Atmospheric and vacuum distillation process

Abstract

The invention discloses an atmospheric-vacuum distillation process and belongs to the technical field of distillation. Heating the sulfur-containing sewage into the distillation flask, and adding inert liquid; the distillation flask is heated, the temperature of the distillation flask is detected in real time through a temperature sensor, the pressure in the distillation flask is detected in real time through a pressure sensor, and negative pressure of the distillation flask is maintained through a capillary pressure reduction pipe extending into the distillation flask; the steam distilled from the distillation flask is condensed through the condenser, and the condensate is collected. According to the atmospheric and vacuum distillation process, through the temperature sensor and the pressure sensor, the temperature of liquid in the distillation flask and the pressure intensity in the distillation flask can be conveniently detected, the purpose of controlling the temperature and the pressure intensity during an experiment is further achieved, the condenser can enable water to be liquefied and condensed water to be liquefied in a contact mode, and the experiment efficiency is improved. Meanwhile, distillation can be selected under a normal pressure condition or a low pressure condition according to whether a capillary pressure reduction pipe is installed or not.

Description

Technical Field

[0001] The invention discloses a normal and reduced pressure distillation process, belonging to the technical field of distillation. Background Art

[0002] Oil refining generally refers to petroleum refining. Originally, oil was separated by distillation to produce kerosene, gasoline, diesel and other fuel oils suitable for use in internal combustion engines, with petroleum gas and residual oil as by-products; components heavier than fuel oil were chemically converted into fuel oils through processes such as thermal cracking and catalytic cracking, and some of these fuel oils were refined by processes such as hydrogenation. The heaviest vacuum residue oil is produced by solvent deasphalting to produce deasphalted oil and petroleum asphalt, or heavy oil is cracked into fuel oil components through delayed coking, and petroleum coke is produced as a by-product. However, the wastewater remaining in the oil refining process contains a large amount of sulfur and other elements. The sulfur-containing wastewater produced by oil refining is difficult to directly reuse in the next oil refining. The sulfur-containing wastewater needs to be distilled. In the laboratory, it is difficult to control the temperature and pressure during the distillation of sulfur-containing wastewater, which is not convenient for accurate control of the data of the distillation experiment of sulfur-containing wastewater. At the same time, the water vapor condensation efficiency is low, which easily causes the problem of waste caused by water vapor discharge. Summary of the invention

[0003] The technical problem to be solved by the present invention is to overcome the deficiencies of the prior art and provide a normal and low pressure distillation process which can conveniently detect the pressure and temperature in the distillation flask, thereby conveniently controlling the temperature and pressure.

[0004] The technical solution adopted by the present invention to solve the technical problem is: the atmospheric and vacuum distillation process is characterized by comprising the following steps: Step S1, heating the sulfur-containing wastewater in a distillation flask and adding an inert liquid; Step S2, heating the distillation flask, detecting the temperature of the distillation flask in real time through a temperature sensor, detecting the pressure in the distillation flask in real time through a pressure sensor, and maintaining a negative pressure in the distillation flask through a capillary pressure reducing tube extending into the distillation flask; Step S3, condensing the steam distilled from the distillation flask through a condenser and collecting the condensate.

[0005] Preferably, the inert liquid is a fluorocarbon inert liquid.

[0006] Preferably, the distillation flask is heated in stages to achieve distillation of the sulfur-containing wastewater by a staged distillation method.

[0007] Preferably, an air guide pipe is connected to the upper part of the distillation flask, and the air guide pipe guides the steam into the distillation flask.

[0008] Preferably, the temperature of the steam in the air duct is measured by a thermometer.

[0009] Preferably, the condenser includes a shell and a condensing tube arranged in the shell, and an air inlet pipe and a liquid outlet pipe are respectively arranged at opposite ends of the shell. The two ends of the condensing tube are respectively connected to the air inlet pipe and the liquid outlet pipe, and the two ends of the shell are also connected to a water inlet pipe and a water outlet pipe.

[0010] Preferably, the condenser also includes a connecting pipe, and connecting pipes are provided at both ends of the shell, the air inlet pipe and the liquid outlet pipe are respectively connected to the connecting pipes on the corresponding sides, and a plurality of condensing pipes are arranged side by side, and both ends of each condensing pipe are respectively connected to the connecting pipes on the corresponding sides.

[0011] Preferably, a solenoid valve is provided at the gas outlet of the distillation flask, and the pressure of the distillation flask is adjusted by the opening of the solenoid valve.

[0012] Preferably, the condensed water discharged from the condenser is collected by a water storage tank.

[0013] Compared with the prior art, the present invention has the following beneficial effects: This atmospheric and vacuum distillation process uses temperature sensors and pressure sensors to detect the liquid temperature inside the distillation flask, as well as the pressure inside the distillation flask, thereby increasing the purpose of controlling temperature and pressure during the experiment. The condenser can liquefy water, and the condensed water is contact-liquefied, thereby achieving the purpose of low-temperature and low-pressure distillation of sulfur-containing wastewater. At the same time, depending on whether a capillary vacuum tube is installed, distillation can be selected under atmospheric pressure or low pressure conditions. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 It is a three-dimensional schematic diagram of a atmospheric and vacuum distillation apparatus; Figure 2 It is a three-dimensional schematic diagram of the connection between the water collecting plate and the condensation plate.

[0015] 1. Solar power generation base plate; 2. Electric furnace; 3. Distillation flask; 4. First support rod; 5. Bracket; 6. Temperature sensor; 7. Pressure sensor; 8. Air duct; 9. Capillary pressure reducing tube; 10. Solenoid valve; 11. Thermometer; 12. Condenser; 13. Air inlet pipe; 14. Liquid outlet pipe; 15. Second support rod; 16. Clamp; 17. Water storage tank; 18. Exhaust pipe; 19. Water inlet pipe; 20. Water outlet pipe; 21. Condenser; 22. Connecting pipe. DETAILED DESCRIPTION

[0016] The present invention is further described below in conjunction with specific embodiments. However, people familiar with the art should understand that the detailed description given here in conjunction with the drawings is for better explanation, and the structure of the present invention necessarily exceeds these limited embodiments. For some equivalent replacement schemes or common means, they are no longer described in detail herein, but still belong to the scope of protection of the present application.

[0017] Figure 1~2 The best embodiment of the present invention is shown below in conjunction with the attached Figure 1~2 The present invention is further described.

[0018] like Figure 1-2 As shown, the atmospheric and vacuum distillation device includes a distillation flask 3, a heating device, a condenser 12 and a capillary vacuum tube 9. The heating device is arranged at the lower side of the distillation flask 3. The upper part of the distillation flask 3 is connected with the input port of the condenser 12. The distillation flask 3 is provided with a temperature detection element and a pressure detection element. The lower end of the capillary vacuum tube 9 extends into the lower part of the distillation flask 3. The atmospheric and vacuum distillation device is convenient for detecting the liquid temperature inside the distillation flask 3 and the pressure inside the distillation flask 3 through the temperature detection element and the pressure detection element installed on the surface of the distillation flask, thereby increasing the purpose of controlling the temperature and pressure during the experiment. The condenser 12 can liquefy water, and the condensed water is contact-liquefied, thereby achieving the purpose of low-temperature and low-pressure distillation 3 of sulfur-containing wastewater. At the same time, according to whether the capillary vacuum tube 9 is installed, it is also possible to choose to distill under normal pressure or low pressure conditions.

[0019] The atmospheric and vacuum distillation device further comprises a solar power generation bottom plate 1, and a heating device is mounted on the solar power generation bottom plate 1. In this embodiment, the heating device is an electric furnace 2. A first support rod 4 is also mounted on the solar power generation bottom plate 1, and a bracket 5 is arranged on the first support rod 4, and a distillation flask 3 is mounted on the bracket 5. The electric furnace 2 is located directly below the distillation flask 3 to achieve heating of the distillation flask 3.

[0020] In this embodiment, the temperature detection element is a temperature sensor 6, and the pressure detection element is a pressure sensor 7. Both the temperature sensor 6 and the pressure sensor 7 are installed on the distillation flask 3 to detect the temperature and pressure in the distillation flask 3 in real time.

[0021] The lower end of the capillary pressure reducing tube 9 extends into the bottom of the distillation flask 3. When distillation is performed, the lower end of the capillary pressure reducing tube 9 is located below the liquid level.

[0022] An air guide tube 8 is provided on one side of the distillation flask 3, the lower end of which is bent toward the distillation flask 3 and connected to the upper part of the distillation flask 3, and a thermometer 11 is provided on the top of the distillation flask 3 for real-time detection of the temperature of the steam in the air guide tube 8. An electromagnetic valve 10 is provided between the air guide tube 8 and the distillation flask 3 for controlling the speed and on-off of the steam discharge.

[0023] A second support rod 15 is also provided on the upper side of the conditioning and power generation base plate 1. The second support rod 15 is vertically arranged. Two second support rods 15 are arranged at intervals. A clamp 16 is provided on each second support rod 15. The condenser 12 is arranged between the two second support rods 15. The two clamps 16 clamp the two sides of the condenser 12 respectively to achieve the fastening of the condenser 12. The condenser 12 is gradually inclined downward along the side away from the distillation flask 3. A water storage tank 17 is provided on the upper side of the solar power generation base plate 1 on the side of the condenser 12 away from the distillation flask 3 for storing condensed water.

[0024] The condenser 12 includes a shell, a condenser tube 21 and a connecting tube 22. The connecting tube 22 has two connecting tubes 22 arranged at both ends, and each connecting tube 22 seals both ends of the shell. The condenser tube 21 is arranged in the shell, and the condenser tube 21 is located between the two connecting tubes 22. The two ends of the condenser tube 21 are respectively connected to the connecting tube 22 on the corresponding side. The connecting tube 22 near the distillation flask 3 is connected to the air inlet pipe 13, and the air inlet pipe 13 is connected to the side of the air guide pipe 8. The connecting tube 22 near the water storage tank 17 is connected to the liquid outlet pipe 14, and the liquid outlet pipe 14 is connected to the water storage tank 17.

[0025] A water outlet pipe 20 is connected to the upper side of the housing near the distillation flask 3, and a water inlet pipe 19 is connected to the lower side of the housing near the water storage tank 17, so that the housing is filled with cooling water. An exhaust pipe 18 is connected to the top of the water storage tank 17.

[0026] The temperature sensor 6 and the pressure sensor 7 installed on the surface of the distillation flask 3 make it convenient for the temperature sensor 6 to detect the temperature of the liquid inside the distillation flask 3, and the pressure sensor 7 to detect the pressure inside the distillation flask 3, thereby increasing the purpose of controlling the temperature and pressure during the experiment. The solar power generation base plate 1 is used as the support plate, which is convenient for the solar power generation base plate 1 to store electric energy after being exposed to the sun, thereby reducing the loss of electric energy. The solenoid valve 10 installed on the air duct 8 is convenient for adjusting the opening and closing degree of the solenoid valve 10 and adjusting the pressure inside the distillation flask 3. The connecting pipe 22 and the condensing pipe 21 installed in the condenser 12 make it convenient for the water vapor inside the connecting pipe 22 to contact and liquefy with the condensed water inside the condenser 12, thereby achieving the purpose of low-temperature and low-pressure distillation of sulfur-containing wastewater. At the same time, depending on whether the capillary pressure reducing tube 9 is installed, it is possible to choose to distill under normal pressure or low pressure conditions.

[0027] The condenser tube 21 is a zigzag tubular component, and the bending angle of the condenser tube 21 is 30 degrees. Fifteen condenser tubes 21 are installed between the two connecting tubes 22 at equal intervals.

[0028] The solar power generation bottom plate 1 is a rectangular plate-shaped member. The angle between the condenser 12 and the solar power generation bottom plate 1 is 40°.

[0029] A atmospheric and vacuum distillation process comprises the following steps: Step S1, heating the sulfur-containing wastewater in the distillation flask 3 and adding an inert liquid.

[0030] The distillation preparation includes exposing the solar power generation base plate 1 to the sun to store electric energy, selecting an appropriate amount of sulfur-containing waste water from refinery gas for standby use, and an appropriate amount of condensed water for standby use.

[0031] The parameters are set as follows: the temperature of the liquid inside the distillation flask 3 is 10-30°C, and the pressure inside the distillation flask 3 is 0.4-0.8kPa. When the temperature sensor 6 detects that the temperature of the liquid inside the distillation flask 3 is lower than 10°C, the electric furnace 2 increases the power; when the temperature of the liquid inside the distillation flask 3 is higher than 30°C, the electric furnace 2 reduces the power; when the pressure sensor 7 detects that the pressure inside the distillation flask 3 is higher than 0.8kPa, the opening degree of the solenoid valve 10 is increased; when the pressure inside the distillation flask 3 is lower than 0.4kPa, the opening degree of the solenoid valve 10 is reduced.

[0032] Step S2, heating the distillation flask 3, detecting the temperature of the distillation flask 3 in real time through the temperature sensor 6, detecting the pressure inside the distillation flask 3 in real time through the pressure sensor 7, and maintaining a negative pressure in the distillation flask 3 through the capillary pressure reducing tube 9 extending into the distillation flask 3.

[0033] In the distillation operation, a proper amount of sulfur-containing wastewater is injected into the distillation flask 3, and the electric furnace 2 is powered by the solar power generation bottom plate 1 to heat the distillation flask 3. The liquid inside the distillation flask 3 rises under the action of the capillary pressure reducing tube 9, so that a negative pressure is formed in the distillation flask 3. After the liquid inside the distillation flask 3 evaporates, it enters the air inlet pipe 13 through the air guide pipe 8. The solenoid valve 10 adjusts the flow rate of the gas by adjusting the opening and closing degree. The thermometer 11 is used to detect the temperature of the gas. The condensed water is injected into the condenser 12 through the water inlet pipe 19 and then discharged from the water outlet pipe 20, while the steam inside the air inlet pipe 13 enters the condenser 12 and liquefies. The liquefied water is gathered into the water storage tank 17 through the liquid outlet pipe 14, and part of the gas is discharged through the exhaust pipe 18; Step S3, condensing the steam distilled from the distillation flask 3 through the condenser 12, and collecting the condensate.

[0034] After the distillation is finished, the power supply of the electric furnace 2 and the solar power generation base plate 1 is disconnected, and the electric furnace 2 is moved away. The air duct 8 on the upper end of the distillation flask 3 is removed, and the air duct 8 is separated from the air inlet pipe 13, and the liquid outlet pipe 14 is separated from the water storage tank 17, and the distillation flask 3 is cleaned.

[0035] Specifically, the distillation operation adopts the staged distillation method, in which the liquid is first heated at a low temperature to produce a small amount of vapor, and then the temperature is increased in stages to produce more vapor, and finally the separated substances are obtained, thereby effectively controlling the liquid mixing ratio and improving the separation effect.

[0036] Specifically, an inert liquid is added during the distillation operation. The inert liquid is a fluorine-containing special reagent fluorocarbon inert liquid. The molecule does not contain chlorine or hydrogen atoms. It is a saturated organic fluorine compound containing 1-15 carbon atoms composed of fluorine, carbon or oxygen and nitrogen atoms. It has unique properties such as chemical inertness, thermal conductivity, low toxicity, non-flammability, high electrical resistance, low surface tension and low thermal conductivity.

[0037] The above is only a preferred embodiment of the present invention, and does not limit the present invention in other forms. Any technician familiar with the profession may use the above disclosed technical content to change or modify it into an equivalent embodiment with equivalent changes. However, any simple modification, equivalent change and modification made to the above embodiment according to the technical essence of the present invention without departing from the technical solution of the present invention still belongs to the protection scope of the technical solution of the present invention.

Claims

1. A atmospheric and vacuum distillation process, characterized in that: The steps include: Step S1, heating the sulfur-containing wastewater in a distillation flask (3) and adding an inert liquid; Step S2, heating the distillation flask (3), detecting the temperature of the distillation flask (3) in real time through the temperature sensor (6), detecting the pressure in the distillation flask (3) in real time through the pressure sensor (7), and maintaining a negative pressure in the distillation flask (3) through a capillary pressure reducing tube (9) extending into the distillation flask (3); Step S3, condensing the steam distilled from the distillation flask (3) through a condenser (12), and collecting the condensate.

2. The atmospheric and vacuum distillation process according to claim 1, characterized in that: The inert liquid is a fluorocarbon inert liquid.

3. The atmospheric and vacuum distillation process according to claim 1, characterized in that: The distillation flask (3) is heated in sections to achieve distillation of the sulfur-containing wastewater by a sectioned distillation method.

4. The atmospheric and vacuum distillation process according to claim 1, characterized in that: An air guide tube (8) is connected to the upper part of the distillation flask (3), and the air guide tube (8) guides steam into the distillation flask (3).

5. The atmospheric and vacuum distillation process according to claim 4, characterized in that: The temperature of the steam in the air duct (8) is measured by a thermometer (11).

6. The atmospheric and vacuum distillation process according to claim 1, characterized in that: The condenser (12) comprises a shell and a condensing tube (21) arranged in the shell, an air inlet pipe (13) and a liquid outlet pipe (14) are respectively arranged at two opposite ends of the shell, and the two ends of the condensing tube (21) are respectively connected to the air inlet pipe (13) and the liquid outlet pipe (14), and the two ends of the shell are also connected to a water inlet pipe (19) and a water outlet pipe (20).

7. The atmospheric and vacuum distillation process according to claim 6, characterized in that: The condenser (12) further comprises a connecting pipe (22), and connecting pipes (22) are arranged at both ends of the shell. The air inlet pipe (13) and the liquid outlet pipe (14) are respectively connected to the connecting pipes (22) on the corresponding sides. A plurality of condensing pipes (22) are arranged side by side, and both ends of each condensing pipe (21) are respectively connected to the connecting pipes (22) on the corresponding sides.

8. The atmospheric and vacuum distillation process according to claim 1, characterized in that: A solenoid valve (10) is provided at the gas outlet of the distillation flask (3), and the pressure of the distillation flask (3) is adjusted by adjusting the opening of the solenoid valve (10).

9. The atmospheric and vacuum distillation process according to claim 1, characterized in that: The condensed water discharged from the condenser (12) is collected by a water storage tank (17).

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