Test device for determining whether oily substances belong to bulk persistent oils

文档序号:1919850 发布日期:2021-12-03 浏览:18次 中文

阅读说明:本技术 一种测定油性物质是否属于散装持久性油类的试验装置 (Test device for determining whether oily substances belong to bulk persistent oils ) 是由 吴保意 王双全 王康 张会光 于 2020-05-28 设计创作,主要内容包括:本发明提供了一种测定油性物质是否属于散装持久性油类的试验装置,包括340℃测试模块、370℃测试模块和控制系统,340℃测试模块和370℃测试模块共用一套控制系统,控制系统分别与340℃测试模块、370℃测试模块控制相连,340℃测试模块和370℃测试模块结构相同,每个模块均由温控系统、蒸馏系统、升降系统三部分组成。本发明通过温度控制程序对坩埚容器和传热介质进行加热,将传热介质加热到目标温度,通过熔盐对蒸馏烧瓶内样品进行加热,解决了目前只能搭建简易蒸馏装置测定散装持久性油类的问题,跟传统蒸馏装置相比,用熔盐作传热介质,既解决了高温蒸馏的难题,也创造了盐浴的环境,保证温度的稳定性,提高了实验的精准度。(The invention provides a test device for determining whether oily substances belong to bulk persistent oils, which comprises a 340 ℃ test module, a 370 ℃ test module and a control system, wherein the 340 ℃ test module and the 370 ℃ test module share one set of control system, the control system is respectively connected with the 340 ℃ test module and the 370 ℃ test module in a control way, the 340 ℃ test module and the 370 ℃ test module have the same structure, and each module consists of a temperature control system, a distillation system and a lifting system. According to the invention, the crucible container and the heat transfer medium are heated through the temperature control program, the heat transfer medium is heated to the target temperature, and the sample in the distillation flask is heated through the molten salt, so that the problem that only a simple distillation device can be set up to measure the bulk persistent oils at present is solved.)

1. A test device for determining whether oily substances belong to bulk persistent oils is characterized by comprising a 340 ℃ test module, a 370 ℃ test module and a control system, wherein the 340 ℃ test module and the 370 ℃ test module share one set of control system, the control system is respectively connected with the 340 ℃ test module and the 370 ℃ test module in a control mode, the 340 ℃ test module and the 370 ℃ test module have the same structure, and each module consists of a temperature control system, a distillation system and a lifting system.

2. The test device for testing whether oily substances belong to bulk permanent oils according to claim 1, wherein the temperature control system comprises an electric heater, a crucible container and a heat transfer medium, the crucible container is arranged on the electric heater, the heat transfer medium is arranged in the crucible container, the heat transfer medium in the crucible container and the crucible container is heated by the electric heater, so that the heat transfer medium is in a molten state, and the temperature of the heat transfer medium can be controlled to be stabilized at 340 +/-2 ℃ or 370 +/-2 ℃.

3. The test device for determining whether oily substances belong to bulk permanent oils according to claim 2, wherein the control system is connected with an electric heater control.

4. The test device for determining whether oily substances belong to bulk permanent oils according to claim 2, wherein the distillation system comprises a distillation flask, a condenser pipe, a collection measuring cylinder and an electronic balance, the condenser pipe is connected with an outlet of a side pipe of the distillation flask, the collection measuring cylinder is connected with an outlet of the condenser pipe, and the collection measuring cylinder is arranged on the electronic balance.

5. The test device for determining whether oily substances belong to bulk permanent oils according to claim 4, wherein the electronic balance is electrically connected with the control system.

6. The testing apparatus for testing whether oily substances belong to bulk permanent oils according to claim 4, wherein the lifting system is disposed below the temperature control system for controlling the lifting of the temperature control system so as to contact or separate the heat transfer medium in the temperature control system with or from the distillation flask.

7. The test device for determining whether oily substances belong to bulk permanent oils according to claim 6, wherein the lifting system is a lifting motor and is controlled and connected by a lifting control program in a control program.

8. The test device for determining whether oily substances belong to bulk permanent oils according to claim 4, wherein the crucible container is cylindrical and has an open top, and the open top is provided with a movable and rotatable cover which is divided into two parts and has a hole in the middle, and the diameter of the hole is slightly larger than that of the neck of the distillation flask.

9. The test device for determining whether oily substances belong to bulk permanent oils according to claim 8, wherein the crucible container has an outer diameter of 119 to 121mm, a wall thickness of 3 to 5mm and a height of 124 to 126 mm.

10. The apparatus of claim 8, wherein the crucible container is made of quartz.

11. The test device for determining whether oily substances belong to bulk permanent oils according to claim 2, wherein the heat transfer medium is potassium nitrate or sodium nitrate.

In the test, potassium nitrate or sodium nitrate is in a molten state and serves as a molten salt bath to provide a stable temperature environment atmosphere, sodium nitrate provides a 340 ℃ molten salt environment, and potassium nitrate provides a 370 ℃ molten salt environment.

12. The test device for determining whether oily substances belong to bulk permanent oils according to claim 2, wherein the temperature of the electric heater is controlled within a range from room temperature to 600 ℃ with an accuracy of ± 2 ℃.

13. The test device for determining whether oily substances belong to bulk permanent oils according to claim 4, wherein a thermometer is provided at the top of the distillation flask to measure the temperature of the distillate in the range of room temperature to 400 ℃.

14. The apparatus for testing oily substances according to claim 4, wherein said condenser is a glass condenser and is condensed with circulating water.

15. The test device for determining whether oily substances belong to bulk permanent oils according to claim 4, wherein the volume of the measuring cylinder of the collecting measuring cylinder is 100-150 mL, and the accuracy is 1 mL.

16. The test device for determining whether oily substances belong to bulk permanent oils according to claim 5, wherein the precision of the electronic balance is 0.0001g, so as to record the mass of the distillate collected by the collecting measuring cylinder and send the information to the control system.

17. The test device for determining whether oily substances belong to bulk permanent oils according to claim 4, wherein the distillation flask has the specification of 124-126 mL, the bottleneck length of 149-151 cm, the outer diameter of 20-22 mm and the inner diameter of 17-19 mm; the side pipe is located 66-68 mm above the round ball, 99-101 mm long, 6-8 mm in outer diameter and 4-6 mm in inner diameter.

Technical Field

The invention relates to the field, in particular to a test device for determining whether oily substances belong to bulk persistent oils.

Background

In order to further reduce the logistics cost, optimize the port operator environment and standardize the pollution prevention and control behaviors of ships and related operation activities thereof, the maritime office of the people's republic of China issues a notice of a name book of bulk liquid pollution hazardous goods needing to arrange oil containment fences or signing ship pollution removal protocols in 2019, 5 and 30 days, and the ships carrying bulk persistent oil cargos are required to carry out loading, unloading and refuting operations, anti-pollution measures including arranging the oil containment fences are adopted according to the forty-th regulation of the maritime ships and related operation activity pollution marine environment prevention and control management regulation of the people's republic of China and the environmental management regulation of the inland river waters of ship pollution prevention and control of the people's republic of China.

The roster lists part of a list of bulk persistent oils and a brief test method, but according to the investigation, no corresponding experimental device has been researched for the test method at home at present.

Disclosure of Invention

Based on the background, the invention provides a test device for determining whether oily substances belong to bulk permanent oils, which is used for determining whether the oily substances belong to the bulk permanent oils in the bulk transportation process, providing technical support for classification of the bulk permanent oils and providing technical guidance for anti-pollution management of the bulk permanent oils by the maritime department.

The invention adopts the following technical scheme:

a test device for determining whether oily substances belong to bulk persistent oils comprises a 340 ℃ test module, a 370 ℃ test module and a control system, wherein the 340 ℃ test module and the 370 ℃ test module share one set of control system, the control system is respectively connected with the 340 ℃ test module and the 370 ℃ test module in a control mode, the 340 ℃ test module and the 370 ℃ test module are identical in structure, and each module consists of a temperature control system, a distillation system and a lifting system.

Further, the temperature control system comprises an electric heater, a crucible container and a heat transfer medium, wherein the crucible container is arranged on the electric heater, the heat transfer medium is arranged in the crucible container, the heat transfer medium in the crucible container and the crucible container is heated by the electric heater to be in a molten state, and the temperature of the heat transfer medium can be controlled to be stabilized at 340 +/-2 ℃ or 370 +/-2 ℃.

Further, the control system is connected with the electric heater control.

Furthermore, the distillation system comprises a distillation flask, a condenser pipe, a collection measuring cylinder and an electronic balance, wherein the condenser pipe is connected with an outlet of a side pipe of the distillation flask, the collection measuring cylinder is connected with an outlet of the condenser pipe, and the collection measuring cylinder is arranged on the electronic balance.

Further, the electronic balance is electrically connected with the control system.

Furthermore, the lifting system is arranged below the temperature control system and used for controlling the lifting of the temperature control system so as to enable the heat transfer medium in the temperature control system to be in contact with or separated from the distillation flask.

Furthermore, the lifting system is a lifting motor and is controlled and connected by a lifting control program in the control program.

The lifting system is arranged below the temperature control system and used for controlling the lifting of the temperature control system, the temperature control system is lifted during a test, the distillation flask is immersed in a crucible container filled with molten salt, and a heat source is provided for the distillation flask; and after the test is finished, returning the temperature control system to the original position. The lifting system is mainly a lifting motor and is controlled by a lifting control program.

Furthermore, the crucible container is cylindrical, the upper part of the crucible container is provided with an opening, a movable and rotatable cover is arranged at the opening, the cover is divided into two parts, the middle part of the cover is provided with a hole, and the diameter of the hole is slightly larger than that of the bottle neck part of the distillation flask.

After the distillation flask is put into the crucible container, the cover is rotated from both sides to reduce the fluctuation of the internal temperature.

Furthermore, the outer diameter of the crucible container is 119-121 mm, the wall thickness is 3-5 mm, and the height is 124-126 mm.

Further, the crucible container is made of quartz.

Further, the heat transfer medium is potassium nitrate or sodium nitrate.

In the test, potassium nitrate or sodium nitrate is in a molten state and serves as a molten salt bath to provide a stable temperature environment atmosphere, sodium nitrate provides a 340 ℃ molten salt environment, and potassium nitrate provides a 370 ℃ molten salt environment.

Further, the temperature control range of the electric heater is between room temperature and 600 ℃, and the precision is +/-2 ℃.

Furthermore, a thermometer is arranged at the top end of the distillation flask, the measuring range is room temperature-400 ℃, and the thermometer is used for measuring the temperature of distillate.

Furthermore, the condenser pipe is a glass condenser pipe and is condensed by circulating water.

Furthermore, the volume of the measuring cylinder of the collecting measuring cylinder is 100-150 mL, and the precision is 1 mL.

Further, the precision of the electronic balance is 0.0001g, the mass of the distillate collected by the collecting measuring cylinder is recorded, and the information is sent to the control system.

In the technical scheme, the precision of the electronic balance is 0.0001g, the electronic balance is used for recording the mass of the slips collected by the collecting measuring cylinder and is connected with the control system, the mass change of the slips in the collecting measuring cylinder is recorded in real time, if the mass increase is less than 0.04g within 10min, no liquid drips out, and the test is automatically stopped.

Furthermore, the specification of the distillation flask is 124-126 mL, the length of a bottleneck is 149-151 cm, the outer diameter is 20-22 mm, and the inner diameter is 17-19 mm; the side pipe is located 66-68 mm above the round ball, 99-101 mm long, 6-8 mm in outer diameter and 4-6 mm in inner diameter.

When the temperature control system is used, the temperature control system is lifted, the distillation flask is immersed in the molten salt, and the sample in the distillation flask is heated through the molten salt.

The invention has the beneficial effects that:

(1) heating the crucible container and the heat transfer medium through a temperature control program, heating the heat transfer medium to a target temperature (340 ℃ or 370 ℃), and stabilizing the heat transfer medium at the target temperature +/-2 ℃ after the heat transfer medium reaches the target temperature; controlling a temperature control system to move upwards by a lifting control program when the heat transfer medium is stabilized at a target temperature, immersing the distillation flask into molten salt, heating a sample in the distillation flask by the molten salt, and controlling the temperature control system to descend to the original position after the test is stopped; in the recording control program, recording the quality of the collected fractions in real time after the test is started, and stopping the test after no fraction is evaporated;

(2) the method comprises the steps of distilling oily substances at 340 ℃ and 370 ℃, collecting distillate, comparing the collected distillate with the total volume (100mL) of the substances, and dividing into permanent oils, wherein the evaporation of the distillate is less than 50% of the total volume of hydrocarbons under the condition of 340 ℃ and less than 95% of the total volume of the hydrocarbons under the condition of 370 ℃;

(3) the invention solves the problem that only a simple distillation device can be set up to measure the bulk persistent oils at present;

(4) compared with the traditional distillation device, the invention uses the molten salt as the heat transfer medium, not only solves the problem of high-temperature distillation, but also creates the environment of the salt bath, ensures the stability of the temperature and improves the accuracy of the experiment;

(5) and a software control program is added, so that the testing process is automated, convenient and fast, and the safety factor is greatly improved.

Drawings

FIG. 1 is a schematic structural diagram of a test apparatus for determining whether an oily substance belongs to bulk permanent oils (from left to right: 340 ℃ test module, 370 ℃ test module, control system, two test modules share a set of test program);

FIG. 2 is an analytic view of a 370 ℃ test module;

FIG. 3 is a partially enlarged schematic view of a distillation system;

FIG. 4 is a schematic view of the structure of the crucible container cover.

Wherein, 1 is a lifting motor, 2 is an electric heater, 3 is a crucible container, 4 is a heat-conducting medium, 5 is a test sample, 6 is a distillation flask, 7 is a thermometer, 8 is a condenser pipe, 9 is a collection graduated flask, 10 is an electronic balance, and 11 is control equipment.

Detailed Description

The invention is described in detail below with reference to the accompanying drawings:

with reference to fig. 1 to 3, a test device for determining whether an oily substance belongs to bulk permanent oils comprises a 340 ℃ test module, a 370 ℃ test module and a control system, wherein the 340 ℃ test module and the 370 ℃ test module share one set of control system, the control system is respectively connected with the 340 ℃ test module and the 370 ℃ test module in a control manner, the 340 ℃ test module and the 370 ℃ test module have the same structure, and each module consists of a temperature control system, a distillation system and a lifting system.

As one embodiment, the temperature control system comprises an electric heater, a crucible container and a heat transfer medium, the crucible container is arranged on the electric heater, the heat transfer medium is arranged in the crucible container, the crucible container and the heat transfer medium in the crucible container are heated by the electric heater, so that the heat transfer medium is in a molten state, and the temperature of the heat transfer medium can be controlled to be stabilized at 340 +/-2 ℃ or 370 +/-2 ℃.

As one of the embodiments, further, the control system is connected with the electric heater control.

As an embodiment thereof, further, the distillation system comprises a distillation flask, a condensation pipe, a collection measuring cylinder and an electronic balance, wherein the condensation pipe is connected with an outlet of a side pipe of the distillation flask, the collection measuring cylinder is connected with an outlet of the condensation pipe, and the collection measuring cylinder is arranged on the electronic balance.

As one of the embodiments, further, the electronic balance is electrically connected to a control system.

As an embodiment, further, the lifting system is disposed below the temperature control system, and is used for controlling the lifting of the temperature control system, so that the heat transfer medium in the temperature control system is contacted with or separated from the distillation flask.

As an embodiment, further, the lifting system is a lifting motor, and is controlled and connected by a lifting control program in the control program.

The lifting system is arranged below the temperature control system and used for controlling the lifting of the temperature control system, the temperature control system is lifted during a test, the distillation flask is immersed in a crucible container filled with molten salt, and a heat source is provided for the distillation flask; and after the test is finished, returning the temperature control system to the original position. The lifting system is mainly a lifting motor and is controlled by a lifting control program.

As one embodiment, the crucible container is cylindrical, the upper part of the crucible container is open, a movable and rotatable cover is arranged at the opening, the cover is divided into two parts, the middle part of the cover is provided with a hole, and the diameter of the hole is slightly larger than that of the neck part of the distillation flask.

After the distillation flask is put into the crucible container, the cover is rotated from both sides to reduce the fluctuation of the internal temperature.

In one embodiment, the crucible container has an outer diameter of 119 to 121mm, a wall thickness of 3 to 5mm, and a height of 124 to 126 mm.

In one embodiment, the crucible container is made of quartz.

As an example thereof, further, the heat transfer medium is potassium nitrate or sodium nitrate.

In the test, potassium nitrate or sodium nitrate is in a molten state and serves as a molten salt bath to provide a stable temperature environment atmosphere, sodium nitrate provides a 340 ℃ molten salt environment, and potassium nitrate provides a 370 ℃ molten salt environment.

As an embodiment, the temperature control range of the electric heater is between room temperature and 600 ℃, and the precision is +/-2 ℃.

As an example, a thermometer is arranged at the top end of the distillation flask, the range of the thermometer is between room temperature and 400 ℃, and the thermometer is used for measuring the temperature of distillate.

As an embodiment, the condenser pipe is a glass condenser pipe, and is condensed by circulating water.

As an embodiment, the volume of the measuring cylinder of the collecting measuring cylinder is 100-150 mL, and the precision is 1 mL.

As an example, the precision of the electronic balance is 0.0001g, and the electronic balance is used for recording the mass of the distillate collected by the collecting measuring cylinder and sending the information to the control system.

The precision of the electronic balance is 0.0001g, the electronic balance is used for recording the mass of the distillate collected by the collecting measuring cylinder and is simultaneously connected with the control system, the mass change of the distillate in the collecting measuring cylinder is recorded in real time, if the mass increase is less than 0.04g within 10min, no liquid drips out, and the test is automatically stopped.

The distillation flask is 124-126 mL in specification, the bottleneck length is 149-151 cm, the outer diameter is 20-22 mm, and the inner diameter is 17-19 mm; the side pipe is located 66-68 mm above the round ball, 99-101 mm long, 6-8 mm in outer diameter and 4-6 mm in inner diameter.

Example 1

A test device for determining whether oily substances belong to bulk persistent oils comprises a 340 ℃ test module, a 370 ℃ test module and a control system, wherein the 340 ℃ test module and the 370 ℃ test module share one set of control system, the control system is respectively connected with the 340 ℃ test module and the 370 ℃ test module in a control mode, the 340 ℃ test module and the 370 ℃ test module are identical in structure, and each module consists of a temperature control system, a distillation system and a lifting system. The temperature control system comprises an electric heater, a crucible container and a heat transfer medium, wherein the crucible container is arranged on the electric heater, the heat transfer medium is arranged in the crucible container, the electric heater is used for heating the heat transfer medium in the crucible container and the crucible container, so that the heat transfer medium is in a molten state, and the temperature of the heat transfer medium can be controlled to be stabilized at 340 +/-2 ℃ or 370 +/-2 ℃. The control system is connected with the electric heater in a control mode. The distillation system comprises a distillation flask, a condenser pipe, a collection measuring cylinder and an electronic balance, wherein the condenser pipe is connected with an outlet of a side pipe of the distillation flask, the collection measuring cylinder is connected with an outlet of the condenser pipe, and the collection measuring cylinder is arranged on the electronic balance. The electronic balance is electrically connected with the control system. The lifting system is arranged below the temperature control system and used for controlling the lifting of the temperature control system so as to enable the heat transfer medium in the temperature control system to be in contact with or separated from the distillation flask. The lifting system is a lifting motor and is controlled and connected by a lifting control program in a control program. The lifting system is arranged below the temperature control system and used for controlling the lifting of the temperature control system, the temperature control system is lifted during a test, the distillation flask is immersed in a crucible container filled with molten salt, and a heat source is provided for the distillation flask; and after the test is finished, returning the temperature control system to the original position. The lifting system is mainly a lifting motor and is controlled by a lifting control program. The crucible container is cylindrical, the upper part of the crucible container is provided with an opening, a movable and rotatable cover is arranged at the opening, the cover is divided into two parts, the middle part of the cover is provided with a hole, and the diameter of the hole is slightly larger than that of the bottle neck part of the distillation flask. After the distillation flask is put into the crucible container, the cover is rotated from both sides to reduce the fluctuation of the internal temperature.

The crucible container has an outer diameter of 119mm, a wall thickness of 3mm and a height of 124 mm.

The crucible container is made of quartz. The heat transfer medium is potassium nitrate or sodium nitrate. In the test, potassium nitrate or sodium nitrate is in a molten state and serves as a molten salt bath to provide a stable temperature environment atmosphere, sodium nitrate provides a 340 ℃ molten salt environment, and potassium nitrate provides a 370 ℃ molten salt environment. The temperature control range of the electric heater is between room temperature and 600 ℃, and the precision is +/-2 ℃. The top end of the distillation flask is provided with a thermometer with the measuring range of room temperature to 400 ℃ for measuring the temperature of the distillate. The condenser pipe is a glass condenser pipe and is condensed by circulating water.

The volume of the measuring cylinder of the collecting measuring cylinder is 100mL, and the precision is 1 mL.

The precision of the electronic balance is 0.0001g, and the electronic balance is used for recording the mass of the distillate collected by the collecting measuring cylinder and sending the information to the control system.

The specification of the distillation flask is 124mL, the length of the flask neck is 149cm, the outer diameter is 20mm, and the inner diameter is 17 mm; the distance between the side pipe and the ball is 66mm, the length is 99mm, the outer diameter is 6mm, and the inner diameter is 4 mm.

Example 2

A test device for determining whether oily substances belong to bulk persistent oils comprises a 340 ℃ test module, a 370 ℃ test module and a control system, wherein the 340 ℃ test module and the 370 ℃ test module share one set of control system, the control system is respectively connected with the 340 ℃ test module and the 370 ℃ test module in a control mode, the 340 ℃ test module and the 370 ℃ test module are identical in structure, and each module consists of a temperature control system, a distillation system and a lifting system. The temperature control system comprises an electric heater, a crucible container and a heat transfer medium, wherein the crucible container is arranged on the electric heater, the heat transfer medium is arranged in the crucible container, the electric heater is used for heating the heat transfer medium in the crucible container and the crucible container, so that the heat transfer medium is in a molten state, and the temperature of the heat transfer medium can be controlled to be stabilized at 340 +/-2 ℃ or 370 +/-2 ℃. The control system is connected with the electric heater in a control mode. The distillation system comprises a distillation flask, a condenser pipe, a collection measuring cylinder and an electronic balance, wherein the condenser pipe is connected with an outlet of a side pipe of the distillation flask, the collection measuring cylinder is connected with an outlet of the condenser pipe, and the collection measuring cylinder is arranged on the electronic balance. The electronic balance is electrically connected with the control system. The lifting system is arranged below the temperature control system and used for controlling the lifting of the temperature control system so as to enable the heat transfer medium in the temperature control system to be in contact with or separated from the distillation flask. The lifting system is a lifting motor and is controlled and connected by a lifting control program in a control program. The lifting system is arranged below the temperature control system and used for controlling the lifting of the temperature control system, the temperature control system is lifted during a test, the distillation flask is immersed in a crucible container filled with molten salt, and a heat source is provided for the distillation flask; and after the test is finished, returning the temperature control system to the original position. The lifting system is mainly a lifting motor and is controlled by a lifting control program. The crucible container is cylindrical, the upper part of the crucible container is provided with an opening, a movable and rotatable cover is arranged at the opening, the cover is divided into two parts, the middle part of the cover is provided with a hole, and the diameter of the hole is slightly larger than that of the bottle neck part of the distillation flask. After the distillation flask is put into the crucible container, the cover is rotated from both sides to reduce the fluctuation of the internal temperature.

The crucible container has an outer diameter of 121mm, a wall thickness of 5mm and a height of 126 mm.

The crucible container is made of quartz. The heat transfer medium is potassium nitrate or sodium nitrate. In the test, potassium nitrate or sodium nitrate is in a molten state and serves as a molten salt bath to provide a stable temperature environment atmosphere, sodium nitrate provides a 340 ℃ molten salt environment, and potassium nitrate provides a 370 ℃ molten salt environment. The temperature control range of the electric heater is between room temperature and 600 ℃, and the precision is +/-2 ℃. The top end of the distillation flask is provided with a thermometer with the measuring range of room temperature to 400 ℃ for measuring the temperature of the distillate. The condenser pipe is a glass condenser pipe and is condensed by circulating water.

The volume of the measuring cylinder of the collecting measuring cylinder is 150mL, and the precision is 1 mL.

The precision of the electronic balance is 0.0001g, and the electronic balance is used for recording the mass of the distillate collected by the collecting measuring cylinder and sending the information to the control system.

The specification of the distillation flask is 126mL, the length of a bottleneck is 151cm, the outer diameter is 22mm, and the inner diameter is 19 mm; the side pipe is positioned 68mm above the round ball, and is 101mm long, 8mm in outer diameter and 6mm in inner diameter.

Example 3

A test device for determining whether oily substances belong to bulk persistent oils comprises a 340 ℃ test module, a 370 ℃ test module and a control system, wherein the 340 ℃ test module and the 370 ℃ test module share one set of control system, the control system is respectively connected with the 340 ℃ test module and the 370 ℃ test module in a control mode, the 340 ℃ test module and the 370 ℃ test module are identical in structure, and each module consists of a temperature control system, a distillation system and a lifting system. The temperature control system comprises an electric heater, a crucible container and a heat transfer medium, wherein the crucible container is arranged on the electric heater, the heat transfer medium is arranged in the crucible container, the electric heater is used for heating the heat transfer medium in the crucible container and the crucible container, so that the heat transfer medium is in a molten state, and the temperature of the heat transfer medium can be controlled to be stabilized at 340 +/-2 ℃ or 370 +/-2 ℃. The control system is connected with the electric heater in a control mode. The distillation system comprises a distillation flask, a condenser pipe, a collection measuring cylinder and an electronic balance, wherein the condenser pipe is connected with an outlet of a side pipe of the distillation flask, the collection measuring cylinder is connected with an outlet of the condenser pipe, and the collection measuring cylinder is arranged on the electronic balance. The electronic balance is electrically connected with the control system. The lifting system is arranged below the temperature control system and used for controlling the lifting of the temperature control system so as to enable the heat transfer medium in the temperature control system to be in contact with or separated from the distillation flask. The lifting system is a lifting motor and is controlled and connected by a lifting control program in a control program. The lifting system is arranged below the temperature control system and used for controlling the lifting of the temperature control system, the temperature control system is lifted during a test, the distillation flask is immersed in a crucible container filled with molten salt, and a heat source is provided for the distillation flask; and after the test is finished, returning the temperature control system to the original position. The lifting system is mainly a lifting motor and is controlled by a lifting control program. The crucible container is cylindrical, the upper part of the crucible container is provided with an opening, a movable and rotatable cover is arranged at the opening, the cover is divided into two parts, the middle part of the cover is provided with a hole, and the diameter of the hole is slightly larger than that of the bottle neck part of the distillation flask. After the distillation flask is put into the crucible container, the cover is rotated from both sides to reduce the fluctuation of the internal temperature.

The crucible container has an outer diameter of 120mm, a wall thickness of 5mm and a height of 125 mm.

The crucible container is made of quartz. The heat transfer medium is potassium nitrate or sodium nitrate. In the test, potassium nitrate or sodium nitrate is in a molten state and serves as a molten salt bath to provide a stable temperature environment atmosphere, sodium nitrate provides a 340 ℃ molten salt environment, and potassium nitrate provides a 370 ℃ molten salt environment. The temperature control range of the electric heater is between room temperature and 600 ℃, and the precision is +/-2 ℃. The top end of the distillation flask is provided with a thermometer with the measuring range of room temperature to 400 ℃ for measuring the temperature of the distillate. The condenser pipe is a glass condenser pipe and is condensed by circulating water.

The volume of the measuring cylinder of the collecting measuring cylinder is 100mL, and the precision is 1 mL.

The precision of the electronic balance is 0.0001g, and the electronic balance is used for recording the mass of the distillate collected by the collecting measuring cylinder and sending the information to the control system.

The specification of the distillation flask is 125mL, the length of a bottleneck is 150cm, the outer diameter is 21mm, and the inner diameter is 18 mm; the side pipe is 67mm away from the upper part of the round ball, the length is 100mm, the outer diameter is 7mm, and the inner diameter is 5 mm.

The working process is as follows:

1. connecting the components:

the electric heater, the crucible container and the heat-conducting medium form a temperature control system. The crucible container is installed in the electric heater, and the heat transfer medium is placed in the crucible container.

The lifting motor and the accessories thereof form a lifting system. The lifting motor controls the lifting of the temperature control system.

The test sample, distillation flask, thermometer, condenser, collection cylinder, and electronic balance comprise a distillation system.

The test sample was placed in a distillation flask, a thermometer was installed at the outlet above the distillation flask, a condenser was attached to the side tube of the distillation flask, and a collection cylinder was placed on an electronic balance below the outlet of the condenser.

The control equipment and the program thereof are a control system for controlling the temperature of the temperature control system, the lifting of the lifting system, the sample distillation record of the distillation system and the like.

Note that: in use, it is recommended that the test be carried out in a fume hood having an air flow rate of 0.5 m/s or less, the exhaust system being adapted to absorb toxic fumes, and then the test be carried out according to the following steps:

2. the method comprises the following steps:

(1) preparation of samples

6 groups of samples were measured, each group being 100 mL. Three groups were used for 340 ℃ testing, and three groups were used for 370 testing, sealed, and stored in an environment below 10 ℃.

(2) Preparing an instrument before testing:

and opening a testing instrument and a program, operating a temperature control system, heating the crucible container and the heat-conducting medium, and preparing for testing after the heat-conducting medium is stabilized at 340 ℃ and 370 ℃.

(3) Testing

A set of samples was added to the distillation flasks of the 340 ℃ test module and the 370 ℃ test module, respectively, and the distillation system was connected. And starting the lifting device, and immersing the distillation flask into a heat-conducting medium for testing.

In the experimental process, the distillate is collected by a measuring cylinder. When the mass increase is less than 0.04g within 10min, the test is automatically stopped. Record the volume of the sluicing in the cylinder.

After completion of the test, the same test was performed with the remaining two groups of samples, and the volume of fractions from each group was recorded.

Other requirements in the test process refer to GB/T6536-2010 atmospheric distillation characterization of petroleum products.

(4) Calculation of results

The volume data of three groups of fractions measured by a 340 ℃ test module and a 370 ℃ test module are respectively averaged, and the obtained volume average of the fractions is compared with a classification principle of the bulk permanent oils (the evaporation of the fractions is less than 50% of the total volume of hydrocarbons under the condition of the 340 ℃ temperature, and the evaporation of the fractions is less than 95% of the total volume of the hydrocarbons under the condition of the 370 ℃ temperature), so as to determine whether the oily substances belong to the bulk permanent oils.

It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art may make modifications, alterations, additions or substitutions within the spirit and scope of the present invention.

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