CN109745723B - A double-column continuous feeding rectification system and control method - Google Patents
A double-column continuous feeding rectification system and control method Download PDFInfo
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Abstract
本发明提供了一种双塔连续供料精馏的控制方法及系统，包括：上料控制、初馏工序控制、输料控制以及精细精馏工序控制；控制1#精馏塔压力P1和压力差ΔP1，升温，待塔顶温度达到T1时，开启塔顶出料口控制阀，待1#精馏塔塔顶温度升高速率为ΔT1，初馏工序完成；精细精馏工序为：控制2#精馏塔塔顶塔釜压力差ΔP2，缓慢升高塔釜温度，控制升温速度ΔT2，控制塔釜温度在T2，待塔顶温度达到T3，完成精细精馏工序控制。本发明的控制方法，采用四个连续的控制步骤，保证了进料过程的连续、安全、高效，提高了精馏系统的分离提纯效率。本发明还提供了双塔连续供料精馏系统，原料配料系统合理，精馏效率高，产品纯度高。
The invention provides a control method and system for double-column continuous feeding rectification, including: feeding control, initial distillation process control, material conveying control and fine rectification process control ; The pressure difference is ΔP 1 , and the temperature rises. When the temperature at the top of the tower reaches T 1 , the control valve at the top of the tower is opened. When the temperature rise rate at the top of the 1# rectifying tower is ΔT 1 , the initial distillation process is completed; the fine rectification process is completed. It is as follows: control the pressure difference ΔP 2 of the tower top of the 2# rectification tower, slowly increase the temperature of the tower kettle, control the temperature rise rate ΔT 2 , control the temperature of the tower kettle at T 2 , and complete the fine rectification when the temperature at the top of the tower reaches T 3 . Process control. The control method of the invention adopts four continuous control steps, which ensures the continuous, safe and efficient feeding process, and improves the separation and purification efficiency of the rectification system. The invention also provides a double-column continuous feeding rectification system, the raw material batching system is reasonable, the rectification efficiency is high, and the product purity is high.
Description
Technical Field
The invention belongs to the technical field of chemical equipment and distillation, relates to a distillation control method and a system, and particularly relates to a control method and a system for double-tower continuous feed rectification.
Background
Rectification is a distillation method for separating components to obtain high-purity separated substances by utilizing different boiling points of the components in a mixture, is a liquid mixture separation operation with the widest industrial application, and is widely applied to petroleum, chemical industry, light industry, food, metallurgy and other departments.
The rectification operations are classified in different ways. According to the operation mode, the method can be divided into continuous rectification and batch rectification; according to the component number of the mixture, binary rectification and multicomponent rectification can be carried out; depending on whether or not an additive affecting vapor-liquid equilibrium is added to the mixture, ordinary rectification and special rectification (including extractive rectification, azeotropic rectification and salt-added rectification) can be used. The volatile component in the liquid phase enters the gas phase, and the non-volatile component in the gas phase is transferred into the liquid phase, so that the nearly pure volatile component can be obtained at the top of the tower, and the nearly pure non-volatile component can be obtained at the bottom of the tower. The feed liquid is added from the middle part of the tower, and the tower section above the feed inlet further thickens the volatile component in the rising steam, which is called as a rectifying section; the section of the column below the feed opening, which extracts the volatile components from the descending liquid, is referred to as the stripping section. Condensing the vapor led out from the tower top, returning a part of condensate as reflux liquid from the tower top to the rectifying tower, and obtaining the rest distillate as a tower top product. The liquid extracted from the tower bottom is partially gasified by a reboiler, the vapor rises along the tower, and the rest liquid is used as a tower bottom product. The ratio of the amount of liquid refluxed into the column at the top of the column to the amount of product at the top of the column is called the reflux ratio, and the size of the reflux ratio affects the separation effect and the energy consumption of the rectification operation. However, whether the materials of the rectifying device can be safely, efficiently and accurately fed is the key point for ensuring the smooth completion of the separation task of the rectifying device. Meanwhile, the rectification purity of the raw material of the existing rectification device is not high after rectification, and the requirement of high-purity purification cannot be met.
Chinese patent publication No. CN108191731A provides a novel butyrolactam preparation process based on biomass raw material aminobutyric acid, which can achieve a high purification rate, but the device used in the process is laboratory articles, and the process is controlled in a small-scale laboratory, and is difficult to be industrialized.
In summary, the problems of the prior art are as follows: the existing rectification system or device has unreasonable raw material batching system, low rectification efficiency and low purity; the control method of rectification can not ensure the continuity, safety and high efficiency of the feeding process and can not ensure the separation efficiency.
Disclosure of Invention
In order to overcome the defects and shortcomings, the invention provides a control method and a control system for double-tower continuous feed rectification, which aim to realize the following purposes:
(1) the control method for the double-tower continuous feed rectification adopts four continuous control steps, ensures the continuity, safety and high efficiency of the feeding process, and improves the separation and purification efficiency of the rectification system.
(2) The double-tower continuous feed rectification provided by the invention has the advantages of reasonable raw material proportioning system, high rectification efficiency and high product purity.
In order to realize the purpose of the invention, the invention adopts the following technical scheme:
a control method of double-tower continuous feed rectification comprises the following steps: feeding control, primary distillation process control, material conveying control and fine distillation process control.
The technical scheme of the invention is further improved as follows:
the control method for the double-tower continuous feed rectification comprises the following steps:
the feeding control is carried out, the raw material to be rectified enters the middle part of a No. 1 rectifying tower, and the raw material in a tower kettle reaches a liquid level L1Then, the primary distillation process is carried out;
starting a 1# rectifying tower vacuum pump, and controlling the pressure P1And pressure difference Δ P1Heating; when the tower top temperature reaches T1When the temperature of the top of the 1# rectifying tower rises sharply, a control valve of a discharge hole at the top of the tower is opened, and the temperature risesHigh rate of Δ T1After the primary distillation process is finished, feeding control is carried out;
opening a tower kettle discharge control valve at the bottom of the 1# rectifying tower, sending the primary rectifying material to the 2# rectifying tower kettle, and controlling the liquid level of the tower kettle to be L2Completing material conveying control, and entering fine rectification process control;
starting a No. 1 vacuum pump of the No. 2 rectifying tower, adjusting an emptying valve of a vacuum buffer tank of the No. 2 rectifying tower, and controlling the vacuum degree of the No. 2 rectifying tower to be P2Opening No. 2 vacuum pump of No. 2 rectifying tower, regulating evacuation valve of vacuum buffer tank, and controlling pressure difference of tower top and tower bottom to be delta P2The vacuum degree of the tower top and the tower kettle fluctuates within the range of +/-0.5 kpa, the temperature of the tower kettle of the 2# rectifying tower is slowly increased, and the temperature rising speed is controlled to be delta T2Controlling the temperature of the tower kettle at T2When the tower top temperature reaches T3And the finished product reaches the top of the tower to finish the fine rectification process control.
The feeding control is the liquid level L of the raw material to be rectified in the tower kettle1When 60% -90%, entering the initial distillation process for control.
The preliminary distillation process is controlled at a pressure P1The pressure difference is-80 kpa to-50 kpa, and the pressure difference is delta P1Is 0.5kpa to 3 kpa;
temperature T1At 60-85 deg.C, delta T1Is 3 to 5 ℃/min.
The material conveying control, L250 percent, the primary rectification material in the tower kettle of the No. 1 rectification tower is sent to the tower kettle of the No. 2 rectification tower, and the conveying speed is controlled to be 15 kg/h-25 kg/h.
Control of the Fine rectification procedure, P2Is-99 kpa to-96 kpa, delta P2Is 0.5 kpa-2 kpa; delta T2Is 2 ℃/min to 5 ℃/min; t is2At 160-220 ℃ and T3Is 120-155 ℃.
The feeding control comprises the following raw materials to be rectified: the content of butyrolactam is 80-95%, the content of water in impurities is about 5-18%, and the content of other impurities such as scrap iron and oxides is about 1-3%.
The purity of the finished product obtained by the control method of the double-tower continuous feeding rectification is more than or equal to 99.5 percent, and the water content is 0.2-0.5 percent.
The invention also provides a double-tower continuous feeding rectification system which is characterized in that,
the double-tower continuous feed rectification system comprises: the system comprises a rectifying tower, a waste liquid tank, a vacuum system, a condensing system, a heat conducting system and a finished product tank;
the top end of the rectifying tower is sequentially connected with a condensing system and a vacuum system, and the bottom end of the rectifying tower is connected with a heat conducting system;
the vacuum system, comprising: a vacuum buffer tank and a vacuum pump;
one end of the vacuum buffer tank is connected to the condensing system, and the other end opposite to the vacuum buffer tank is connected with the vacuum pump;
the rectifying tower sequentially comprises a tower kettle, a middle tower and a top tower part from bottom to top;
the rectifying tower comprises a 1# rectifying tower and a 2# rectifying tower, and a tower kettle of the 1# rectifying tower is connected with a tower middle phase of the 2# rectifying tower;
one side of the top of the 1# rectifying tower is connected with a waste liquid tank through a first pipeline, and a light component detection device is arranged on the first pipeline;
one side of the top of the 2# rectifying tower is connected with a finished product tank through a second pipeline, and a light component detection device is arranged on the second pipeline;
the top of the rectifying tower is also provided with a sight glass which is a glass sight glass and is used for observing the distillation reflux effect;
the heat conduction system is directly connected to the tower kettle of the rectifying tower; a pressure and liquid level detection device is arranged on the tower kettle;
a first cooling device and a second cooling device are arranged at the top of the 2# rectifying tower, the first cooling device is horizontally arranged, and the second cooling device is vertically arranged in the 2# rectifying tower;
a feeding motor is also arranged between the raw material tank and the No. 1 rectifying tower; and a feeding motor is also arranged between the No. 1 rectifying tower and the No. 2 rectifying tower.
The invention has the following beneficial effects:
(1) according to the control method for the double-tower continuous feed rectification, four continuous control steps are adopted, so that the continuity, safety and high efficiency of the feeding process are ensured, the separation and purification efficiency of a rectification system is improved, and the product purity is improved; taking butyrolactam as an example, the purity of the product reaches over 99.5 percent, and the water content of impurities is 0.2 to 0.5 percent.
(2) The double-tower continuous feeding rectification system has the advantages that the raw material proportioning system is reasonable, the rectification can be more sufficient by adopting the arrangement of the two rectification towers, the rectification process of the raw material is kept to be continuously and stably output by adopting a continuous feeding method, the rectification efficiency is improved, the evaporation process in the rectification towers can be accelerated by the heat conduction system, the pressure and the temperature can be adjusted for different liquids to be rectified, the applicability is strong, and the double-tower continuous feeding rectification system is suitable for butyrolactam, caprolactam and other materials with the boiling point below 400 ℃.
For a further understanding of the present invention, reference should be made to the following detailed description taken in conjunction with the accompanying drawings.
Drawings
FIG. 1 is a schematic diagram of a double column continuous feed rectification system of the present invention;
reference numbers in the figures: 001-raw material tank, 002-feeding motor, 003-1# rectifying tower, vacuum buffer tank of 004-1# rectifying tower, 005-waste liquid tank, heat conducting system of 006-1# rectifying tower, 007-condensing system, vacuum pump of 008-1# rectifying tower, 009-feeding motor, 010-2# rectifying tower, vacuum buffer tank of 011-2# rectifying tower, 012-finished product tank, vacuum pump of 013-2# rectifying tower and heat conducting system of 014-2# rectifying tower.
FIG. 2 is an enlarged view of the identification of each component of the 2# rectifying tower;
reference numbers in the figures: 110-sight glass, 111-top of tower, 112-middle of tower, 113-bottom of tower, 114-light component detecting device, 130-pressure, liquid level detecting device, first cooling device 151 and second cooling device 152.
FIG. 3 is an enlarged view of the identification of each component of the No. 1 rectifying tower;
reference numbers in the figures: 110-sight glass, 111-top of the tower, 112-middle of the tower, 113-bottom of the tower, 114-light component detection device, 130-pressure and liquid level detection device.
Detailed Description
For the purpose of enhancing the understanding of the present invention, the present invention will be further described in detail with reference to the following examples and the accompanying drawings, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
Control method for double-tower continuous feed rectification
The invention relates to a control method of double-tower continuous feed rectification, which comprises the following steps:
the method comprises the following steps: feeding control
The raw materials that the feedstock pump will wait to rectify carry 1# rectifying column middle part through the head tank, wait to rectify the raw materials and include: the content of butyrolactam is 80-95%, the content of water in impurities is about 5-18%, and the content of other impurities such as scrap iron and oxides is about 1-3%; the raw materials are gradually filled in a rectifying layer in the tower to a tower kettle, the liquid level of the tower kettle is controlled to be 60-90%, and the raw materials enter the tower kettle of the No. 1 rectifying tower after passing through the filler of the rectifying layer in the tower.
The rectifying tower is divided into a tower kettle, a tower neutralizing tower top and a tower kettle according to functions: heating to generate steam; in the tower: starting feeding and filling; the light and heavy components are further separated except for the discharge at the tower top; the rectification layer is distributed in the tower and the top of the tower, and can primarily separate light and heavy components.
Compare in tower cauldron and top of the tower feeding, the feeding can make the material dispersion that gets into the rectifying column in the tower, when tower cauldron temperature risees, the material steam of tower cauldron meets with rectification layer material, accelerate the circulation of material, the rectification is accomplished more than 8 hours to tower cauldron feeding, accomplish within 5 hours in the rectification in the tower, the serialization production of being convenient for, the efficiency of rectification is improved, the material circulation can be accelerated in the top of the tower feeding, but easily cause the top of the tower steam volume to increase, arouse the top of the tower to explode and boil, bring the difficulty for serialization rectification process control.
All be equipped with first rectifying layer and second rectifying layer in 1# rectifying column and the 2# rectifying column, first rectifying layer and second rectifying layer are by supreme arranging down.
The 1# rectifying tower is internally provided with a first rectifying layer and a second rectifying layer, the first rectifying layer is provided with two layers, and the second rectifying layer is a layer;
a first rectifying layer and a second rectifying layer are arranged in the 2# rectifying tower, the first rectifying layer is provided with two layers, and the second rectifying layer is provided with two layers. The second rectifying layer of the 2# rectifying tower is arranged into two layers, so that the light and heavy component separation effect can be ensured.
Step two: preliminary distillation process control
Starting a vacuum pump of the 1# rectifying tower, controlling the pressure range of the 1# rectifying tower to be-80 kpa to-50 kpa by adjusting an evacuation valve, and adjusting the pressure difference of a tower top kettle to be 0.5kpa to 3 kpa;
meanwhile, the temperature is slowly raised through a heat conduction system, the temperature rise speed is controlled to be 3-5 ℃/min,
controlling the temperature of a tower kettle to be 150-240 ℃, when the temperature in the tower rises and the temperature of the tower top reaches 60-85 ℃, observing the generation of light components on a sight glass of the tower top, starting a control valve of a discharge hole at the tower top, maintaining the process stable, namely, the temperature of the tower kettle fluctuates at +/-3 ℃ of a set temperature, the temperature of the tower top fluctuates at +/-2 ℃, and when the temperature of the tower top of the 1# rectifying tower sharply rises, namely the temperature of the tower top rises at a speed of more than 2 ℃/min and no obvious fall-back occurs within 10min, finishing the primary rectification of the 1# rectifying tower.
After the rectification of the No. 1 rectifying tower, light components such as steam and the like pass through the top of the No. 1 rectifying tower, are cooled by a cooling system and enter a waste liquid tank, and the waste liquid tank is connected with a vacuum pump pipeline through a pipeline, so that the pressure balance in the waste liquid tank and the rectifying tower can be maintained; and refluxing the primary rectification material to a discharge hole at the bottom of the 1# rectification tower.
In the process, when the liquid level volume of the tower kettle is lower than 25%, the feeding motor is controlled to slowly convey the raw material to be rectified into the tower kettle, the feeding speed of the feeding motor is controlled to be 5 kg/h-8 kg/h, the rectification stability of the whole 1# rectification tower is ensured, and the process has no obvious change.
Step three: material delivery control
Opening a tower kettle discharge control valve at the bottom of the 1# rectifying tower, connecting the bottom of the 1# rectifying tower with the middle of the 2# rectifying tower through a pipeline, conveying the primary rectified material of the tower kettle of the 1# rectifying tower to the tower kettle of the 2# rectifying tower through a feeding motor, controlling the conveying speed at 15 kg/h-25 kg/h, controlling the liquid level of the tower kettle to be more than 50%, and finishing material conveying.
The middle part of the present invention refers to the upper part of the first rectifying layer.
The good packing of raw materials of preliminary distillation dewatering is guaranteed at the rectification layer in middle part feeding, both can improve rectification efficiency, is convenient for realize serialization rectification again, and 2# rectifying column second rectification layer is equipped with two-layerly simultaneously, ensures that the finished product after 2# rectifying column rectification reaches the purity requirement.
Step four: fine rectification process control
Firstly, starting a No. 1 vacuum pump of a No. 2 rectifying tower, adjusting an evacuation valve of a vacuum buffer tank of the No. 2 rectifying tower, controlling the vacuum degree of the No. 2 rectifying tower to be-99 kpa to-96 kpa, starting the No. 2 vacuum pump of the No. 2 rectifying tower, adjusting the evacuation valve of the vacuum buffer tank, controlling the pressure difference of a tower top kettle to be 0.5kpa to 2kpa, controlling the vacuum degrees of the tower top and the tower kettle to fluctuate within the range of +/-0.5 kpa, slowly raising the temperature of the tower top kettle of the No. 2 rectifying tower, controlling the temperature raising speed to be 2 ℃/min to 5 ℃/min, controlling the temperature of the tower kettle to be 160 ℃ -220 ℃, and when the temperature of the tower top reaches 120 ℃ -155 ℃, and enabling a refined finished product to reach the tower top.
In order to guarantee the condensation effect, the top of the 2# rectifying tower is provided with two cooling devices, namely a first cooling device and a second cooling device, the first cooling device is horizontally arranged, and the second cooling device is vertically arranged in the 2# rectifying tower. The tower bottom steam reaches the tower top, condenses into liquid under the effect of second cooling device, and the steam loss of part abundant condensation is to first cooling device, cools off once more, and two sets of cooling device have accelerated the rate of condensation, have guaranteed the condensation effect again.
And (3) after the refined and purified finished product reaches the top of the tower, the finished product is observed to be generated by a sight glass, namely, liquid drops can be found through the sight glass to drop, a control valve of a discharge port at the top of the tower is opened, the process is maintained to be stable, when the temperature of the top of the 2# rectifying tower rises sharply, namely, the top of the tower rises at a speed of more than 2 ℃/min and no obvious drop occurs within 10min, the refined rectification is completed, the finished product is obtained, and the finished product is collected in a.
The purity of the obtained finished product is more than 99.5%, and the water content is about 0.2-0.5%.
The method is mainly used for rectifying butyrolactams, but not limited to butyrolactams, such as caprolactam, and the like, and can also be used for other materials with the boiling point below 400 ℃.
Example 1 control method of double-column continuous feed rectification
The embodiment provides a rectification and purification process of a chemical raw material butyrolactam, which comprises the following steps:
the method comprises the following steps: feeding control
Delivering butyrolactam to be rectified to a No. 1 rectifying tower, wherein the purity is 83 percent, the water content is 14 percent, the content of other impurities is 3 percent, and controlling the liquid level of a tower kettle to 90 percent.
Step two: preliminary distillation process control
Starting a vacuum pump, adjusting an emptying valve of a vacuum buffer tank, controlling the vacuum degree of a tower kettle to be minus 80 +/-1 kpa, controlling the temperature of the tower kettle to be 160 +/-2 ℃, keeping the pressure difference of the tower kettle at the top of the tower to be 0.5 +/-0.1 kpa, observing the generation of light components from a sight glass when the temperature of the tower top reaches about 60 +/-1 ℃, and finishing the preliminary rectification when the temperature of a discharge hole rises.
Step three: material delivery control
Conveying the primary rectification liquid to a tower kettle of a 2# rectification tower, and specifically: opening a tower kettle discharge control valve at the bottom of the 1# rectifying tower, connecting the bottom of the 1# rectifying tower with the middle of the 2# rectifying tower through a pipeline, conveying the primary rectified material of the tower kettle of the 1# rectifying tower to the tower kettle of the 2# rectifying tower through a feeding motor, controlling the conveying speed at 15 kg/h-25 kg/h, controlling the liquid level of the tower kettle to be more than 50%, and finishing material conveying.
Step four: fine rectification process control
Starting a vacuum pump of a 2# rectifying tower, adjusting a vacuum buffer tank to ensure that the vacuum degree of a tower kettle is-99 +/-1 kpa, controlling the temperature of the tower kettle to be 160 +/-2 ℃, keeping the pressure difference of the tower kettle at the top of the tower to be 0.5 +/-0.1 kpa, observing that a finished product is output at the top of the tower when the temperature of the top of the tower reaches 120 +/-1 ℃, starting a discharge control valve, finishing the rectification when the temperature of a discharge port at the top of the tower rises to obtain a finished product, and analyzing and detecting that the purity is 99.6%, the moisture content is 0.3% and other impurities are 0.1%.
Example 2 control method of double-tower continuous feed rectification
The embodiment provides a rectification and purification process of a chemical raw material butyrolactam, which comprises the following steps:
the method comprises the following steps: feeding control
Delivering butyrolactam to be rectified to a No. 1 rectifying tower, wherein the purity is 90%, the water content is 8%, the content of other impurities is 2%, and controlling the liquid level of a tower kettle to 80%.
Step two: preliminary distillation process control
Starting a vacuum pump, adjusting an emptying valve of a vacuum buffer tank, controlling the vacuum degree of a tower kettle to be minus 70 +/-1.5 kpa, controlling the temperature of the tower kettle to be 200 +/-3 ℃, keeping the pressure difference of the tower kettle at the top of the tower to be 1.5 +/-0.2 kpa, observing the generation of light components from a sight glass when the temperature of the top of the tower reaches about 70 +/-1 ℃, and finishing the primary rectification when the temperature of a discharge hole rises.
Step three: material delivery control
Conveying the primary rectification liquid to a tower kettle of a 2# rectification tower, and specifically: opening a tower kettle discharge control valve at the bottom of the 1# rectifying tower, connecting the bottom of the 1# rectifying tower with the middle of the 2# rectifying tower through a pipeline, conveying the primary rectified material of the tower kettle of the 1# rectifying tower to the tower kettle of the 2# rectifying tower through a feeding motor, controlling the conveying speed at 15 kg/h-25 kg/h, controlling the liquid level of the tower kettle to be more than 50%, and finishing material conveying.
Step four: fine rectification process control
Starting a vacuum pump of a 2# rectifying tower, adjusting a vacuum buffer tank to ensure that the vacuum degree of a tower kettle is-97 +/-1 kpa, controlling the temperature of the tower kettle to be 180 +/-3 ℃, keeping the pressure difference of the tower kettle at the top of the tower to be 2 +/-0.2 kpa, observing that a finished product is output at the top of the tower when the temperature of the top of the tower reaches 140 +/-1 ℃, starting a discharge control valve, finishing rectification when the temperature of a discharge port at the top of the tower rises to obtain a finished product, and analyzing and detecting that the purity is 99.5% and the moisture content is 0.4%.
Example 3 control method of double-column continuous feed rectification
The embodiment provides a rectification and purification process of a chemical raw material butyrolactam, which comprises the following steps:
the method comprises the following steps: feeding control
Delivering butyrolactam to be rectified to a No. 1 rectifying tower, wherein the purity is 95 percent, the water content is 4 percent, the content of other impurities is 1 percent, and controlling the liquid level of a tower kettle to 60 percent.
Step two: preliminary distillation process control
Starting a vacuum pump, adjusting an emptying valve of a vacuum buffer tank, controlling the vacuum degree of a tower kettle to be minus 50 +/-1 kpa, controlling the temperature of the tower kettle to be 240 +/-2 ℃, keeping the pressure difference of the tower kettle at the top of the tower to be 1 +/-0.2 kpa, observing the generation of light components from a sight glass when the temperature of the tower top reaches about 85 +/-1 ℃, and finishing the preliminary rectification when the temperature of a discharge hole rises.
Step three: material delivery control
Conveying the primary rectification liquid to a tower kettle of a 2# rectification tower, and specifically: opening a tower kettle discharge control valve at the bottom of the 1# rectifying tower, connecting the bottom of the 1# rectifying tower with the middle of the 2# rectifying tower through a pipeline, conveying the primary rectified material of the tower kettle of the 1# rectifying tower to the tower kettle of the 2# rectifying tower through a feeding motor, controlling the conveying speed at 15 kg/h-25 kg/h, controlling the liquid level of the tower kettle to be more than 50%, and finishing material conveying.
Step four: fine rectification process control
Starting a vacuum pump of a 2# rectifying tower, adjusting a vacuum buffer tank to ensure that the vacuum degree of a tower kettle is-95 +/-1 kpa, controlling the temperature of the tower kettle to be 220 +/-2 ℃, keeping the pressure difference of the tower kettle at the top of the tower to be 1 +/-0.2 kpa, observing that a finished product is output at the top of the tower when the temperature of the top of the tower reaches 155 +/-1 ℃, starting a discharge control valve, finishing rectification when the temperature of a discharge port at the top of the tower rises to obtain a finished product, and analyzing and detecting that the purity is 99.8% and the moisture content is 0.15%.
Example 4 double column continuous feed rectification
As shown in fig. 1 to 3, the present invention provides a double-column continuous feed rectification system, comprising: the system comprises a rectifying tower (003, 010), a waste liquid tank 005, a vacuum system (004, 008), a condensation system 007, a heat conduction system 006, 014 and a finished product tank 012; the top end of the rectifying tower is sequentially connected with a condensing system 007 and a vacuum system (004 and 008), and the bottom end of the rectifying tower is connected with heat conducting systems 006 and 014; the heat conducting system 006, 014 is directly connected to a column still 113113 of the rectifying column (003, 010), the vacuum system (004, 008) includes: vacuum buffer tanks 004, 011 and vacuum pumps 008, 012; one end of each vacuum buffer tank 004, 011 is connected to the condensing system 007, the other end opposite to the vacuum buffer tank is connected to the vacuum pump 008, 012, the bottom of each vacuum buffer tank 004, 011 is provided with a control valve, and the vacuum buffer tanks 004, 011 ensure that the pressure of the whole system is in a normal state; the rectifying tower (003, 010) is divided into a tower kettle 113, a middle tower 112 and a tower top 111 from bottom to top according to functions, wherein the tower kettle 113: heating to generate steam; 112 in the tower: starting feeding and filling; the tower top 111 further realizes the separation of light and heavy components besides discharging; the rectification layers are distributed in the tower 112 and the tower top 111, so that the light and heavy components can be primarily separated; preferably, a pressure and liquid level detection device is also arranged on the tower kettle 113; the rectifying tower comprises a 1# rectifying tower and a 2# rectifying tower, and a tower kettle 113 of the 1# rectifying tower is connected with a tower middle 112 of the 2# rectifying tower; all be equipped with first rectifying layer and second rectifying layer in 1# rectifying column and the 2# rectifying column, first rectifying layer and second rectifying layer are by supreme arranging down. The 1# rectifying tower is internally provided with a first rectifying layer and a second rectifying layer, the first rectifying layer is provided with two layers, and the second rectifying layer is a layer; a first rectifying layer and a second rectifying layer are arranged in the 2# rectifying tower, the first rectifying layer is provided with two layers, and the second rectifying layer is provided with two layers. The second rectifying layer of the 2# rectifying tower is arranged into two layers, so that the light and heavy component separation effect can be ensured.
The tower top 111 of the 1# rectifying tower is connected with a waste liquid tank 005; the top 111 of the 2# rectifying tower is connected with a finished product tank 012, and the middle 112 part of the 1# rectifying tower is also connected with a raw material tank. The head tank with still be equipped with the feeding motor between the 1# rectifying column, the 1# rectifying column with still be equipped with pay-off motor 009 between the 2# rectifying column, can control the speed of feeding according to the technological requirement, can be through adjusting the frequency control input speed of feeding motor 002, according to the demand feeding.
Furthermore, one side of the top 111 of the 1# rectifying tower is connected with a waste liquid tank 005 through a first pipeline, waste liquids of the 1# rectifying tower 003 and the 2# rectifying tower 010 are recovered and are uniformly conveyed to a raw material tank according to a detection standard, and recycling can be realized; a light component detection device is arranged on the first pipeline; one side of the top 111 of the 2# rectifying tower is connected with a finished product tank 012 through a second pipeline, and the second pipeline is provided with a light component detection device.
Further, the top 111 of the rectifying tower is further provided with a viewing mirror 110, and the viewing mirror 110 is a glass viewing mirror 110 and is used for observing the distillation reflux effect.
Preferably, the 2# rectifying tower top 111 is provided with a first cooling device 151 and a second cooling device 152, the first cooling device 151 is horizontally arranged, and the second cooling device 152 is vertically arranged in the 2# rectifying tower. Furthermore, the 2# rectifying tower is provided with two vacuum pumps, and the work load of the two vacuum pumps is more than 10 times of that of the 1# rectifying tower vacuum pump.
Specifically, the working process of the double-tower continuous feed rectification system is as follows: the method comprises the steps that a to-be-rectified liquid in a raw material tank 001 enters the middle of a 1# rectifying tower 003 through a feeding motor 002, the to-be-rectified liquid gradually fills the rectifying middle and then reaches the tower kettle of the 1# rectifying tower 003, the raw material gradually enters the tower through the tower kettle after the rectification starts and the tower top, the liquid level of the 1# rectifying tower is reduced along with the extension of the rectification time, online material supplement is carried out by controlling the power of a delivery pump, the to-be-rectified liquid enters the middle of a 2# rectifying tower 010 through the bottom of the 1# rectifying tower 003 after the 1# rectifying tower 003 finishes full reflux, and the to-be-rectified liquid falls into the tower kettle of the.
Two tower continuous feed rectifying system include 1# rectifying column 003 and 2# rectifying column 010, 1# rectifying column 003 and 2# rectifying column 010 upper end all link to each other with vacuum buffer tank 004 and vacuum buffer tank 011 respectively via condensing system 007, 1# rectifying column 003 one side is passed through the pipeline, feeding motor 002 links to each other with head tank 001, vacuum tank 004 top links to each other with vacuum pump 008, the bottom is connected with waste liquid jar 005, waste liquid jar 005 is connected with 1# rectifying column 003 top of the tower discharge gate simultaneously. The bottom of 1# rectifying column 003 and 2# rectifying column 010 all links to each other with conduction oil system 006, 014, and 1# rectifying column 003 and 2# rectifying column 010 light component rectification thing link to each other with the finished product jar via the pipeline from the top of the tower.
The bottom of the 1# rectifying tower 003 is connected with the 2# rectifying tower 010 through a pipeline valve and a feeding motor 009, the top of the 2# rectifying tower 010 is connected with a cooling device (151, 152), namely, the top of the 2# rectifying tower is provided with a first cooling device 151 and a second cooling device 152, the first cooling device 151 is horizontally arranged, the second cooling device 152 is vertically arranged in the 2# rectifying tower 010 to form a condensing system 007, the top of the tower is connected with a vacuum buffer tank 011 of the 2# rectifying tower through a pipeline, and a tank body of the vacuum buffer tank (011, 006) is provided with an emptying valve; the finished product tank 012 is respectively connected with a vacuum buffer tank 011, a 2# rectifying tower vacuum pump 013 and a 2# rectifying tower top material outlet through pipelines,
the drain outlet of the tower kettle of the No. 1 rectifying tower 003 is connected with the waste liquid tank 005, the drain outlet in the tower of the No. 2 rectifying tower 010 can also be connected with the waste liquid tank 005, the waste liquid of the No. 1 rectifying tower 003 and the No. 2 rectifying tower 010 is recycled, and is uniformly conveyed to a raw material tank according to the detection standard, so that the recycling can be realized; the environment protection and economy are ensured, and meanwhile, the residual liquid discharged by sewage disposal is uniformly stored and treated after being treated for multiple times, so that the environment protection and no pollution are ensured, and the resource utilization efficiency is improved.
Liquid level and pressure detection devices are arranged in the tower kettles of the No. 1 rectifying tower 003 and the No. 2 rectifying tower 010 respectively. Glass sight glass devices are arranged at the tops of the 1# rectifying tower 003 and the 2# rectifying tower 010, so that the distillation reflux effect can be observed through sight glasses while the pressure of the top and the bottom of the rectifying tower is ensured; a light component detection device is arranged in the pipeline connection. A light component receiving tank of the No. 1 rectifying tower 003, namely a waste liquid tank 005 and a light component receiving tank of the No. 2 rectifying tower 010, namely a finished product tank 012 is not only connected with the top of the tower, but also respectively connected with a vacuum pump 008 and a vacuum pump 013; the bottom of the 1# rectifying tower is provided with a discharge valve, and the raw materials are discharged through the bottom discharge valve after the 1# rectifying tower passes through the whole total reflux process, utilize the feeding motor between 1# rectifying tower and the 2# rectifying tower, get into the 2# rectifying tower, realize the effect of secondary rectification through controlling technological parameters. The double-tower continuous feeding rectification system can be used as a negative pressure distillation device for purifying the butyrolactam which is a liquefied product of aminobutyric acid.
Unless otherwise stated, the percentages used in the present invention are percentages by weight, and the proportions described in the present invention are proportions by mass.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (1)
1. The control method is characterized in that the control method carries out feeding control, preliminary distillation process control, material conveying control and fine distillation process control on a double-tower continuous feeding and rectifying system;
the system for dual column continuous feed rectification comprising: the system comprises a rectifying tower, a waste liquid tank, a vacuum system, a condensing system, a heat conducting system and a finished product tank;
the top end of the rectifying tower is sequentially connected with a condensing system and a vacuum system, and the bottom end of the rectifying tower is connected with a heat conducting system;
the vacuum system, comprising: a vacuum buffer tank and a vacuum pump;
one end of the vacuum buffer tank is connected to the condensing system, and the other end opposite to the vacuum buffer tank is connected with the vacuum pump;
the rectifying tower sequentially comprises a tower kettle, a middle tower and a top tower part from bottom to top;
the rectifying tower comprises a 1# rectifying tower and a 2# rectifying tower, and a tower kettle of the 1# rectifying tower is connected with a tower middle phase of the 2# rectifying tower;
one side of the top of the 1# rectifying tower is connected with a waste liquid tank through a first pipeline, and a light component detection device is arranged on the first pipeline;
one side of the top of the 2# rectifying tower is connected with a finished product tank through a second pipeline, and a light component detection device is arranged on the second pipeline;
the top of the rectifying tower is also provided with a sight glass which is a glass sight glass and is used for observing the distillation reflux effect;
the heat conduction system is directly connected to the tower kettle of the rectifying tower; a pressure and liquid level detection device is arranged on the tower kettle;
a first cooling device and a second cooling device are arranged at the top of the 2# rectifying tower, the first cooling device is horizontally arranged, and the second cooling device is vertically arranged in the 2# rectifying tower;
a feeding motor is also arranged between the raw material tank and the No. 1 rectifying tower; a feeding motor is further arranged between the No. 1 rectifying tower and the No. 2 rectifying tower;
the feeding control is that the raw material to be rectified enters the middle part of a No. 1 rectifying tower, and the raw material enters the primary distillation process control when the liquid level L1 of the raw material in the tower kettle is 60-90%;
the feeding control comprises the following raw materials to be rectified: the content of butyrolactam is 80% -95%, the content of water is 5% -18%, and the content of other impurities is 1% -3%;
controlling the primary distillation process, starting a No. 1 rectifying tower vacuum pump, controlling the pressure P1 and the pressure difference delta P1, and heating; when the temperature at the top of the tower reaches T1, opening a control valve of a discharge hole at the top of the tower, when the temperature at the top of the 1# rectifying tower rises and the rising rate is delta T1, finishing the primary distillation process, and entering material conveying control;
the primary distillation process is controlled, the pressure P1 is-80 kpa to-50 kpa, the pressure difference delta P1 is 0.5kpa-3kpa, the temperature T1 is 60 ℃ to 85 ℃, and the delta T1 is 3 ℃/min to 5 ℃/min;
the material conveying control is to open a tower kettle discharge control valve at the bottom of the 1# rectifying tower, send the primary rectifying material prepared in the primary distillation process to the tower kettle of the 2# rectifying tower, control the liquid level of the tower kettle to be more than L2, finish the material conveying control and enter the fine rectification process control;
the material conveying is controlled, the L2 is 50%, the primary rectification material at the tower kettle of the No. 1 rectification tower is conveyed to the tower kettle of the No. 2 rectification tower, and the conveying speed is controlled to be 15 kg/h-25 kg/h;
controlling the fine rectification process, namely starting a No. 1 vacuum pump of a No. 2 rectification tower, adjusting an evacuation valve of a vacuum buffer tank of the No. 2 rectification tower, controlling the vacuum degree of the No. 2 rectification tower to be P2, starting a No. 2 vacuum pump of the No. 2 rectification tower, adjusting an evacuation valve of the vacuum buffer tank, controlling the pressure difference of a tower top kettle to be delta P2, controlling the vacuum degrees of the tower top and the tower kettle to fluctuate within the range of +/-0.5 kpa, slowly increasing the temperature of the tower top kettle of the No. 2 rectification tower, controlling the temperature rise speed to be delta T2, controlling the temperature of the tower kettle to be T2, and finishing the control of the fine rectification process when the temperature of the tower top reaches T3 and a finished;
controlling the fine rectification process, wherein P2 is-99 kpa to-96 kpa, and delta P2 is 0.5kpa to 2 kpa; the delta T2 is 2-5 ℃/min; t2 is 160-220 ℃, and T3 is 120-155 ℃;
the purity of the finished product obtained by the control method of the double-tower continuous feeding rectification is more than or equal to 99.5 percent, and the water content is 0.2-0.5 percent.
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| CN113117364A (en) * | 2021-05-25 | 2021-07-16 | 杭州广泰环保技术有限公司 | NMP recovery coupling rectification system and rectification control process thereof |
| CN114253130B (en) * | 2021-12-21 | 2022-12-16 | 南通大学 | An active disturbance rejection control structure and control method for a binary distillation process |
| CN116147286B (en) * | 2022-12-05 | 2024-01-12 | 广钢气体(广州)有限公司 | High-purity oxygen rectification control method and device thereof |
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