qualified, pumping low-temperature liquid gas-phase material in the pressure-resistant steel cylinder into the buffer tank by means of negative pressure in a buffer until the reading of the pressure sensor of the buffer tank is unchanged, and closing the pressure-resistant valve switch;
Starting a low-temperature cooling circulation device to cool the buffer tank until the temperature of a temperature sensor in the buffer tank is at least 10 ℃ below the boiling point temperature of the gas-phase material, so as to ensure that the gas-phase material in the buffer tank is completely converted into a liquid state;
after all the gas phase materials in the buffer tank are converted into liquid, the valve switches of the feed pipeline of the electronic balance and the pressure piston device are opened, a piston pull rod handle of the pressure piston device which is made of pressure-resistant metal materials, sealed and provided with a cooling coil pipe and a heat-insulating filling material in the tank wall is pulled, and the handle can control the gas phase materials which are all converted into liquid in the buffer tank to be pumped into the pressure piston device, so that the mass change of the electronic balance is recorded. If the quality of the low-temperature gas phase material extracted at one time is not less than the material quantity required by the adiabatic heat test, repeating the operation for a plurality of times until the material quality meets the material quantity required by the adiabatic heat test;
After the material quality meets the material quantity required by the adiabatic heat test, closing a valve switch of a feeding pipeline of the pressure piston device, starting an electronic balance for weighing the weight of the pressure piston device, pulling a piston pull rod of the pressure piston device, and opening a pressure reducing valve of a nitrogen steel cylinder and a valve switch of a nitrogen feeding pipeline of the pressure piston device. The valve is a three-way valve, and when feeding materials, the pressure of nitrogen is controlled and controlled, and the low-temperature liquid gas phase materials in the pressure piston device are driven into a calorimeter tank in a adiabatic heat test system. After the material feeding is finished, the pressure of the nitrogen added into the pressure piston device can be controlled to be released to normal pressure.
The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited thereto.
The invention can be realized by referring to the prior art in the parts not described.
It should be noted that: any equivalent or obvious modifications made by those skilled in the art under the teachings of this specification shall fall within the scope of this invention.
Claims (4)
1. The utility model provides a normal atmospheric temperature gaseous state material converts into quantitative sampling device of low temperature liquid, its includes nitrogen gas steel bottle, gaseous phase material steel bottle, buffer tank, pressure piston device, electronic scale, cryogenic cooling circulating device, adiabatic calorimetric test device, relevant pipeline and valve, its characterized in that: the gas-phase materials entering the buffer tank are cooled by the low-temperature cooling circulation device and are converted into liquid; recording the mass of the gas-phase material which enters into the pressure piston device and is converted into liquid state through the electronic scale;
The heat insulation calorimetric test device is used for measuring the materials which are sufficient to record by the electronic scale;
The buffer tank comprises a tank wall and a tank body, wherein a cooling coil pipe and a heat insulation material are arranged in the tank wall, and the cooling coil pipe is communicated with the low-temperature cooling circulation device so as to form a cooling circulation for the tank body;
the tank body is connected with a first pipeline, a second pipeline and a third pipeline, wherein the first pipeline is connected with the gas-phase material steel cylinder, gas-phase materials are conveyed into the tank body through the first pipeline, the second pipeline is connected with a vacuum pump, a vacuum-pumping pipeline valve is connected to the second pipeline, and the tank body is vacuumized through the vacuum pump; the third pipeline is connected with the pressure piston device and is used for conveying liquid materials formed after being cooled by the low-temperature cooling circulation device to the pressure piston device;
The electronic scale is positioned below the pressure piston device, the pressure piston device comprises a piston chamber and a piston pull rod, the piston pull rod horizontally reciprocates in the piston chamber, a handle is arranged at the end part of the piston pull rod far away from the piston chamber, and the handle is pulled to draw the material which is converted into liquid in the buffer tank into the pressure piston device;
The piston chamber is connected to the nitrogen steel cylinder through a fourth pipeline connected with the piston chamber, a fifth pipeline is connected between the piston chamber and the adiabatic calorimetric test device, and the electronic scale records sufficient materials and sends the materials into the adiabatic calorimetric test device for measurement through the fifth pipeline;
The adiabatic heat testing device comprises a calorimetric tank, wherein the calorimetric tank is provided with a calorimetric tank temperature sensor and a calorimetric tank pressure sensor;
The buffer tank is provided with a material pressure sensor, a tank wall temperature sensor and a material temperature sensor;
Valves are arranged on the first pipeline, the second pipeline, the third pipeline, the fourth pipeline and the fifth pipeline;
the outer wall of the piston chamber is also provided with a coil pipe for cooling and lowering the temperature of materials, and the coil pipe is connected with the low-temperature cooling circulation device to form a cooling circulation.
2. The quantitative sample injection device for converting normal-temperature gaseous substances into low-temperature liquid according to claim 1, wherein the quantitative sample injection device is characterized in that: the periphery of the piston chamber is coated by the heat insulation material.
3. A quantitative sample injection method for converting normal-temperature gaseous substances into low-temperature liquid is characterized by comprising the following steps of: a quantitative sample injection device for converting a normal-temperature gaseous substance into a low-temperature liquid according to any one of claims 1-2, wherein the method comprises the following steps:
S1, firstly detecting the air tightness of the device, and after the air tightness is detected to be qualified, feeding gas-phase materials into a buffer tank;
s2, starting a low-temperature cooling circulation device, and cooling the buffer tank until the temperature in the buffer tank is lower than the boiling point temperature of the gas-phase material by at least 10 ℃, wherein the gas-phase material in the buffer tank is completely converted into a liquid state;
S3, starting the electronic scale and the pressure piston device, pumping all the gas-phase materials which are converted into liquid in the buffer tank into the pressure piston device by controlling a piston pull rod and a handle of the pressure piston device, and recording the mass change of the electronic scale;
and S4, stopping material entering when the record of the electronic scale reaches a certain quality, inputting nitrogen into the pressure piston device, recording through the electronic scale, and sending the material therein into the adiabatic heat testing device for measurement by controlling the nitrogen pressure in the pressure piston device.
4. The quantitative sample injection method for converting normal-temperature gaseous substances into low-temperature liquid according to claim 3, wherein the quantitative sample injection method is characterized by comprising the following steps of: in step S4, after materials in the pressure piston device are all sent into the adiabatic heat testing device, the nitrogen pressure in the pressure piston device is released to normal pressure.
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