CN108745207B - Method and device for separating medium-boiling components of complex system and returning low-boiling components to original system - Google Patents
Method and device for separating medium-boiling components of complex system and returning low-boiling components to original system Download PDFInfo
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- CN108745207B CN108745207B CN201810883116.2A CN201810883116A CN108745207B CN 108745207 B CN108745207 B CN 108745207B CN 201810883116 A CN201810883116 A CN 201810883116A CN 108745207 B CN108745207 B CN 108745207B
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0003—Condensation of vapours; Recovering volatile solvents by condensation by using heat-exchange surfaces for indirect contact between gases or vapours and the cooling medium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0033—Other features
- B01D5/0036—Multiple-effect condensation; Fractional condensation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0033—Other features
- B01D5/0051—Regulation processes; Control systems, e.g. valves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0078—Condensation of vapours; Recovering volatile solvents by condensation characterised by auxiliary systems or arrangements
- B01D5/009—Collecting, removing and/or treatment of the condensate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
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Abstract
The invention relates to a method and a device for separating middle boiling components of a complex system and returning low boiling components to an original system, which can realize the separation of middle boiling components and simultaneously return the low boiling components to the original system by adjusting a temperature control system. The separation device mainly comprises a reactor interface, a valve, a tee joint device, a temperature control system, a liquid collector and a tail gas collecting device. The separation device can respectively realize the condensation of the medium-boiling components and the condensation of the low-boiling components by adjusting the parameters of two temperature control systems, and then the medium-boiling components are separated from the system and the low-boiling components are returned to the original system through valve control. The separation device has simple principle, convenient operation and wide application range, can be manufactured into large, medium and small-sized equipment according to different reaction systems, is widely applied to various reaction systems which are not provided with rectification towers, realizes good separation of medium-boiling components, and improves the reaction efficiency.
Description
Technical Field
The invention relates to a special separation device and a method for separating specific components from a complex system, belonging to the field of chemical separation and purification.
Background
When a liquid substance is heated, molecules of the substance escape from the surface of the liquid due to molecular movement, creating a vapor pressure. As the temperature increases, the vapor pressure increases and when the vapor pressure and the atmospheric pressure or given pressure equalize, the liquid boils, at a temperature known as the boiling point of the liquid. Each pure liquid organic compound has a fixed boiling point at a certain pressure. Liquid mixtures having widely differing boiling points (e.g., differing by 30 ℃) can be separated by distillation. If the liquid with larger difference in boiling point is distilled, the liquid with lower boiling point is distilled first, and the liquid with higher boiling point is distilled later, thus the purposes of separation and purification can be achieved. However, when a mixture having a relatively close boiling point is distilled, vapors of various substances are distilled out simultaneously, so that it is difficult to achieve the separation and purification purposes, and a fractionation operation is required.
Fractionation is essentially a series of heat exchanges by passing the boiling mixture vapor through a fractionation column (commercially available fractionation columns). Because the air outside the column is cooled, the components with high boiling point in the vapor are cooled into liquid and flow back into the flask, the components with low boiling point in the rising vapor are relatively increased, when the rising vapor is encountered during the flowing back of condensate, the heat exchange is carried out between the components with high boiling point in the rising vapor, the components with low boiling point are still further rising, and the components with easy volatilization are increased, so that the procedures of vaporization, condensation, backflow and the like are repeatedly carried out in the fractionating column, and when the efficiency of the fractionating column is quite high and the operation is correct, the vapor coming out from the top of the fractionating column is close to the components with pure low boiling point, thus finally, substances with different boiling points can be separated. On the basis of fractional distillation, the mixture separation technologies of rectification, reduced pressure distillation, reduced pressure fractional distillation and the like are further developed.
Today, separation techniques such as vacuum distillation, pressure distillation, atmospheric distillation, rectification have been widely used for separation and purification of liquid phase mixtures, and various commercial applications have been realized. This is of great importance for the recycling of the components of the mixture and in terms of green chemistry.
In the prior art, both in industrial production in factories and in laboratory scientific research, the above-mentioned separation methods lead to the components with the lowest boiling points first in the separation of the mixtures. However, in many cases, only the intermediate components are separated, and the low-boiling and high-boiling components still need to be returned to the original reactor for further reaction. In industry, the intermediate components can be separated by discharging in the middle of the rectifying tower. However, it is difficult to achieve good separation of intermediate components for some reaction systems not equipped with a rectifying column. Particularly for those systems requiring the low boiling component to continue to participate in the reaction, the reaction is stopped gradually as the low boiling component is distilled off with the intermediate component. This has caused a great impediment to the expansion of the scale of industrial production and the benefits.
Therefore, designing a method and a device for separating the medium-boiling components of a complex system and returning the low-boiling components to the original system becomes a problem to be solved.
Disclosure of Invention
Aiming at the current situation and the defect that the separation of the middle components of the existing complex system is difficult, the invention provides a method and a device for separating the middle boiling components of the complex system and returning the low boiling components to the original system. By adjusting the temperature control system, separation of intermediate boiling range components can be achieved while returning low boiling components to the original system. The separation device mainly comprises a reactor interface, a valve, a tee joint, a temperature control system, a liquid collector and a tail gas collecting device. The separation device can respectively realize the condensation of the medium-boiling components and the condensation of the low-boiling components by adjusting the parameters of two temperature control systems, and then the medium-boiling components are separated from the system and the low-boiling components are returned to the original system through valve control. The separation device has simple principle, convenient operation and wide application range, can be manufactured into large, medium and small-sized equipment according to different reaction systems, is widely applied to various reaction systems which are not provided with rectification towers, realizes good separation of medium-boiling components, and improves the reaction efficiency.
The invention aims to solve the difficulty of separating the intermediate components of the existing complex system, realize good separation of the intermediate components through adjustment of parameters of a temperature control system and valve control, and simultaneously return the low-boiling components to the original system.
The technical scheme of the invention is as follows:
the device for separating the medium-boiling components of the complex system and returning the low-boiling components to the original system comprises a reactor interface, a first tee joint, a first valve, a first liquid collecting device, a second tee joint, a first temperature control system, a tail gas collecting device, a second temperature control system, a third tee joint, a second valve, a second liquid collecting device and a third valve;
the reactor interface is respectively connected with a first liquid collecting device and a second temperature control system through a first tee joint, the first liquid collecting device is respectively connected with the first temperature control system and the second temperature control system through a second tee joint, and the second temperature control system is respectively connected with the first tee joint and the second liquid collecting device through a third tee joint; the first temperature control system is also connected with the tail gas collecting device;
the first valve is arranged between the first tee joint and the first liquid collecting device, the third valve is arranged between the second tee joint and the second temperature control system, and the second valve is arranged between the third tee joint and the second liquid collecting device.
According to the present invention, preferably, the second liquid collecting device is further connected to a fifth valve. For discharging the liquid material in the second liquid collecting means.
According to the invention, preferably, a third temperature control system and a fourth valve are further arranged between the first tee joint and the third tee joint. When the temperature of the reaction system is high, and gas with the boiling point higher than that of the medium-boiling component is generated, a third temperature control system and a fourth valve are arranged for separation.
According to the invention, preferably, a fourth tee joint and a fourth temperature control system are further arranged between the third valve and the second temperature control system, and the fourth tee joint is further connected with the sixth valve, the third liquid collecting device and the seventh valve in sequence. When the reaction system simultaneously generates a plurality of medium boiling components, the temperature control system is added to separate the medium boiling components. Namely: a plurality of tees and temperature control systems may be provided between the third valve and the second temperature control system to further separate the plurality of medium boiling components.
According to the present invention, preferably, the first temperature control system, the second temperature control system, the third temperature control system and the fourth temperature control system are all systems which can be controlled by parameters, can respond to the temperature in the systems, can control the temperature change of the systems, include but are not limited to temperature measuring elements, temperature control elements and temperature sensitive elements, and can change the shape and the material according to the actual reaction system conditions;
further preferably, the first temperature control system, the second temperature control system, the third temperature control system and the fourth temperature control system are preferably one or more of common temperature control systems such as an embedded resistance wire temperature control system, a circulating water temperature control system and a circulating air temperature control system.
According to the present invention, it is preferable that the first liquid collecting device, the second liquid collecting device, and the third liquid collecting device are devices capable of collecting liquids, and include containers of various shapes and materials, and the shapes and materials can be changed according to the actual reaction system.
According to the present invention, preferably, the exhaust gas collecting device is a device which is communicated with the atmosphere, can collect the exhaust gas generated by the system and perform innocent treatment, and can perform shape and material variation according to the actual reaction system condition;
further preferably, the tail gas absorbing device is a drying head, a single-stage or multi-stage absorbing tower, a liquid system for absorbing tail gas with the characteristic of preventing liquid recharging, and the like.
According to the present invention, preferably, the reactor interface is an interface for connecting the apparatus of the present invention and the reactor, and the shape and the material may be changed according to the actual reaction system.
According to the present invention, preferably, the first valve, the second valve, the third valve, the fourth valve, the fifth valve, the sixth valve and the seventh valve are all valves for controlling fluid circulation, and the fluid may include gas or/and liquid, and may change in shape and material according to the actual reaction system.
According to the present invention, preferably, the first tee, the second tee, the third tee and the fourth tee are all devices for simultaneously connecting three parts, the inside of the devices is through, and the communication of the three parts, the communication of any two parts or the isolation of the three parts can be realized according to the control condition of the connected valve, so that the shape and the material can be changed according to the condition of an actual reaction system.
According to the present invention, the angle of the pipeline is changed according to the actual reaction system based on the structure provided by the drawings, and the scope of the present invention is also defined.
According to the invention, the method for separating the medium-boiling components of the complex system and returning the low-boiling components to the original system by adopting the device comprises the following steps:
(1) All valves in the device are closed firstly, a reactor interface is connected with a reactor before the system starts to react, and after the connection is completed, a first valve is opened, so that gas in the system sequentially passes through the first valve, a first liquid collecting device, a first temperature control system and a tail gas collecting device and is communicated with the outside atmosphere;
(2) After the reaction starts, the first temperature control system is regulated to enable the low-boiling components to generate reflux, so that loss caused by the low-boiling components collected by the tail gas collecting device is avoided, and the system is stable; the low-boiling component is directly returned to the reactor through the first liquid collecting device, the first valve and the reactor interface;
(3) Opening the third valve and the fourth valve, and closing the first valve at the same time, wherein the gas in the reaction system is communicated with the external atmosphere through the fourth valve, the third temperature control system, the second temperature control system, the third valve, the first temperature control system and the tail gas collecting device in sequence; the third temperature control system is regulated to enable components with boiling points higher than those of the medium-boiling components to flow back at the third temperature control system, and the second temperature control system is regulated to enable the medium-boiling components to flow back at the second temperature control system, so that the system is stable; the low-boiling component flows into the first liquid collecting device at this time; the medium-boiling component becomes liquid at the second temperature control system, flows to the third temperature control system to become gas again, and circularly flows in the third tee joint; components above the boiling point of the medium boiling components flow back into the reactor via a fourth valve and the reactor interface;
(4) Opening a second valve to stabilize the system; the low-boiling component flows into the first liquid collecting device at this time; the medium boiling component flows into the second liquid collecting device; components above the boiling point of the medium boiling components flow back into the reactor via a fourth valve and the reactor interface;
(5) Opening a fifth valve, wherein medium boiling components can be discharged from the second liquid collecting device through the fifth valve;
(6) Closing the fifth valve and opening the first valve; the low-boiling component in the first liquid collecting device flows back to the reactor through the first valve and the reactor interface;
(7) The steps (3) - (6) are repeated in sequence, so that the controllable separation and collection of the medium-boiling components can be realized, and the low-boiling components are returned to the original system of the reactor.
In the invention, the first temperature control system, the second temperature control system and the third temperature control system control the fluid to generate reflux by controlling the temperature. For example: in the step (2), the first temperature control system is regulated to enable the low-boiling component to generate reflux, namely: and controlling the temperature of the first temperature control system below the boiling point of the low-boiling component, so that the low-boiling component passes through the first temperature control system and then is cooled and refluxed. In the step (3), the second temperature control system is regulated to enable the medium-boiling component to generate reflux at the second temperature control system, namely: and controlling the temperature of the second temperature control system below the boiling point of the medium-boiling component, so that the medium-boiling component passes through the second temperature control system and then is cooled and refluxed. Adjusting the third temperature control system to enable components with boiling points higher than those of the medium boiling components to generate reflux at the third temperature control system, namely: the temperature of the third temperature control system is controlled to be higher than the boiling point of the medium boiling component and lower than the boiling point of the component higher than the boiling point of the medium boiling component, so that the component higher than the boiling point of the medium boiling component generates reflux at the third temperature control system, and the medium boiling component still continues to evaporate at the third temperature control system.
According to the invention, the separation effect is better when the adjacent boiling points of the low-boiling component, the medium-boiling component and the high-boiling component differ by 20 ℃ or more.
The invention is not described in detail in the prior art.
The principle and the beneficial effects of the invention are as follows:
the invention skillfully utilizes a plurality of three-way devices, a plurality of valves and a plurality of temperature control systems to realize the condensation of medium-boiling components and the condensation of low-boiling components in two areas respectively, and after two liquid collecting devices are used for collecting the two components respectively, the operation of collecting the medium-boiling components and returning the low-boiling components to the original system can be realized through the valves.
Compared with the prior art, the invention has the following advantages:
1. the low-boiling components in the system can be returned to the original system in time, so that the defects of huge device, long pipeline and high device sealing requirement caused by the existing method of firstly fractionating and then returning to the original system can be avoided, and continuous uninterrupted production can be realized;
2. the method can separate specific medium boiling components in the system according to the requirements, further, the number of temperature control systems and liquid collectors for separating the medium boiling components is increased, and the temperature control parameters are adjusted, so that the separation among various medium boiling components can be realized at the same time, and the method has the characteristics of flexibility, high efficiency and multiple purposes;
3. the principle of the invention is simple and easy to understand, the operation is convenient, and the invention is convenient for workers to learn and use; the method has wide application range, can be manufactured into equipment with various shapes, materials and scales according to different reaction systems, is widely applied to various reaction systems, realizes good separation of medium-boiling components, and improves the reaction efficiency.
Drawings
FIG. 1 is a schematic diagram of the apparatus for separating medium boiling components and returning low boiling components to the original system according to the present invention.
Fig. 2 is a schematic structural diagram of embodiment 1 of the present invention.
Fig. 3 is a schematic structural diagram of embodiment 5 of the present invention.
Fig. 4 is a schematic structural diagram of embodiment 6 of the present invention.
Wherein: 1. the reactor comprises a reactor interface, 2, a first tee joint, 3, a first valve, 4, a first liquid collecting device, 5, a second tee joint, 6, a first temperature control system, 7, a tail gas collecting device, 8, a second temperature control system, 9, a third tee joint, 10, a second valve, 11, a second liquid collecting device, 12, a third valve, 13, a third temperature control system, 14, a fourth valve, 15, a fifth valve, 16, a fourth tee joint, 17, a fourth temperature control system, 18, a sixth valve, 19, a third liquid collecting device, 20 and a seventh valve.
Detailed Description
The invention is further illustrated, but not limited, by the following figures and examples.
As shown in fig. 1, a device for separating medium-boiling components of a complex system and returning low-boiling components to an original system comprises a reactor interface 1, a first tee joint 2, a first valve 3, a first liquid collecting device 4, a second tee joint 5, a first temperature control system 6, a tail gas collecting device 7, a second temperature control system 8, a third tee joint 9, a second valve 10, a second liquid collecting device 11 and a third valve 12;
the reactor interface 1 is respectively connected with the first liquid collecting device 4 and the second temperature control system 8 through a first tee joint 2, the first liquid collecting device 4 is respectively connected with the first temperature control system 6 and the second temperature control system 8 through a second tee joint 5, and the second temperature control system 8 is respectively connected with the first tee joint 2 and the second liquid collecting device 11 through a third tee joint 9; the first temperature control system 6 is also connected with an exhaust gas collecting device 7;
a first valve 3 is arranged between the first tee joint 2 and the first liquid collecting device 4, a third valve 12 is arranged between the second tee joint 5 and the second temperature control system 8, and a second valve 10 is arranged between the third tee joint 9 and the second liquid collecting device 11. Preferably, the second liquid collecting device 11 is further connected with a fifth valve 15. Preferably, a third temperature control system 13 and a fourth valve 14 are further arranged between the first tee 2 and the third tee 9.
Example 1
As shown in fig. 2, an apparatus for separating medium boiling components of a complex system and returning low boiling components to the original system includes a reactor interface 1, a first liquid collecting device 4, a first temperature control system 6, a tail gas collecting device 7, a second temperature control system 8, a second liquid collecting device 11, and a third temperature control system 13. Wherein the first liquid collecting device 4 and the second liquid collecting device 11 are spherical containers; the first temperature control system 6 and the second temperature control system 8 are serpentine condensers, and the temperature control mode is that circulating water with specific temperature is controlled; the third temperature control system 13 is a straight condenser, and the temperature control mode is the temperature control of circulating water with specific temperature; the tail gas collecting device 7 is a spherical drying pipe filled with absorption particles;
the reactor interface 1 is respectively connected with the first liquid collecting device 4 and the third temperature control system 13 through the first tee joint 2, the first liquid collecting device 4 is respectively connected with the first temperature control system 6 and the second temperature control system 8 through the second tee joint 5, and the second temperature control system 8 is respectively connected with the third temperature control system 13 and the second liquid collecting device 11 through the third tee joint 9; the first temperature control system 6 is also connected with an exhaust gas collecting device 7;
a first valve 3 is arranged between the first tee joint 2 and the first liquid collecting device 4, a third valve 12 is arranged between the second tee joint 5 and the second temperature control system 8, a second valve 10 is arranged between the third tee joint 9 and the second liquid collecting device 11, and a fourth valve 14 is arranged between the third temperature control system 13 and the first tee joint 2;
the second liquid collecting device 15 is also connected with a fifth valve 15. For discharging the liquid material in the second liquid collecting means.
Example 2
A method for separating the medium boiling components of a complex system and returning the low boiling components to the original system using the apparatus described in example 1 comprising the steps of:
(1) All valves in the device are closed firstly, a reactor interface 1 is connected with a reactor before the system starts to react, and after the connection is completed, a first valve 3 is opened, so that gas in the system sequentially passes through the first valve 3, a first liquid collecting device 4, a first temperature control system 6 and a tail gas collecting device 7 and is communicated with the outside atmosphere;
(2) After the reaction starts and reaches stability, the first temperature control system 6 is regulated to enable the low-boiling components to generate reflux, so that the loss caused by the collection of the low-boiling components by the tail gas collection device 7 is avoided, and the system is stabilized; the low-boiling component is directly returned to the reactor through the first liquid collecting device 4, the first valve 3 and the reactor interface 1;
(3) The third valve 12 and the fourth valve 14 are opened, and the first valve 3 is closed, so that the gas in the reaction system is communicated with the external atmosphere through the fourth valve 14, the third temperature control system 13, the second temperature control system 8, the third valve 12, the first temperature control system 6 and the tail gas collecting device 7 in sequence; the third temperature control system 13 is regulated to enable components with boiling points higher than those of the medium boiling components to flow back at the third temperature control system 13, and the second temperature control system 8 is regulated to enable the medium boiling components to flow back at the second temperature control system 8, so that the system is stable; the low boiling component flows into the first liquid collecting device 4 at this time; the medium-boiling component becomes liquid at the second temperature control system 8, flows to the third temperature control system 13 and becomes gas again, and circularly flows in the third tee 9; components above the boiling point of the medium boiling components flow back into the reactor via fourth valve 14 and reactor interface 1;
(4) Opening the second valve 10 to stabilize the system; the low boiling component flows into the first liquid collecting device 4 at this time; the medium boiling components flow into the second liquid collecting device 11; components above the boiling point of the medium boiling components flow back into the reactor via fourth valve 14 and reactor interface 1;
(5) Opening the fifth valve 15, at which time medium boiling components can be discharged from the second liquid collecting device 11 via the fifth valve 15;
(6) Closing the fifth valve 15 and opening the first valve 3; the low-boiling components in the first liquid collection device 4 then flow back into the reactor via the first valve 3 and the reactor connection 1;
(7) The steps (3) - (6) are repeated in sequence, so that the controllable separation and collection of the medium-boiling components can be realized, and the low-boiling components are returned to the original system of the reactor.
Example 3
An apparatus for separating medium boiling components of a complex system and returning low boiling components to the original system, as described in example 1, except that: the first temperature control system 6 and the second temperature control system 8 are spherical condensers, and the temperature control mode is that circulating water with specific temperature is controlled; the tail gas collecting device 7 is a tail gas absorbing pipe with a liquid absorbing tank.
Example 4
An apparatus for separating medium boiling components of a complex system and returning low boiling components to the original system, as described in example 1, except that: the first temperature control system 6, the second temperature control system 8 and the third temperature control system 13 are all fractionation columns with internal filling filler and external resistance wire heating, and the tail gas collecting device 7 is a triple gas absorption tower (three absorption towers are respectively filled with solid paraffin, flaky sodium hydroxide and anhydrous calcium chloride particles).
Example 5
As shown in fig. 3, an apparatus for separating medium boiling components of a complex system and returning low boiling components to the original system is described in example 1, except that: because the temperature of the reaction system is insufficient to generate a gas higher than the boiling point of the medium boiling component, the third temperature control system 13 and the fourth valve 14 are omitted from the apparatus. The third tee 9 is directly connected with the first tee 2 by a pipeline.
Example 6
As shown in fig. 4, an apparatus for separating medium boiling components of a complex system and returning low boiling components to the original system is described in example 1, except that: because the reaction system simultaneously generates a plurality of medium boiling components, a temperature control system is added, and the separation operation is carried out on the plurality of medium boiling components. The added parts comprise a fourth temperature control system 17, a fourth tee 16, a sixth valve 18, a third liquid collecting device 19 and a seventh valve 20. Namely: a fourth tee 16 and a fourth temperature control system 17 are arranged between the third valve 12 and the second temperature control system 8, the fourth tee 16 is further connected with a sixth valve 18, a third liquid collecting device 19 and a seventh valve 20 in sequence. When the reaction system simultaneously generates a plurality of medium boiling components, a plurality of tee joints and a plurality of temperature control systems are arranged between the third valve 12 and the second temperature control system 8 so as to further separate the plurality of medium boiling components.
Test example 1
The reactor mixture contained methylene chloride (boiling point 39.75 ℃ C. As a low boiling component), ethanol (boiling point 78 ℃ C., as a medium boiling component), toluene (boiling point 110.6 ℃ C., as a high boiling component). The medium-boiling components of the above system were separated and the low-boiling components were returned to the original system using the apparatus described in example 1. The specific procedure is as in example 2. The liquid component collected in the second liquid collecting device 11 was analyzed, and the component was ethanol with a purity of 95%.
Test example 2
The reactor mixture contained diethyl ether (boiling point 34.6, low boiling point component), tetrahydrofuran (boiling point 65 ℃ C., first medium boiling point component), isopropyl alcohol (boiling point 82 ℃ C., second medium boiling point component), dimethyl sulfoxide (189 ℃ C., high boiling point component). The separation was performed using the apparatus as in example 6. The medium-boiling components of the above system were separated and the low-boiling components were returned to the original system using the apparatus described in example 1. The specific procedure is as in example 2. The liquid components collected in the second liquid collecting device 11 and the third liquid collecting device 19 are analyzed. The liquid component in the third liquid collecting device 19 was found to be tetrahydrofuran, purity 90%; the liquid component in the second liquid collecting apparatus 11 was isopropyl alcohol, and the purity was 93%.
Claims (7)
1. A method for separating middle boiling components of a complex system and returning low boiling components to an original system, comprising the steps of using a device for separating middle boiling components of the complex system and returning low boiling components to the original system, wherein the device comprises a reactor interface, a first tee joint, a first valve, a first liquid collecting device, a second tee joint, a first temperature control system, a tail gas collecting device, a second temperature control system, a third tee joint, a second valve, a second liquid collecting device and a third valve;
the reactor interface is respectively connected with a first liquid collecting device and a second temperature control system through a first tee joint, the first liquid collecting device is respectively connected with the first temperature control system and the second temperature control system through a second tee joint, and the second temperature control system is respectively connected with the first tee joint and the second liquid collecting device through a third tee joint; the first temperature control system is also connected with the tail gas collecting device;
a first valve is arranged between the first tee joint and the first liquid collecting device, a third valve is arranged between the second tee joint and the second temperature control system, and a second valve is arranged between the third tee joint and the second liquid collecting device;
the second liquid collecting device is also connected with a fifth valve, and a third temperature control system and a fourth valve are also arranged between the first tee joint and the third tee joint;
the method comprises the following steps:
(1) All valves in the device are closed firstly, a reactor interface is connected with a reactor before the system starts to react, and after the connection is completed, a first valve is opened, so that gas in the system sequentially passes through the first valve, a first liquid collecting device, a first temperature control system and a tail gas collecting device and is communicated with the outside atmosphere;
(2) After the reaction starts, the first temperature control system is regulated to enable the low-boiling components to generate reflux, so that loss caused by the low-boiling components collected by the tail gas collecting device is avoided, and the system is stable; the low-boiling component is directly returned to the reactor through the first liquid collecting device, the first valve and the reactor interface;
(3) Opening the third valve and the fourth valve, and closing the first valve at the same time, wherein the gas in the reaction system is communicated with the external atmosphere through the fourth valve, the third temperature control system, the second temperature control system, the third valve, the first temperature control system and the tail gas collecting device in sequence; the third temperature control system is regulated to enable components with boiling points higher than those of the medium-boiling components to flow back at the third temperature control system, and the second temperature control system is regulated to enable the medium-boiling components to flow back at the second temperature control system, so that the system is stable; the low-boiling component flows into the first liquid collecting device at this time; the medium-boiling component becomes liquid at the second temperature control system, flows to the third temperature control system to become gas again, and circularly flows in the third tee joint; components above the boiling point of the medium boiling components flow back into the reactor via a fourth valve and the reactor interface;
(4) Opening a second valve to stabilize the system; the low-boiling component flows into the first liquid collecting device at this time; the medium boiling component flows into the second liquid collecting device; components above the boiling point of the medium boiling components flow back into the reactor via a fourth valve and the reactor interface;
(5) Opening a fifth valve, wherein medium boiling components can be discharged from the second liquid collecting device through the fifth valve;
(6) Closing the fifth valve and opening the first valve; the low-boiling component in the first liquid collecting device flows back to the reactor through the first valve and the reactor interface;
(7) The steps (3) - (6) are repeated in sequence, so that the controllable separation and collection of the medium-boiling components can be realized, and the low-boiling components are returned to the original system of the reactor.
2. The method for separating medium boiling components and returning low boiling components to original system according to claim 1, wherein a fourth tee joint and a fourth temperature control system are further arranged between the third valve and the second temperature control system, and the fourth tee joint is further connected with a sixth valve, a third liquid collecting device and a seventh valve in sequence.
3. The method of claim 1, wherein the first temperature control system, the second temperature control system, the third temperature control system, and the fourth temperature control system are all parameter-controllable systems capable of responding to the temperature in the system and controlling the temperature change of the system.
4. The method for separating medium boiling components and returning low boiling components to original system according to claim 3, wherein the first temperature control system, the second temperature control system, the third temperature control system and the fourth temperature control system are one or more of an embedded resistance wire temperature control system, a circulating water temperature control system and a circulating air temperature control system.
5. The method for separating medium-boiling components and returning low-boiling components to a complex system according to claim 1, wherein the tail gas collecting device is a device which is communicated with the atmosphere, can collect tail gas generated by the system and is harmless to the system.
6. The method for separating medium-boiling components and returning low-boiling components to original system according to claim 5, wherein said tail gas collecting device is a drying head, a single-stage or multi-stage absorption tower, a liquid system for tail gas absorption with the feature of preventing liquid recharging.
7. The method for separating medium-boiling components and returning low-boiling components to original system according to claim 2, wherein said first tee, second tee, third tee and fourth tee are all devices for connecting three parts simultaneously, the interior of which is through and can realize communication of three parts, communication of any two parts or isolation of three parts according to the control condition of the connected valve.
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