Using method of green absolute ethyl alcohol refining practice device capable of carrying out sieve plate and filler rectification contrast experiment

Abstract

The invention discloses a use method of a green absolute ethyl alcohol refining practice device capable of carrying out a sieve plate and filler rectification contrast experiment, and particularly relates to the technical field of ethyl alcohol production. 2, checking and preparing equipment; 3, preparing a solution; 4, feeding and refluxing, and then extracting; step 5, treating tower kettle overflow kettle liquid in a tank; and step 6, tower kettle overflow kettle liquid tank treatment. Compared with the prior art, the method can be used for carrying out contrast experiments and continuous production, provides possibility for process optimization, and can be used for screening an excellent rectification mode through contrast, improving the purity of absolute ethyl alcohol and the product quality and defining the energy-saving effect so as to reduce the cost, strict valve inspection, accurate solution preparation, coordination of equipment operation, reasonable control of rotating speed and flow and the like in operation; accuracy and stability are improved, and controllability and repeatability are enhanced through clear qualified standards and normative exception handling.

Description

Technical Field

[0001] The invention relates to the technical field of ethanol production, and more specifically to a method for using a green anhydrous ethanol refining practice device capable of performing a sieve plate and filler distillation comparison experiment. Background Art

[0002] In the chemical industry, the production of anhydrous ethanol is an important topic. With the increasing requirements for energy and environmental protection, the refining technology of green anhydrous ethanol has attracted much attention. Lepark's original green anhydrous ethanol refining practice device adopts a three-tower distillation process to prepare anhydrous ethanol. The three towers, crude ethanol refining tower, extractive distillation tower and solvent recovery tower are all packed towers.

[0003] Although this process can be used for continuous anhydrous ethanol production, it has certain limitations. On the one hand, the process using only packed towers cannot meet the needs of the comparative experiment of distillation effects of different types of distillation towers. In teaching and scientific research, comparing the effects of different distillation methods is crucial for in-depth understanding of distillation principles and optimization of process parameters. On the other hand, in actual production, a single packed tower process may have shortcomings in some aspects, such as limited improvement in product purity, high energy consumption, and less than ideal operating stability. In order to overcome these limitations, it is necessary to improve the existing process. Therefore, a method for using a green anhydrous ethanol refining practice device that can perform sieve plate and packed distillation comparative experiments is proposed to meet the various needs of teaching, scientific research and actual production. Summary of the invention

[0004] In order to overcome the above-mentioned defects of the prior art, the present invention provides a method for using a green anhydrous ethanol refining practice device capable of conducting sieve plate and filler distillation comparative experiments, so as to solve the problems raised in the above-mentioned background technology.

[0005] To achieve the above object, the present invention provides the following technical solution: a method for using a green anhydrous ethanol refining practice device capable of conducting a sieve plate and filler distillation comparison experiment, specifically comprising the following steps:

[0006] Step 1: Turn on the device and power on the main power supply and control power supply of the unit module;

[0007] Step 2: Equipment inspection and preparation, check whether the temperature and pressure display are normal, and check whether the valve status is in the closed state;

[0008] Step 3: Solution preparation. After confirming that the valve status is correct, add ethanol and purified water through the VA101 feed port to prepare the ethanol solution. Add 1.5-2L of ethanol solution to the kettle of the preparation tower. The liquid level of the kettle should be higher than the upper edge of the electric heater.

[0009] Step 4: After the feed is refluxed, it is extracted, the tower kettle is started to heat, and the tower top air cooler is turned on at the same time. When steam is generated, the tower top temperature changes, and there is a liquid level in the fractionator, the full reflux operation is started. After the crude ethanol refining tower runs stably, the feed pump is turned on, the flow meter is turned on to start feeding, and the top product concentration is analyzed every 5 minutes. If the product concentration is unqualified, the valve is opened, the material enters the ethanol tank, and the material is re-fed. After the product concentration is qualified, the valve is closed, and the valve is opened to start extraction;

[0010] Step 5: When the tower kettle overflows and the kettle liquid tank is treated, when the tower kettle liquid level reaches the overflow level, the tower kettle air cooler and the tower kettle peristaltic pump are turned on, and the wastewater tank valve is opened, and the tower kettle overflow liquid enters the wastewater tank or kettle liquid tank of the unit module;

[0011] Step six: Treatment of the overflow kettle liquid tank of the tower bottom. During the experiment, observe the tower bottom pressure and adjust the tower bottom heating power, feed rate and reflux rate in time. When the tower bottom overflow liquid enters the kettle liquid tank, when the kettle liquid tank level reaches 1 / 3 of the liquid level, start the feed pump. When the solvent recovery tower bottom liquid level reaches 1 / 2 of the overflow liquid level, stop adding, turn on the electric heating, turn on the tower top air cooler, start the full reflux operation, turn on the feed pump after the full reflux is stable, analyze the concentration of the tower top and tower bottom overflow liquid every 5 minutes, and judge the qualification degree of the tower top condensate and the tower bottom overflow liquid. If the solvent recovery tower bottom concentration is unqualified, open the tower bottom liquid reflux pipeline, open the air cooler and the valve, and let the solvent recovery tower bottom overflow liquid return to the kettle liquid tank.

[0012] Preferably, the unit module in step one is one of a crude ethanol refining unit module and an extractive distillation unit module, and the production tower in step three is one of a crude ethanol refining tower and an extractive distillation tower, the crude ethanol refining tower is specifically a sieve plate distillation tower, and the extractive distillation tower is specifically a packed distillation tower.

[0013] Preferably, the full reflux operation in step 4 is specifically to open the reflux pump P102 and turn on the flow meter FI102. The feed flow rate in step 4 is 80 ml / min and the reflux ratio is 2:1.

[0014] Preferably, in step six, the tower bottom pressure is observed and the tower bottom heating power, feed rate and reflux rate are adjusted in time to avoid flooding. The full reflux operation in step six is ​​specifically to open the reflux pump P206 and turn on the flow meter FI202.

[0015] Preferably, in step 6, the criteria for judging the qualification of the tower top condensate and the tower bottom overflow liquid are that the tower top condensate is qualified if it does not contain ethylene glycol, the tower top temperature is <100°C, the tower bottom overflow liquid is qualified if the ethylene glycol concentration reaches 98% or more, and the tower bottom temperature is ≥196°C.

[0016] Preferably, in step 2, the inspection of the valve status should include confirming that the valve is tightly closed and has no leakage.

[0017] Preferably, in step 5, the rotation speeds of the tower kettle air cooler and the tower kettle peristaltic pump are adjusted between 20-60 rpm to avoid large fluctuations in the rotation speed from affecting the experiment.

[0018] Preferably, the volume fraction of the ethanol solution prepared in step 3 is about 40% to ensure the reliability of the experimental results. When adding ethanol and pure water to prepare the solution, it should be ensured that the solution is mixed evenly and the volume fraction is measured accurately.

[0019] Preferably, in step 4, the start-up of the feed pump and the flow meter should be coordinated to ensure stable control of the feed flow rate.

[0020] Preferably, in step six, the speed of the feed pump is adjusted to 60 rpm, and the reflux ratio is 5:1.

[0021] Technical effects and advantages of the present invention:

[0022] 1. By comparing the effects of different distillation methods, it is convenient to screen out a better distillation method for application in the production process, which is helpful to further optimize the process parameters, improve the purity of anhydrous ethanol, reduce the impurity content, and improve the overall quality of the product. While conducting comparative experiments, it does not affect the continuous production of anhydrous ethanol, maintains a stable product output, and ensures production efficiency. During the experiment, the tower bottom pressure can be observed and the heating power, feed rate and reflux rate can be adjusted in time to avoid liquid flooding, thereby improving the controllability of the experiment. According to the clear qualified standards of the tower top condensate and the tower bottom overflow liquid, the experimental results are clearer and clearer, which is convenient for adjusting and optimizing the experimental process. The treatment method for the unqualified concentration of the solvent recovery tower bottom is clear, which makes the experimental operation more standardized and improves the repeatability of the experiment.

[0023] 2. By comparing the effects of different distillation towers, we can analyze which distillation method is more energy-efficient, and then reasonably select and optimize the operation to achieve efficient use of energy and reduce production costs. The inspection of the valve status includes confirming that it is tightly closed and leak-free, which improves the accuracy and safety of the experimental operation, ensures that the volume fraction of the ethanol solution is about 40% and is evenly mixed and accurately measured, and ensures the reliability of the experimental results. The feed pump and flow meter are turned on in a coordinated manner to ensure stable control of the feed flow, which is conducive to the stable progress of the experimental process;

[0024] 3. In summary, through the mutual influence of the above-mentioned multiple effects, the use method of the green anhydrous ethanol refining practice device that can carry out sieve plate and filler distillation comparative experiments has many important beneficial effects. In terms of teaching and scientific research, it enriches the experimental courses, helps students and scientific researchers to deeply understand different distillation methods, and improves the quality of teaching and scientific research. In production, comparative experiments can be carried out, and continuous production can be carried out at the same time, which provides the possibility for process optimization. By comparing and screening the best distillation method, the purity of anhydrous ethanol and product quality can be improved, and the energy-saving effect can be clearly defined to reduce costs. In operation, strict valve inspection, accurate solution preparation, coordinated equipment operation and reasonable control of speed and flow rate, etc., improve accuracy and stability, and clear qualification standards and standardized exception handling enhance controllability and repeatability. In short, this method interacts with each other in teaching, production and operation, bringing important value and contribution to the field of green anhydrous ethanol refining. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a schematic diagram of the structure between the crude ethanol tank V-101 and the feed pump P104 of the present invention.

[0026] Figure 2 It is a schematic diagram of the structure between the anhydrous ethanol V203 and the solvent tank V208 of the present invention. DETAILED DESCRIPTION

[0027] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0028] Embodiment 1:

[0029] Step 1: Power on and turn on the main power supply and control power supply of the crude ethanol refining unit module;

[0030] Step 2: Check whether the temperature and pressure display are normal, and check whether the valve status is closed;

[0031] Step 3: After confirming that the valve status is correct, add ethanol and pure water through the VA101 feed port to prepare a crude ethanol solution with a volume fraction of about 40%; add about 2L of crude ethanol solution to the kettle of the crude ethanol refining tower, and the liquid level of the kettle is higher than the upper edge of the electric heating;

[0032] Step 4: Start heating the kettle of crude ethanol refining tower, and open the tower top air cooler at the same time, wait for steam to be generated, the tower top temperature changes, and when there is liquid level in the fractionator V103, start full reflux operation (open the reflux pump P102 and open the flowmeter FI102), and after the crude ethanol refining tower runs stably, open the feed P101, open the flowmeter FI101 to start feeding, the feed flow rate is about 80ml / min, and the reflux ratio is 2:1; analyze the tower top product concentration every 5 minutes, if the product concentration is unqualified, open the valve VA111, the material enters the ethanol tank V101, re-feed, close the valve VA111 after the product concentration is qualified, and open the valve VA114 to start extraction;

[0033] Step 5: When the tower bottom liquid level reaches the overflow level, turn on the tower bottom air cooler and the tower bottom peristaltic pump, adjust the speed to about 20-60rpm, open the wastewater tank valve VA218, and the tower bottom overflow liquid enters the wastewater tank of the extraction distillation module;

[0034] Step 6: During the experiment, pay attention to the tower kettle pressure and adjust the tower kettle heating power, feed rate and reflux rate in time to avoid flooding.

[0035] Embodiment 2:

[0036] Step 1: Power on and turn on the main power supply and control power supply of the extraction and distillation unit module;

[0037] Step 2: Check whether the temperature and pressure display are normal, check whether the valve status is in the closed state, and pay attention to the closing of valve VA245;

[0038] Step 3: After the valve status is confirmed to be correct, add ethanol and pure water through the VA115 feed port to prepare a crude ethanol solution with a volume fraction of about 40%; add about 2L of crude ethanol solution to the kettle of the extractive distillation tower, and the liquid level of the kettle is higher than the upper edge of the electric heater;

[0039] Step 4: Start the extraction distillation tower kettle heating and open the top air cooler. When steam is generated, the top temperature changes, and liquid appears in the fractionator V202, start the full reflux operation, open the reflux pump P202, and open the flow meter FI202. After the extraction distillation tower is stable, turn on the feed pump P104, open the flow meter FI201 to start feeding, the feed flow rate is about 80ml / min, and the reflux ratio is 2:1; analyze the top product concentration every 5 minutes. If the product concentration is unqualified, open valve VA206, and the material enters the 95% ethanol tank V104, re-feed, and close valve VA206 when the product concentration is qualified, and open valve VA207 to start extraction

[0040] Step 5: When the tower bottom liquid level reaches the overflow level, turn on the tower bottom air cooler and the tower bottom peristaltic pump, adjust the speed to about 20-40rpm, open the wastewater tank valve VA218, and the tower bottom overflow liquid enters the wastewater tank of the extraction distillation module;

[0041] Step 6: During the experiment, pay attention to the tower kettle pressure and adjust the tower kettle heating power, feed rate and reflux rate in time to avoid flooding.

[0042] Embodiment 3:

[0043] Step 1: Power on and turn on the main power supply and control power supply of the extraction and distillation unit module;

[0044] Step 2: Check whether the temperature and pressure display are normal, and check whether the valve status is closed;

[0045] Step 3: Add 1.5L ethylene glycol and 0.5L 95 ethanol to the extractive distillation tower, and the liquid level reaches 5-10cm above the transparent liquid level gauge, and add 15L-20L ethylene glycol solution to the solvent tank;

[0046] Step 4: Start the extraction distillation tower kettle heating, open the tower top air cooler, wait for steam to be generated, that is, the tower top temperature changes, start the full reflux operation, open the reflux pump P202, open the flow meter FI202, and when the crude ethanol refining unit distillation tower starts to be produced, open the raw material pump P104 and the solvent pump P208, and start feeding the tower 2, the 95 ethanol feed flow rate is 20ml / min, and the ethylene glycol feed flow rate is 60ml / min (3ml / rpm); the solvent ratio is 3:1, and the reflux ratio is 2:1. During the experiment, the concentration of the top product of the extraction distillation tower is analyzed every 5 minutes. After the concentration is qualified, the anhydrous ethanol tank valve VA207 is opened and the product is produced to the anhydrous ethanol tank V203;

[0047] Step 5: When the tower kettle liquid level reaches the overflow level, open the tower kettle air cooler and the tower kettle peristaltic pump P201, the kettle liquid tank inlet valve VA209, adjust the speed at 60rpm, and the tower kettle overflow liquid enters the V204 kettle liquid tank;

[0048] Step six: When the liquid level of V204 reaches 1 / 3, start the feed pump P204. When the liquid level of the bottom of the solvent recovery tower reaches 1 / 2 of the overflow level, stop adding, turn on the electric heating, turn on the top air cooler, and start the full reflux operation (turn on the reflux pump P206 and turn on the flowmeter FI202). After the full reflux is stable, turn on the feed pump P204, adjust the speed at 60rpm, and the reflux ratio is 5:1. Analyze the concentration of the overflow liquid at the top and bottom every 5 minutes. The top condensate is qualified if it does not contain ethylene glycol (tower top temperature <100℃), and the bottom overflow liquid is qualified if the ethylene glycol concentration reaches more than 98% (tower bottom temperature ≥196℃). If the concentration of the solvent recovery tower bottom is unqualified, open the bottom liquid reflux pipeline, open the air cooler E207 and valves VA242 and VA210, and return the solvent recovery tower bottom overflow liquid to the bottom liquid tank V204.

[0049] The improved process replaces the packed distillation of the crude ethanol refining tower with a sieve plate distillation tower, unifies the outer diameters of the three towers and increases the feed loop. Example 1 has the problems of large fluctuations in product purity, high energy consumption, and easily affected operational stability. The effect of the sieve plate distillation tower under the improved process of Example 2 is that the product purity is improved, the energy consumption is reduced, and the operational stability is enhanced. The comparison between the packed and sieve plate distillations under the improved process of Example 3 can clarify the differences between the two in product purity, energy consumption, and operational stability, providing a basis for process selection.

[0050] Finally, it should be noted that the drawings of the embodiments disclosed in the present invention only involve structures related to the embodiments disclosed in the present invention, and other structures can refer to common designs. In the absence of conflicts, the same embodiment and different embodiments of the present invention can be combined with each other;

[0051] Finally: The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for using a green anhydrous ethanol refining practice device capable of conducting a sieve plate and filler distillation comparison experiment, characterized in that: The specific steps include: Step 1: Turn on the device and power on the main power supply and control power supply of the unit module; Step 2: Equipment inspection and preparation, check whether the temperature and pressure display are normal, and check whether the valve status is in the closed state; Step 3: Solution preparation. After confirming that the valve status is correct, add ethanol and purified water through the VA101 feed port to prepare the ethanol solution. Add 1.5-2L of ethanol solution to the kettle of the preparation tower. The liquid level of the kettle should be higher than the upper edge of the electric heater. Step 4: After the feed is refluxed, it is extracted, the heating of the crude refining tower kettle is started, and the tower top air cooler is turned on at the same time. When steam is generated, the tower top temperature changes, and there is a liquid level in the fractionator, the full reflux operation is started. After the refining tower runs stably, the feed pump is turned on, the flow meter is turned on to start feeding, and the concentration of the tower top product is analyzed every 5 minutes. If the product concentration is unqualified, the valve is opened, the material enters the ethanol tank, and the material is re-fed. After the product concentration is qualified, the valve is closed, and the valve is opened to start extraction; Step 5: When the tower kettle overflows and the kettle liquid tank is treated, when the tower kettle liquid level reaches the overflow level, the tower kettle air cooler and the tower kettle peristaltic pump are turned on, and the wastewater tank valve is opened, and the tower kettle overflow liquid enters the wastewater tank or kettle liquid tank of the unit module; Step six: Reflux treatment of the kettle liquid tank. During the experiment, observe the kettle pressure and adjust the kettle heating power, feed rate and reflux rate in time. When the kettle overflow liquid enters the kettle liquid tank, when the kettle liquid tank level reaches 1 / 3 of the liquid level, start the feed pump. When the solvent recovery tower kettle liquid level reaches 1 / 2 of the overflow level, stop adding, turn on the electric heating, turn on the tower top air cooler, start full reflux operation, turn on the feed pump after the full reflux is stable, analyze the overflow liquid concentration of the tower top and tower kettle every 5 minutes, and judge the qualification degree of the tower top condensate and the tower kettle overflow liquid. If the solvent recovery tower kettle concentration is unqualified, open the tower kettle liquid reflux pipeline, open the air cooler and valve, and let the solvent recovery tower kettle overflow liquid return to the kettle liquid tank.

2. The method for using the green anhydrous ethanol refining practice device capable of performing sieve plate and filler distillation comparative experiments according to claim 1, characterized in that: The unit module in step one is one of a crude ethanol refining unit module and an extractive distillation unit module, and the refining tower in step three is one of a crude ethanol refining tower and an extractive distillation tower, the crude ethanol refining tower is specifically a sieve plate distillation tower, and the extractive distillation tower is specifically a packed distillation tower.

3. The method for using the green anhydrous ethanol refining practice device capable of performing sieve plate and filler distillation comparative experiments according to claim 1, characterized in that: The full reflux operation in step 4 is specifically to open the reflux pumps P102 and P202, and turn on the flow meters FI102 and FI202. The feed flow rate in step 4 is 80 ml / min, and the reflux ratio is 2:

1.

4. The method for using the green anhydrous ethanol refining practice device capable of performing sieve plate and filler distillation comparative experiments according to claim 1, characterized in that: In step six, the tower kettle pressure is observed and the tower kettle heating power, feed rate and reflux rate are adjusted in time to avoid flooding. The full reflux operation in step six is ​​specifically to open the reflux pump P206 and turn on the flow meter FI202.

5. The method for using the green anhydrous ethanol refining practice device capable of performing sieve plate and filler distillation comparative experiments according to claim 1, characterized in that: In the step 6, the standards for judging the qualification of the tower top condensate and the tower bottom overflow liquid are that the tower top condensate is qualified if it does not contain ethylene glycol, the tower top temperature is <100°C, the tower bottom overflow liquid is qualified if the ethylene glycol concentration reaches more than 98%, and the tower bottom temperature is ≥196°C.

6. The method for using the green anhydrous ethanol refining practice device capable of performing sieve plate and filler distillation comparison experiments according to claim 1, characterized in that: In step 2, the inspection of the valve status should include confirming that the valve is tightly closed and has no leakage.

7. The method for using the green anhydrous ethanol refining practice device capable of performing sieve plate and filler distillation comparison experiments according to claim 1, characterized in that: In the step 5, the speed of the tower kettle air cooler and the tower kettle peristaltic pump is adjusted between 20-60 rpm to avoid large fluctuations in the speed from affecting the experiment.

8. The method for using the green anhydrous ethanol refining practice device capable of performing sieve plate and filler distillation comparison experiments according to claim 1, characterized in that: The volume fraction of the ethanol solution prepared in step 3 is about 40%. To ensure the reliability of the experimental results, when adding ethanol and pure water to prepare the solution, it should be ensured that the solution is mixed evenly and the volume fraction is measured accurately.

9. The method for using the green anhydrous ethanol refining practice device capable of performing sieve plate and filler distillation comparison experiments according to claim 1, characterized in that: In step 4, the opening of the feed pump and the flow meter should be coordinated to ensure stable control of the feed flow rate.

10. The method for using the green anhydrous ethanol refining practice device capable of performing sieve plate and filler distillation comparison experiments according to claim 1, characterized in that: In step 6, the speed of the feed pump is adjusted to 60 rpm, and the reflux ratio is 5:1.

Images