CN113274764A - Liquid phase adsorption separation system and temperature control process method thereof - Google Patents
Liquid phase adsorption separation system and temperature control process method thereof Download PDFInfo
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- CN113274764A CN113274764A CN202110679320.4A CN202110679320A CN113274764A CN 113274764 A CN113274764 A CN 113274764A CN 202110679320 A CN202110679320 A CN 202110679320A CN 113274764 A CN113274764 A CN 113274764A
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- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/16—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the fluid carrier
- B01D15/161—Temperature conditioning
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Abstract
The invention discloses a liquid phase adsorption separation system and a temperature control process method thereof, belonging to the technical field of adsorption separation. The liquid phase adsorption separation system comprises a preheating system, a constant temperature system, a heat dissipation system, an adsorption separation tower, a high-pressure constant flow pump, a sensing device and related pipeline valves, and is simple in structure, mature in technology, high in heat transfer efficiency, stable in temperature, long in service life and low in overall equipment maintenance cost. Meanwhile, a temperature control process method of the liquid phase adsorption separation system is also provided, the control precision of the chromatographic column temperature is further improved, the method has better applicability and practicability, is suitable for the existing liquid phase adsorption separation technologies such as fixed column type and rotary valve type, and can meet the requirement of precision in industrial amplification production.
Description
Technical Field
The invention belongs to the technical field of liquid phase adsorption separation, and particularly relates to a liquid phase adsorption separation system and a temperature control process method.
Background
In recent years, the corresponding disadvantages of the conventional refining and purifying process are gradually shown, for example, more trays and longer distillation range are needed, the liquid phase adsorption separation is used as a new replaceable method, and the method is gradually applied to the industrial field, especially for isomerides and near-boiling compounds, the liquid phase adsorption separation becomes a high-efficiency separation means, especially in various fields of petrochemical production, such as separation of aromatic isomers, preferably toluene, xylene and ethylbenzene mixed industrial raw materials, separation of diamine isomers, preferably 1, 5-pentanediamine industrial raw materials, separation of cresol isomers, preferably m-p-cresol industrial raw materials, separation of polyol isomers, preferably 2, 3-butanediol, 1, 2-pentanediol, 1, 2-hexanediol and other industrial raw materials, so as to extract target products, Concentration and separation, and at the same time, the corresponding liquid phase adsorption separation equipment becomes the most critical technology, and is especially important in the process of mass production.
In the existing literature, regarding a liquid phase adsorption separation system and a temperature control process, for example, patents CN108226364A and JP4110142B2, mainly stay on the traditional liquid chromatography apparatus, and are difficult to apply to the field of industrial production amplification requirements. Patent CN 112245971a proposes a liquid phase adsorption separation system, but it is not mentioned here whether the circulation pump can operate for a long time in a high temperature medium environment, and it is known from the market that the circulation pump capable of withstanding high temperature is few, and expensive, and the cost is increased virtually. Correspondingly provide a constant temperature system in patent CN2918042Y, CN208878618U, increased mechanical stirring in the oil groove, to a certain extent, can realize the inside convection heat transfer of oil tank, but the motor direct drive's of universal adoption installation on the oil tank shell mode, on the one hand, the oil tank temperature risees, and the motor coil is heated the conduction and heaies up, and coil self is generated heat when on the other hand motor operation, must influence its life, has also increased the potential safety hazard simultaneously.
It is known that the current adsorption separation equipment can be roughly classified into sequential type and rotary valve type simulated moving bed technology in structure, wherein the temperature control of the chromatographic column of the core component directly affects the analysis precision and accuracy of the sample, therefore, the structural design and temperature control effect of the column temperature system and the temperature control process method have significant influence on the improvement of the precision of the qualitative and quantitative results.
Therefore, the development of a constant temperature system and a temperature control process method which are suitable for a mainstream fixed column type, a rotary valve type and other liquid phase adsorption separation simulated moving bed has great significance.
Disclosure of Invention
Aiming at the technical problems, the liquid phase adsorption separation system comprises components such as preheating, constant temperature and heat dissipation, liquid is used as a heat conducting medium in the preheating link, a traditional coaxial driving mode is replaced by magnetic transmission based on a brand-new magnetic coupling principle, a convection stirring mode of a unique splitter plate is matched, the preheating of raw materials and a desorbent is completed, then a radiation heat supply mode is adopted in the multi-module constant temperature link, the temperature of a chromatographic column is guaranteed to be constant, and finally the heat dissipation link protects a circulating pump from being damaged easily due to overhigh medium temperature and long-time operation. The technical problem is solved, and a temperature control process method is also provided, so that the control precision of the chromatographic column temperature is further improved.
The technical scheme of the invention is as follows:
on one hand, the invention provides a liquid phase adsorption separation system, which comprises a preheating system, a constant temperature system, a heat dissipation system, an adsorption separation tower, a high-pressure constant flow pump, a sensing device, a pipeline and a valve piece, wherein the preheating system is connected with the constant temperature system; the preheating system is designed in a cylindrical structure and comprises a main body, a stirring system, a heating pipe, a flow distribution plate, a temperature sensor I and a coil pipe, wherein a heat insulation layer is coated outside the main body, and the thickness range of the heat insulation layer is 0.15-0.3 mm; the stirring system comprises a motor, a shaft collar, a magnetic transmission system and a stirring paddle, wherein the stirring paddle comprises a shaft core extending into the main body and a blade arranged on the shaft core, the magnetic transmission system comprises an outer magnet and an inner magnet, the inner magnet is connected with the shaft core, the outer magnet is connected with a power shaft of the motor, the range of a gap between the outer magnet and the inner magnet is 0.2-1.2mm, and the range of magnetic rotation torque is 1.2-5.5 N.m; the coil pipes are formed by coiling stainless steel pipes, the outlet ends of the coil pipes are connected with a connector I arranged at the top end of the main body, the effective length range of the coil pipes is 3-5m, and the number of the coil pipes is not less than 3; the temperature sensor I is arranged at the top end of the main body and has a temperature range of 105-225 ℃; the heating pipe and the flow distribution plate are both arranged inside the main body.
Further, the constant temperature system comprises a cylindrical sleeve and a heat preservation shell, the cylindrical sleeve is in a module design, all modules are mutually connected through lock catches, the number of the cylindrical sleeve modules comprises but is not less than 2, a heating rope is spread between the outside of the cylindrical sleeve and the inside of the heat preservation shell in each module, a temperature sensor II is installed inside the heating rope, and the temperature range of the temperature sensor II is 120-500 ℃.
Furthermore, the heat dissipation system comprises a heat exchange tube, a circulating pump, a radiator, a temperature sensor III, a high-temperature pipeline and a low-temperature pipeline, wherein one end of the high-temperature pipeline is connected with an outlet at the bottom end of the heat exchange tube through the circulating pump, and the other end of the high-temperature pipeline is connected with an inlet of the radiator; one end of the low-temperature pipeline is connected with an outlet at the top end of the heat exchange tube, and the other end of the low-temperature pipeline is connected with an outlet of the radiator; the radiator comprises a snake-shaped capillary tube and a fan, a liquid injection port and an overflow port are designed at the top end of the radiator, and the range of a gap between the fan and the rear part of the capillary tube is 0.15-0.5 mm.
Further, the adsorption separation tower is connected with the high-pressure constant flow pump through a pipeline, the high-pressure constant flow pump comprises a desorbent pump, a raw material pump, an extraction liquid pump and a circulating liquid pump, the pipeline comprises a desorbent pipeline, a raw material pipeline, an extraction liquid pipeline, a circulating liquid pipeline and a raffinate pipeline, the desorbent pump is respectively connected with a desorbent storage tank and the adsorption separation tower through the desorbent pipeline, the raw material pump is respectively connected with the raw material storage tank and the adsorption separation tower through the raw material pipeline, the extraction liquid pump is respectively connected with an extraction liquid storage tank and the adsorption separation tower through the extract pipeline, the circulating liquid pump is respectively connected with the bottom end and the top end of the adsorption separation tower through the circulating liquid pipeline, and the raffinate pipeline is respectively connected with the raffinate storage tank and the adsorption separation tower; the desorbent pipeline and the raw material pipeline are respectively provided with a pressure sensor I and a pressure sensor II at outlet sections of the desorbent pump and the raw material pump and pass through the preheating system, the extract pipeline and the raffinate pipeline respectively pass through the heat dissipation system and then are provided with a pressure sensor III and a pressure sensor IV, respectively enter the extract storage tank and before entering the raffinate storage tank, and are provided with a regulating valve I and a regulating valve II, the circulating liquid pipeline passes through the circulating liquid pump, passes through the heat dissipation system from the bottom end of the adsorption separation tower, passes through the preheating system and then enters the top end of the adsorption separation tower, and is provided with a pressure sensor V at an outlet of the circulating liquid pump.
Further, a pressure sensor VI and a temperature sensor IV are arranged at the top end of the adsorption separation tower, wherein the range of the pressure sensor VI is 0.8-1.5Mpa, and the range of the temperature sensor IV is 125-185 ℃.
Furthermore, the heating pipe is in a special-shaped vertical design, an included angle of 75-85 degrees is formed between the top end 1/8-3/8 and a vertical plane, and the heating pipe is located at the position 5-15mm away from the bottom of the paddle; the flow distribution plate is designed in a semi-circular arc mode, and the top end of the flow distribution plate is designed with an ordered porous channel, wherein the open pore area of the porous channel occupies 1/4-1/2 of the flow distribution plate 14.
Further, the temperature difference between the temperature sensor I in the preheating system and the temperature sensor II in the constant temperature system is 5-20 ℃.
Furthermore, the heat exchange tube is designed in a closed mode, a curling coil II is designed in the heat exchange tube, the curling coil II is connected with a joint II, the number of the curling coil II comprises at least 3 groups, a temperature sensor III is installed in the area of the curling coil II, the circulating pump and the rotating speed of the fan are regulated and controlled through the temperature sensor III in a feedback mode, and the temperature range of the temperature sensor III is 20-35 ℃.
In another aspect, the invention provides a temperature control process method using the liquid phase adsorption separation system, comprising the following process steps:
step 1, in a room temperature Rt state, starting all high-pressure constant flow pumps, adjusting an adjusting valve I and an adjusting valve II, maintaining a system pressure sensor VI to be stable in an initial state of 0.5-0.8Mpa, determining the system temperature by a temperature sensor IV, and controlling the temperature by adopting three-level gradient according to a target temperature T;
step 2, setting a first gradient k1, wherein the pre-temperature system temperature value t1 is greater than or equal to Rt +35, the constant-temperature system temperature value t2 is greater than or equal to Rt +55, and the relation of the rotating speed of the heat dissipation system and the pressure regulator Rv (k1) is greater than or equal to 5 v;
and step 4, setting a third gradient k3, wherein the pre-temperature system temperature value T1 is more than or equal to T +75, the constant-temperature system temperature value T2 is more than or equal to T +95, and the relation of the rotating speed of the heat dissipation system and the pressure regulator Rv (k3) is more than or equal to 24 v.
Furthermore, the temperature control process method is suitable for a fixed column type simulated moving bed or a rotary valve type simulated moving bed, wherein the number of fixed columns of the fixed column type simulated moving bed is 4-15, and the number of layers of the rotary valve type simulated moving bed is 10-24.
Advantageous effects
1) The invention discloses a liquid phase adsorption separation system and a temperature control process method thereof, which effectively solve the technical problems of the existing equipment, can effectively avoid the defects that the traditional temperature control mode is easy to cause unstable temperature of a chromatographic column, low heat transfer efficiency, easy carbon formation of a heating tube and a heat-conducting medium and the like, and has the advantages of simple structure, mature technology, high heat transfer efficiency, stable temperature, better temperature control effect and higher precision.
2) The invention discloses a liquid phase adsorption separation system, wherein a brand new magnetic transmission mode is adopted in a stirring mode of a preheating part, so that the transmission of force and torque can be realized without direct contact between a driving shaft and a driven shaft, the phenomena of frequent damage and forced stop of a motor caused by overheating are effectively avoided, and the invention also provides a temperature control process method, a unique preheating, constant temperature and heat dissipation design is provided, and a circulating pump can not run for a long time due to overhigh temperature of a fluid medium while the temperature of a chromatographic column is ensured to be constant, so that the phenomenon of easy damage is avoided, high-price devices are avoided from being purchased, and the liquid phase adsorption separation system has the advantages of longer service life, lower maintenance cost and the like.
3) The invention discloses a liquid phase adsorption separation system and a temperature control process method thereof, which are suitable for the existing liquid phase adsorption separation technologies such as fixed column type and rotary valve type, have strong applicability, can accurately stabilize the temperature of a chromatographic column at a target value +/-5 ℃, and have better practicability.
Drawings
FIG. 1 is a schematic flow diagram of a liquid phase adsorption separation system of the present invention.
FIG. 2 is a schematic diagram of a preheating system in a liquid phase adsorption separation system according to the present invention.
FIG. 3 is a schematic structural diagram of a heat dissipation system in a liquid phase adsorption separation system according to the present invention.
FIG. 4 is a schematic structural view of a constant temperature system in a liquid phase adsorption separation system according to the present invention.
In the figure, 1-adsorption separation column; 2-a constant temperature system; 3-a pre-temperature system; 4-a heat dissipation system; 5-1-a desorbent pump; 5-2-raw material pump; 5-3-an extraction liquid pump; 5-4-circulating liquid pump; 6-1 — desorbent line; 6-2-feedstock line; 6-3-extract line; 6-4-circulating liquid pipeline; 6-5-raffinate line; 7-1-desorbent storage tank; 7-2-raw material storage tank; 7-3-a raffinate storage tank; 7-4-an extract storage tank; 8, a motor; 9-magnetic transmission system; 10-a collar; 11-a heating pipe; 12-an axle core; 13-a porous channel; 14-a splitter plate; 15-a main body; 16-1-linker i; 16-2-linker II; 17-a heat insulation layer; 18-1-coiled pipe I; 18-2-coiled pipe II; 19-liquid injection port; 20-overflow outlet; 21-a fan; 22-capillary tube; 23-a circulating pump; 24-heat exchange tube; 25-a sleeve; 26, locking and buckling; 27-heating rope; 28-a stirring system; 29-temperature sensor i; 30-an outer magnet; 31 — an inner magnet; 32-a blade; 33-coil tubing; 34-a stirring paddle; 35-a power shaft; 36-1-pressure sensor i; 36-2-pressure sensor ii; 36-3-pressure sensor iii; 36-4-pressure sensor IV; 36-5-pressure sensor v; 36-6-pressure sensor VI; 37-1-regulating valve I; 37-2-regulating valve II; 38-temperature sensor ii; 39-heat preservation shell; 40-temperature sensor III; 41-a radiator; 42-high temperature pipeline; 43-cryogenic line; 44-a sewage draining outlet; 45-temperature sensor IV.
Detailed Description
The following further description of the preferred embodiments with reference to the attached drawings will make the advantages and features of the present invention easier to understand by those skilled in the art, and thus the scope of the present invention will be clearly and clearly defined.
Example 1
As shown in fig. 1 to 4, a liquid phase adsorption separation system includes a preheating system 3, a constant temperature system 2, a heat dissipation system 4, an adsorption separation tower 1, a high-pressure constant flow pump, a sensing device, a pipeline, and a valve.
The preheating system 3 is designed in a cylindrical structure and comprises a main body 15, a stirring system 28, a heating pipe 11, a flow distribution plate 14, a temperature sensor I29 and a coil pipe 33, wherein a heat insulation layer 17 is coated outside the main body 15, and the thickness range of the heat insulation layer is 0.15-0.3 mm.
The stirring system 28 comprises a motor 8, a shaft collar 10, a magnetic transmission system 9 and a stirring paddle 34, wherein the stirring paddle 34 comprises a shaft core 12 extending into the main body 15 and a blade 32 mounted on the shaft core 12, the magnetic transmission system 9 comprises an outer magnet 30 and an inner magnet 31, the inner magnet 31 is connected with the shaft core 12, the outer magnet 30 is connected with a power shaft 35 of the motor 8, a gap range between the outer magnet 30 and the inner magnet 31 is 0.2-1.2mm, and a magnetic rotating torque range is 1.2-5.5N · m.
The coil pipe line 33 is formed by coiling stainless steel pipes, the outlet end of the coil pipe line is connected with a connector I16-1 arranged at the top end of the main body 15, the effective length range of the coil pipe line 33 is 3-5m, and the number of the coil pipe lines 33 is not less than 3 groups.
The temperature sensor I29 is arranged at the top end of the main body 15 and has a temperature range of 105-225 ℃.
The heating pipe 11 and the diverter plate 14 are both mounted inside the body 15.
Wherein coiled tubing line 33 forms coiled tubing i 18-1 within body 15.
The constant temperature system 2 comprises a cylindrical sleeve 25 and a heat preservation shell 39, wherein the cylindrical sleeve 25 is in a module design, each module is mutually connected by a lock catch 26, the number of the cylindrical sleeve 25 modules comprises but is not less than 2, a heating rope 27 is spread between the outside of the cylindrical sleeve 25 and the inside of the heat preservation shell 39 in each module, a temperature sensor II 38 is installed inside the heating rope 27, and the temperature range of the temperature sensor II 38 is 120-.
The heat dissipation system 4 comprises a heat exchange pipe 24, a circulating pump 23, a radiator 41, a temperature sensor iii 40, a high-temperature pipeline 42 and a low-temperature pipeline 43.
One end of the high-temperature pipeline 42 is connected with the outlet at the bottom end of the heat exchange pipe 24 through the circulating pump 23, and the other end of the high-temperature pipeline is connected with the inlet of the radiator 41; one end of the low-temperature pipeline 43 is connected with an outlet at the top end of the heat exchange tube 24, and the other end is connected with an outlet of the radiator 41.
The radiator 41 comprises a snake-shaped capillary tube 22 and a fan 21, the top end of the radiator 41 is provided with a liquid injection port 19 and an overflow port 20, and the range of a gap between the fan 21 and the rear part of the capillary tube 22 is 0.15-0.5 mm.
The adsorption separation tower 1 is connected with the high-pressure constant flow pump through a pipeline, the high-pressure constant flow pump comprises a desorbent pump 5-1, a raw material pump 5-2, an extraction liquid pump 5-3 and a circulating liquid pump 5-4, the pipeline comprises a desorbent pipeline 6-1, a raw material pipeline 6-2, an extraction liquid pipeline 6-3, a circulating liquid pipeline 6-4 and a raffinate pipeline 6-5, the desorbent pump 5-1 is respectively connected with a desorbent storage tank 7-1 and the adsorption separation tower 1 through the desorbent pipeline 6-1, the raw material pump 5-2 is respectively connected with the raw material storage tank 7-2 and the adsorption separation tower 1 through the raw material pipeline 6-2, the extraction liquid pump 5-3 is respectively connected with the extraction liquid storage tank 7-4 and the adsorption separation tower 1 through the extract pipeline 6-3, the circulating liquid pump 5-4 is respectively connected with the bottom end and the top end of the adsorption separation tower 1 through the circulating liquid pipeline 6-4, and the raffinate pipeline 6-5 is respectively connected with the raffinate storage tank 7-3 and the adsorption separation tower 1.
The desorbent pipeline 6-1 and the raw material pipeline 6-2 are respectively provided with a pressure sensor I36-1 and a pressure sensor II 36-2 at outlet sections of the desorbent pump 5-1 and the raw material pump 5-2 and pass through the pre-heating system 3, the extract pipeline 6-3 and the raffinate pipeline 6-5 are respectively provided with a pressure sensor III 36-3 and a pressure sensor IV 36-4 after passing through the heat dissipation system 4 and are respectively provided with a regulating valve I37-1 and a regulating valve II 37-2 before entering the extract storage tank 7-4 and the raffinate storage tank 7-3, the recycle liquid pipeline 6-4 passes through the recycle liquid pump 5-4 from the bottom end of the adsorption separation tower 1, passes through the heat dissipation system 4 and the pre-heating system 3, enters the top end of the adsorption separation tower 1 and exits at the recycle liquid pump 5-4 A pressure sensor V36-5 is arranged at the opening.
The top end of the adsorption separation tower 1 is provided with a pressure sensor VI 36-6 and a temperature sensor IV 45, wherein the range of the pressure sensor VI 36-6 is 0.8-1.5Mpa, and the range of the temperature sensor IV 45 is 125-185 ℃.
The heating pipe 11 is in a special-shaped vertical design, an included angle of 75-85 degrees is formed between the top end 1/8-3/8 and a vertical plane, and the heating pipe 11 is located at the position 5-15mm away from the bottom of the paddle 32.
The flow distribution plate 14 is designed in a semi-circular arc manner, and the top end of the flow distribution plate is designed with an ordered porous channel 13, wherein the open area of the porous channel 13 occupies 1/4-1/2 of the flow distribution plate 14.
The temperature difference between the temperature sensor I29 in the preheating system 3 and the temperature sensor II 38 in the constant temperature system 2 is 5-20 ℃.
The heat exchange tube 24 is designed in a closed mode, a curling coil II 18-2 is designed in the heat exchange tube 24, the curling coil II 18-2 is connected with a joint II 16-2, the number of the curling coil II 18-2 comprises at least 3 groups, a temperature sensor III 40 is installed in the area of the curling coil II 18-2, the rotating speed of the circulating pump 23 and the rotating speed of the fan 21 are regulated and controlled through the temperature sensor III 40 in a feedback mode, and the temperature range of the temperature sensor III 40 is 20-35 ℃.
At this time, the liquid phase adsorption separation system of embodiment 1 can effectively solve the technical problems of the existing equipment, and the system can effectively avoid the defects that the traditional temperature control method is easy to cause unstable temperature of the chromatographic column, low heat transfer efficiency, easy carbon deposition of the heating tube and the heat conducting medium, and the like, and has the advantages of simple structure, mature technology, high heat transfer efficiency, stable temperature, better temperature control effect and higher precision; and its stirring mode adopts brand-new magnetic transmission mode at the part of preheating, realizes that can carry out the transmission of power and moment between driving shaft and the driven shaft through direct contact, effectively avoids because of overheated frequent damage of motor, the emergence of compelling the parking phenomenon.
Example 2
As shown in fig. 1 to 4, a temperature control process method using the liquid phase adsorption separation system includes the following steps:
step 1, in a room temperature Rt state, all high-pressure constant flow pumps are started, the regulating valve I37-1 and the regulating valve II 37-2 are regulated, the system pressure sensor VI 36-6 is maintained to be stable in an initial state of 0.5-0.8Mpa, the system temperature is determined by the temperature sensor IV 45, and three-level gradient temperature control is adopted according to a target temperature T;
step 2, setting a first gradient k1, setting a temperature value t1 of the preheating system 3 to be more than or equal to Rt +35, setting a temperature value t2 of the constant temperature system 2 to be more than or equal to Rt +55, and setting a relation of the rotating speed of the heat dissipation system 4 and a pressure regulator Rv (k1) to be more than or equal to 5 v;
and step 4, setting a third gradient k3, wherein the temperature value T1 of the preheating system 3 is more than or equal to T +75, the temperature value T2 of the constant temperature system 2 is more than or equal to T +95, and the relation of the rotating speed of the heat dissipation system 4 and a pressure regulator Rv (k3) is more than or equal to 24 v.
At this moment, the temperature control process method using the liquid phase adsorption separation system in embodiment 2 has unique preheating, constant temperature and heat dissipation designs, ensures that the temperature of the chromatographic column is constant, enables the circulating pump not to operate for a long time due to overhigh temperature of the fluid medium, avoids the occurrence of fragile phenomenon, avoids purchasing expensive devices, has the advantages of long service life, low maintenance cost and the like, can be applied to the existing liquid phase adsorption separation technologies such as fixed column type and rotary valve type, has strong applicability, can accurately stabilize the temperature of the chromatographic column at a target value of +/-5 ℃, and has high practicability.
Example 3
As shown in fig. 2, in the preheating system, a byproduct ditolyl ether of industrially produced cresol isomers is used as a liquid heat-conducting medium, as shown in fig. 1-4, the liquid phase adsorption separation system is adopted and is suitable for a rotary valve type simulated moving bed, the number of bed layers of the rotary valve type simulated moving bed is 10-24, preferably 24, the liquid phase adsorption separation system is applied to the adsorption separation moving simulated bed technology of m-p-cresol, the temperature of a chromatographic column is 150 ℃, and the system pressure is 1.0 Mpa; desorbing agent: n-hexanol/toluene (mass ratio 1:1), adsorbent: BaX, wherein the temperature control technological parameters are as follows:
TABLE 1
Room temperature Rt ═ 21 ℃;
the whole set of equipment is continuously operated for 367h, the temperature of the chromatographic column is stabilized to 142 +/-5 ℃, the pressure value is 0.8-1.0Mpa, the heat-conducting medium of the preheating system and the surface of the heating pipe are smooth, and no coking substance is generated. The temperature of the pump head of the circulating pump is stabilized to 32 +/-2 ℃.
Example 4
In the continuous operation of the whole set of equipment in the embodiment 3, as shown in fig. 2, in the preheating system, preheating stirring is closed, the whole set of equipment is continuously operated for 24 hours, the temperature of the chromatographic column is stabilized to 145 +/-5 ℃, the pressure value is 0.7-0.8Mpa, the color of the heat-conducting medium of the preheating system is darkened, the mobility is poor, the accumulation of the coke on the surface of the heating pipe begins, the continuous operation is continued for 16 hours, the heating pipe is burnt out, a large amount of coke on the surface of the heating pipe and the surface of the coil pipe is enriched, the heat-conducting medium is blackened, and the heat-conducting benefit is lost.
Example 5
As shown in fig. 2, in the preheating system, wulin heat transfer oil company WD340, which is a clear, pale yellow viscous liquid, is used as a liquid heat transfer medium. As shown in fig. 1-4, the liquid phase adsorption separation system is suitable for a fixed column type simulated moving bed, the number of fixed columns of the fixed column type simulated moving bed is 4-15, preferably 8, the liquid phase adsorption separation system is applied to the adsorption separation moving simulated bed technology of m-cresol and p-cresol, the temperature of a chromatographic column is 130 ℃, and the system pressure is 0.8 Mpa; desorbing agent: 2-heptanol/hexanol (mass ratio 3:97), adsorbent: BaX.
TABLE 2
Room temperature Rt ═ 20 ℃;
the whole set of equipment is continuously operated for 432 hours, the temperature of a chromatographic column is stabilized to 127 +/-5 ℃, the pressure value is 0.6-0.7Mpa, the heat-conducting medium of the preheating system is slightly darkened, no coking matter is on the surface of a heating pipe, and the temperature of a pump head of the circulating pump is stabilized to 24 +/-2 ℃.
Example 6
In the continuous operation of the whole set of equipment in the embodiment 5, as shown in fig. 3, in the heat dissipation system, the pressure regulator is closed, the PEEK material support pad is used to isolate the body and the pump head of the circulating pump, the whole set of equipment is continuously operated for 28 hours, the temperature of the chromatographic column is stabilized to 125 ± 5 ℃, the pressure value is 0.3-0.5Mpa, the temperature of the heat dissipation t3 is raised to 67 ± 5 ℃, and the temperature of the circulating pump head is raised to 45 ± 5 ℃; continuously operating for 36h, wherein the temperature of the chromatographic column begins to fluctuate, the precision is reduced, namely 121 +/-15 ℃, when the pressure value of the system is reduced to be below 0.3Mpa, the pump head sealing element deforms due to long-time high-temperature environment operation of the circulating pump, liquid seepage occurs, the operation is stopped, the temperature of the heat dissipation t3 reaches 82 +/-5 ℃, and the temperature of the pump head of the circulating pump approaches 63 +/-5 ℃.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. The liquid phase adsorption separation system is characterized by comprising a preheating system (3), a constant temperature system (2), a heat dissipation system (4), an adsorption separation tower (1), a high-pressure constant-flow pump, a sensing device, a pipeline and a valve piece;
the preheating system (3) is designed in a cylindrical structure and comprises a main body (15), a stirring system (28), a heating pipe (11), a flow distribution plate (14), a temperature sensor I (29) and a coil pipe (33), wherein a heat insulation layer (17) is coated outside the main body (15), and the thickness range of the heat insulation layer is 0.15-0.3 mm;
the stirring system (28) comprises a motor (8), a shaft collar (10), a magnetic transmission system (9) and a stirring paddle (34), wherein the stirring paddle (34) comprises a shaft core (12) extending into the main body (15) and a blade (32) installed on the shaft core (12), the magnetic transmission system (9) comprises an outer magnet (30) and an inner magnet (31), the inner magnet (31) is connected with the shaft core (12), the outer magnet (30) is connected with a power shaft (35) of the motor (8), the gap range between the outer magnet (30) and the inner magnet (31) is 0.2-1.2mm, and the magnetic rotation torque range is 1.2-5.5 N.m;
the coil pipe lines (33) are formed by coiling stainless steel pipes, and the outlet ends of the coil pipe lines are connected with a connector I (16-1) arranged at the top end of the main body (15), wherein the effective length range of the coil pipe lines (33) is 3-5m, and the number of the coil pipe lines (33) comprises not less than 3 groups;
the temperature sensor I (29) is arranged at the top end of the main body (15) and has the temperature range of 105-225 ℃;
the heating pipe (11) and the flow distribution plate (14) are both installed inside the main body (15).
2. The liquid phase adsorption separation system of claim 1, wherein the constant temperature system (2) comprises a cylindrical sleeve (25) and a heat preservation shell (39), the cylindrical sleeve (25) is in a module design, each module is connected with each other by a lock catch (26), the number of the cylindrical sleeve (25) modules comprises but is not less than 2, a heating rope (27) is spread between the outside of the cylindrical sleeve (25) and the inside of the heat preservation shell (39) in each module, a temperature sensor II (38) is installed inside the heating rope (27), and the temperature range of the temperature sensor II (38) is 120-.
3. The liquid-phase adsorptive separation system according to claim 1, wherein said heat-dissipating system (4) comprises a heat exchange pipe (24), a circulation pump (23), a heat sink (41), a temperature sensor iii (40), a high-temperature pipe (42) and a low-temperature pipe (43);
one end of the high-temperature pipeline (42) is connected with an outlet at the bottom end of the heat exchange pipe (24) through the circulating pump (23), and the other end of the high-temperature pipeline is connected with an inlet of the radiator (41); one end of the low-temperature pipeline (43) is connected with an outlet at the top end of the heat exchange tube (24), and the other end of the low-temperature pipeline is connected with an outlet of the radiator (41);
the radiator (41) comprises a snake-shaped capillary tube (22) and a fan (21), the top end of the radiator (41) is provided with a liquid injection port (19) and an overflow port (20), and the range of a gap between the fan (21) and the rear part of the capillary tube (22) is 0.15-0.5 mm.
4. The liquid-phase adsorptive separation system according to claim 1, wherein said adsorptive separation column (1) is connected to said high-pressure constant flow pump by a pipeline, said high-pressure constant flow pump comprises a desorbent pump (5-1), a raw material pump (5-2), an extract pump (5-3) and a recycle liquid pump (5-4), said pipeline comprises a desorbent pipeline (6-1), a raw material pipeline (6-2), an extract pipeline (6-3), a recycle liquid pipeline (6-4), and a raffinate pipeline (6-5), said desorbent pump (5-1) is connected to said adsorptive separation column (1) through said desorbent pipeline (6-1), said raw material pump (5-2) is connected to said raw material storage tank (7-2) and said adsorptive separation column (6-2) through said raw material pipeline (6-2), respectively 1) The de-extraction liquid pump (5-3) is respectively connected with an extraction liquid storage tank (7-4) and the adsorption separation tower (1) through the extraction liquid pipeline (6-3), the circulating liquid pump (5-4) is respectively connected with the bottom end and the top end of the adsorption separation tower (1) through the circulating liquid pipeline (6-4), and the raffinate pipeline (6-5) is respectively connected with a raffinate storage tank (7-3) and the adsorption separation tower (1);
the desorbent pipeline (6-1) and the raw material pipeline (6-2) are respectively provided with a pressure sensor I (36-1) and a pressure sensor II (36-2) at outlet sections of the desorbent pump (5-1) and the raw material pump (5-2) and pass through the preheating system (3), the extract pipeline (6-3) and the raffinate pipeline (6-5) are respectively provided with a pressure sensor III (36-3) and a pressure sensor IV (36-4) after passing through the heat dissipation system (4) and are respectively provided with a regulating valve I (37-1) and a regulating valve II (37-2) before entering the extract storage tank (7-4) and the raffinate storage tank (7-3), and the recycle pipeline (6-4) passes through the heat dissipation system (5-4) from the bottom end of the adsorption separation tower (1) and passes through the bottom end of the heat dissipation tower (1), and the recycle pipeline (6-4) is respectively provided with a regulating valve I (37-1-3) And the system (4) and the preheating system (3) enter the top end of the adsorption separation tower (1) and a pressure sensor V (36-5) is arranged at the outlet of the circulating liquid pump (5-4).
5. The liquid-phase adsorptive separation system according to claim 1, wherein said adsorptive separation column (1) is equipped at its top with a pressure sensor vi (36-6) and a temperature sensor iv (45), wherein said pressure sensor vi (36-6) is in the range of 0.8-1.5Mpa and said temperature sensor iv (45) is in the range of 125-.
6. The liquid phase adsorptive separation system according to claim 1, wherein said heating pipe (11) is of a profiled vertical design with top end 1/8-3/8 being at an angle of 75-85 ° to the vertical, said heating pipe (11) being located 5-15mm from the bottom of said blade (32);
the flow distribution plate (14) is designed in a semi-circular arc manner, and the top end of the flow distribution plate is designed with an ordered porous channel (13), wherein the open area of the porous channel (13) occupies 1/4-1/2 of the flow distribution plate (14).
7. A liquid phase adsorptive separation system according to claim 2 wherein said temperature sensor i (29) in said pre-warming system (3) and said temperature sensor ii (38) in said constant temperature system (2) are at a temperature difference of 5 to 20 ℃.
8. The liquid phase adsorption separation system according to claim 3, wherein the heat exchange tube (24) is of a closed design, a coiled coil II (18-2) is designed in the heat exchange tube, the coiled coil II (18-2) is connected with a joint II (16-2), the number of the coiled coils II (18-2) comprises not less than 3 groups, a temperature sensor III (40) is arranged in the area of the coiled coil II (18-2), the rotating speeds of the circulating pump (23) and the fan (21) are controlled by the temperature sensor III (40) in a feedback mode, and the temperature range of the temperature sensor III (40) is 20-35 ℃.
9. A temperature control process using the liquid phase adsorption separation system according to any one of claims 1 to 8, wherein the temperature control process comprises the steps of:
step 1, in a room temperature Rt state, all high-pressure constant flow pumps are started, a regulating valve I (37-1) and a regulating valve II (37-2) are adjusted, a system pressure sensor VI (36-6) is maintained to be stable in an initial state of 0.5-0.8Mpa, a system temperature is determined by a temperature sensor IV (45), and three-level gradient temperature control is adopted according to a target temperature T;
step 2, setting a first gradient k1, setting a temperature value t1 of the preheating system (3) to be more than or equal to Rt +35, setting a temperature value t2 of the constant temperature system (2) to be more than or equal to Rt +55, and setting a relation expression Rv (k1) between the rotating speed of the heat dissipation system (4) and a pressure regulator to be more than or equal to 5 v;
step 3, setting a second gradient k2, wherein a temperature value t1 of the preheating system (3) is more than or equal to Rt +65, a temperature value t2 of the constant temperature system (2) is more than or equal to Rt +75, and a relation expression Rv (k2) between the rotating speed of the heat dissipation system (4) and a pressure regulator is more than or equal to 12 v;
and 4, setting a third gradient k3, wherein the temperature value T1 of the preheating system (3) is more than or equal to T +75, the temperature value T2 of the constant temperature system (2) is more than or equal to T +95, and the relation of the rotating speed of the heat dissipation system (4) and a pressure regulator Rv (f (k 3)) is more than or equal to 24 v.
10. The temperature-controlled process method of a liquid-phase adsorption separation system according to claim 9, wherein the temperature-controlled process method is applied to a fixed-column simulated moving bed or a rotary valve-type simulated moving bed, wherein the number of fixed columns of the fixed-column simulated moving bed is 4 to 15, and the number of layers of the rotary valve-type simulated moving bed is 10 to 24.
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