CN111097192A - Separation device and separation method for triethylene diamine and ethanolamine - Google Patents

Separation device and separation method for triethylene diamine and ethanolamine Download PDF

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Publication number
CN111097192A
CN111097192A CN201911377606.6A CN201911377606A CN111097192A CN 111097192 A CN111097192 A CN 111097192A CN 201911377606 A CN201911377606 A CN 201911377606A CN 111097192 A CN111097192 A CN 111097192A
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cavity
plate
extraction
ethanolamine
triethylene diamine
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王继宝
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Ningbo Levi Industrial Co Ltd
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Ningbo Levi Industrial Co Ltd
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Priority to CN201911377606.6A priority Critical patent/CN111097192A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0492Applications, solvents used
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D36/00Filter circuits or combinations of filters with other separating devices
    • B01D36/003Filters in combination with devices for the removal of liquids
    • B01D36/006Purge means
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D36/00Filter circuits or combinations of filters with other separating devices
    • B01D36/003Filters in combination with devices for the removal of liquids
    • B01D36/008Means to filter or treat the separated liquid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D36/00Filter circuits or combinations of filters with other separating devices
    • B01D36/02Combinations of filters of different kinds
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C213/00Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
    • C07C213/10Separation; Purification; Stabilisation; Use of additives
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D487/00Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
    • C07D487/02Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains two hetero rings
    • C07D487/08Bridged systems

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to the technical field of chemical industry, and relates to a separation device and a separation method of triethylene diamine and ethanolamine, wherein an extraction cavity is arranged in an extraction tower in the separation device, a sealing plate is arranged at the bottom of the extraction cavity, and the sealing plate is connected with a movable rod of an electric lifting rod; the bottom surface of the extraction cavity is provided with a sleeve, the movable rod is positioned in the sleeve, the top surface of the sleeve is connected with an organ sleeve, and the top end of the organ sleeve is connected with the bottom surface of the sealing plate; the top of the extraction tower is provided with a light-phase liquid outlet which is connected with a treatment device, a treatment cavity is arranged in the treatment device, the top of the treatment cavity is provided with a metal cylinder, and two ends of the metal cylinder are both communicated with the outer side of the treatment device; a drawing plate is arranged below the metal cylinder, an accommodating cavity is arranged in the drawing plate, dry ice blocks are contained in the accommodating cavity, and a heat conducting plate is arranged at the cavity opening of the accommodating cavity; a first sieve plate is arranged below the drawing plate; the bottom surface of the first sieve plate is attached with an eccentric wheel. The present invention can separate triethylene diamine and ethanolamine preferably.

Description

Separation device and separation method for triethylene diamine and ethanolamine
Technical Field
The invention relates to the technical field of chemical industry, in particular to a separation device and a separation method for triethylene diamine and ethanolamine.
Background
Triethylene diamine is a blowing agent for producing soft, semi-hard and hard polyurethane foams, and is also used in ethylene polymerization catalysts, coatings, plastic products and the like.
At present, raw materials for preparing triethylene diamine mainly comprise N-hydroxyethyl piperazine, ethylenediamine, ethanolamine, piperazine and the like. When ethanolamine and liquid ammonia are used as raw materials to catalyze amination to synthesize ethylenediamine or piperazine, triethylene diamine can be co-produced. Because the boiling points of triethylene diamine (the boiling point is 174 ℃) and ethanolamine (the boiling point is 170 ℃) are very close, the triethylene diamine and the ethanolamine are easy to form an azeotrope, and the triethylene diamine and the ethanolamine are difficult to separate by adopting a conventional rectification method.
In the separation method of triethylene diamine and ethanolamine, the operation is often carried out through an extraction tower, but the extraction time of the existing extraction tower is long, the separation operation is often carried out through a plurality of devices, the operation is complex, the cooling and filtering effects are poor, and the efficiency is low.
Disclosure of Invention
The invention provides a separation device and a separation method for triethylene diamine and ethanolamine, which can overcome certain defects in the prior art.
The separation device for triethylene diamine and ethanolamine comprises an extraction tower, wherein an extraction cavity is arranged in the extraction tower, a sealing plate is arranged at the bottom of the extraction cavity, the bottom end of the sealing plate is connected with a movable rod of an electric lifting rod, and a rod body of the electric lifting rod penetrates out of the bottom of the extraction tower; the bottom surface of the extraction cavity is provided with a sleeve, the movable rod is positioned in the sleeve, the top surface of the sleeve is connected with an organ sleeve, and the top end of the organ sleeve is connected with the bottom surface of the sealing plate; the top of the extraction tower is provided with a light-phase liquid outlet, the light-phase liquid outlet is connected with a treatment device through a pipeline, a treatment cavity is arranged in the treatment device, the top of the treatment cavity is provided with a plurality of horizontal metal cylinders, and two ends of each metal cylinder are communicated with the outer side of the treatment device; a movable drawing plate is arranged below the metal cylinder, one end of the drawing plate penetrates out of the treatment device, an accommodating cavity with an upward opening is arranged in the drawing plate, dry ice blocks are contained in the accommodating cavity, and a heat conducting plate is arranged at the cavity opening of the accommodating cavity; a first sieve plate is obliquely arranged below the drawing plate, one end of the first sieve plate is hinged to the wall of the treatment cavity, and the other end of the first sieve plate penetrates through the treatment cavity and corresponds to a collecting tank; the bottom surface of the first sieve plate is attached with an eccentric wheel, and the eccentric wheel is driven by a first motor.
Through the lift of electric lift pole, drive reciprocating of closing plate for space in the extraction tower can change the size, when dwindling, can be convenient with the liquid extrusion in the extraction tower, thereby make the play liquid speed of extraction tower faster, shorten the time, raise the efficiency. Liquid with low density is discharged from the light-phase liquid outlet, the discharged liquid is led into a treatment cavity in the treatment device from the pipeline, the drawing plate can block the liquid, then dry ice and the metal cylinder in the drawing plate can rapidly cool the liquid, and two ends of the metal cylinder are communicated with the outer side of the treatment device, so that cooling substances can be introduced into the metal cylinder, and the cooling efficiency is improved. After cooling, the pumping plate can be pumped to discharge the cooled liquid, which is very convenient. Because what come out from light phase liquid outlet after triethylene diamine and ethanolamine mixture extract is the mixture of triethylene diamine and extractant, can produce the triethylene diamine solid after the cooling, the solid falls into first sieve and filters, because first sieve slope sets up, the solid can fall into to collect the inslot, remaining liquid falls into the treatment chamber bottom, like this, triethylene diamine just can effectual separation. First motor drive eccentric wheel rotates, makes first sieve shake, improves filterable efficiency, also makes faster entering of solid to collect the inslot.
Because the liquid can flow out from the clearance between closing plate and the extraction cavity wall, so the setting of sleeve and wind musical instrument cover can prevent that liquid from flowing into on the movable rod of electric lift pole, guarantees the stability of electric lift pole work. The piano cover can be lifted along with the lifting of the electric lifting rod, so that liquid cannot flow into the movable rod of the electric lifting rod in the lifting process of the electric lifting rod.
In the embodiment, the top end of the extraction cavity is rotatably connected with a rotating rod, the bottom end of the rotating rod is connected with a supporting block, the supporting block is positioned above the sealing plate, a reinforcing block is rotatably sleeved on the rod body of the rotating rod, the supporting block and the reinforcing block are connected to the wall of the extraction cavity through a plurality of connecting rods, the rotating rod is provided with a plurality of rotating discs, and the plurality of rotating discs are positioned between the supporting block and the reinforcing block; the turntable is matched with a fixing ring which is connected on the wall of the extraction cavity; the rotating rod is driven by a second motor, and the second motor is positioned on the top surface of the extraction tower.
The fixed ring divides the tower into a plurality of small spaces, the second motor drives the rotating rod to rotate, the rotating disc on the rotating rod rotates to enable the shearing stress generated in the liquid to break the dispersed phase into a plurality of fine liquid drops, and strong vortex motion is generated in the liquid phase, so that the interphase contact area and the mass transfer coefficient are increased. The setting of supporting shoe and reinforcing block has improved carousel pivoted stability.
In this embodiment, a valve is disposed on the pipeline.
The valve can control the on-off of liquid in the pipeline.
In this embodiment, the extraction tower bottom is equipped with a plurality of branches, be equipped with the backup pad between a plurality of branches, electric lift rod bottom end is fixed in the backup pad.
The support rod is used for supporting the extraction tower, and the support plate is used for supporting the electric lifting rod.
In this embodiment, the first liquid outlet is arranged at the lowest part of the side surface of the extraction cavity.
The first liquid outlet is arranged to discharge liquid leaking from the sealing plate.
In this embodiment, processing apparatus one side is equipped with the export, and export is worn out to first sieve one end.
The outlet is arranged to facilitate vibration of the first screening deck.
In the embodiment, a second sieve plate is arranged in the collecting tank, and the bottom end of the collecting tank is communicated with the bottom end of the treatment cavity; the bottom end of the collecting tank is also provided with a second liquid outlet.
The second sieve plate can carry out secondary filtration, so that the liquid attached to the triethylene diamine solid can flow into the bottom of the collecting tank after a long time. The bottom end of the collecting groove is communicated with the bottom end of the processing cavity, so that the liquid at the bottom end of the processing cavity can be collected to the bottom end of the collecting groove, and then the liquid can be conveniently discharged from the second liquid outlet.
The embodiment also provides a separation method of triethylene diamine and ethanolamine, which comprises the following steps:
firstly, adding an azeotrope of triethylene diamine and ethanolamine from the lower part of an extraction tower, adding an extracting agent from the upper part of the extraction tower, controlling the temperature to be 90-130 ℃, and then controlling a rotating rod to rotate for stirring;
opening a valve on the pipeline, then controlling an electric lifting rod to lift a sealing plate, and enabling a mixture of the triethylene diamine and the extractant to flow into the treatment cavity;
thirdly, the mixture of the triethylene diamine and the extractant falls into a space above the drawing plate, cold air is filled into the metal cylinder, and the mixture is cooled by the cold air and dry ice on the drawing plate to generate triethylene diamine solid;
fourthly, after cooling, drawing out the drawing plate, enabling the triethylene diamine solid to fall into a first sieve plate for filtering, controlling an eccentric wheel to rotate, enabling the solid to fall into the collecting tank quickly, enabling the residual liquid to fall into the cavity bottom of the treatment cavity, and then enabling the residual liquid to flow into the bottom of the collecting tank;
fifthly, the solid in the collecting tank is blocked by the second sieve plate, and the liquid attached to the solid falls into the bottom of the collecting tank;
sixthly, the liquid at the bottom of the collecting tank is circulated to the top of the treatment cavity;
and seventhly, taking out the mixture of the extracting agent and the ethanolamine at the bottom of the extracting tower, and then carrying out rectification separation in a rectifying tower to obtain the ethanolamine.
Wherein the extractant is 1, 3-dimethyl imidazolidinone.
The method can conveniently separate the triethylene diamine and the ethanolamine, and has the advantages of less time consumption, high efficiency, less used equipment and low cost.
Drawings
FIG. 1 is a schematic view showing a structure of a separation apparatus for triethylenediamine and ethanolamine according to example 1;
FIG. 2 is an enlarged view of the structure of the sleeve in embodiment 1;
fig. 3 is a schematic structural view of an eccentric wheel in embodiment 1.
Detailed Description
For a further understanding of the invention, reference should be made to the following detailed description taken in conjunction with the accompanying drawings and examples. It is to be understood that the examples are illustrative of the invention and not limiting.
Example 1
As shown in fig. 1, fig. 2 and fig. 3, the present embodiment provides a separation apparatus for triethylene diamine and ethanolamine, which includes an extraction tower 110, an extraction chamber 111 is disposed in the extraction tower 110, a sealing plate 120 is disposed at the bottom of the extraction chamber 111, the bottom end of the sealing plate 120 is connected to a movable rod of an electric lifting rod 130, and a rod body of the electric lifting rod 130 penetrates through the bottom of the extraction tower 110; the bottom surface of the extraction cavity 111 is provided with a sleeve 140, the movable rod is positioned in the sleeve 140, the top surface of the sleeve 140 is connected with a wind instrument sleeve 150, and the top end of the wind instrument sleeve 150 is connected with the bottom surface of the sealing plate 120; the top of the extraction tower 110 is provided with a light phase liquid outlet 112, the light phase liquid outlet 112 is connected with a processing device 210 through a pipeline 160, a processing cavity 211 is arranged in the processing device 210, the top of the processing cavity 211 is provided with a plurality of horizontal metal cylinders 220, and two ends of each metal cylinder 220 are communicated with the outer side of the processing device 210; a movable drawing plate 230 is arranged below the metal cylinder 220, one end of the drawing plate 230 penetrates out of the processing device 210, an accommodating cavity 231 with an upward opening is arranged in the drawing plate 230, dry ice blocks 232 are contained in the accommodating cavity 231, and a heat conducting plate 233 is arranged at the cavity opening of the accommodating cavity 231; a first sieve plate 240 is obliquely arranged below the drawing plate 230, one end of the first sieve plate 240 is hinged to the wall of the treatment cavity 211, and the other end of the first sieve plate 240 penetrates through the treatment cavity 211 and then corresponds to a collecting tank 250; the first screening plate 240 has an eccentric 260 attached to a bottom surface thereof, and the eccentric 260 is driven by a first motor 270.
Through the lift of electric lift pole 130, drive reciprocating of closing plate 120 for the space in the extraction tower 110 can change the size, when reducing, can be convenient with the liquid extrusion in the extraction tower 110, thereby make the play liquid speed of extraction tower 110 faster, shorten the time, raise the efficiency. Liquid with lower density is discharged from the light-phase liquid outlet 112, the discharged liquid is led into the treatment cavity 211 in the treatment device 210 from the pipeline 160, the drawing plate 230 can block the liquid, then the dry ice in the drawing plate 230 and the metal cylinder 220 can rapidly cool the liquid, and two ends of the metal cylinder 220 are communicated with the outer side of the treatment device 210, so that cooling substances can be led into the metal cylinder 220, and the cooling efficiency is improved. After cooling, the pumping plate 230 is pumped to discharge the cooled liquid, which is very convenient. Because what come out from light phase liquid outlet 112 after triethylene diamine and ethanolamine mixture extract is the mixture of triethylene diamine and extractant, can produce the triethylene diamine solid after the cooling, the solid falls into first sieve 240 and filters, because first sieve 240 slope sets up, the solid can fall into to collect the inslot 250, and remaining liquid falls into the bottom of treatment chamber 211, and like this, triethylene diamine just can effectual separation. The first motor 270 drives the eccentric 260 to rotate, shaking the first screen deck 240, increasing the efficiency of the filtration, and allowing solids to enter the collection tank 250 more quickly.
Since the liquid flows out from the gap between the sealing plate 120 and the wall of the extraction chamber 111, the sleeve 140 and the piano cover 150 can prevent the liquid from flowing into the movable rod of the electric lift rod 130, thereby ensuring the stability of the operation of the electric lift rod 130. The wind instrument cover 150 can be lifted up and down along with the lifting and lowering of the electric lift rod 130, so that liquid does not flow into the movable rod of the electric lift rod 130 even during the lifting and lowering of the electric lift rod 130.
In this embodiment, the top end of the extraction chamber 111 is rotatably connected with a rotating rod 171, the bottom end of the rotating rod 171 is connected with a supporting block 172, the supporting block 172 is located above the sealing plate 120, the rod body of the rotating rod 171 is rotatably sleeved with a reinforcing block 173, the supporting block 172 and the reinforcing block 173 are connected to the wall of the extraction chamber 111 through a plurality of connecting rods 174, the rotating rod 171 is provided with a plurality of rotating discs 175, and the plurality of rotating discs 175 are located between the supporting block 172 and the reinforcing block 173; the turntable 175 is matched with a fixing ring 176, and the fixing ring 176 is connected on the wall of the extraction cavity 111; the rotary shaft 171 is driven by a second motor 177, and the second motor 177 is located on the top surface of the extraction column 110.
The fixed ring 176 divides the tower into a plurality of small spaces, the second motor 177 drives the rotating rod 171 to rotate, the rotating disc 175 on the rotating rod 171 rotates to enable shear stress generated in the liquid to break the dispersed phase into a plurality of fine liquid drops, and strong vortex motion is generated in the liquid phase, so that the interphase contact area and the mass transfer coefficient are increased. The provision of the support blocks 172 and the reinforcing blocks 173 improves the stability of the rotation of the turntable 175.
In this embodiment, a valve 161 is disposed on the pipe 160.
Valve 161 can control the opening and closing of the fluid in conduit 160.
In this embodiment, the bottom of the extraction tower 110 is provided with a plurality of support rods 113, a support plate 114 is disposed between the plurality of support rods 113, and the bottom end of the electric lifting rod 130 is fixed on the support plate 114.
The support rods 113 are used to support the extraction tower 110, and the support plates 114 are used to support the motorized lift pins 130.
In this embodiment, the first liquid outlet 115 is disposed at the lowest position of the side surface of the extraction chamber 111.
The first outlet port 115 is provided to discharge the liquid leaked from the sealing plate 120.
In this embodiment, an outlet 212 is disposed at one side of the processing device 210, and one end of the first screen plate 240 penetrates through the outlet 212.
The provision of the outlet 212 facilitates vibration of the first screening deck 240.
In this embodiment, a second sieve plate 251 is disposed in the collecting tank 250, and the bottom end of the collecting tank 250 is communicated with the bottom end of the processing cavity 211; the bottom end of the collection tank 250 is also provided with a second liquid outlet 252.
The second sieve plate 251 can perform secondary filtration, so that the liquid attached to the triethylenediamine solid flows into the bottom of the collection tank 250 after a long time. The bottom end of the collection tank 250 is in communication with the bottom end of the processing chamber 211, which enables liquid in the bottom end of the processing chamber 211 to collect in the bottom end of the collection tank 250 and then conveniently exit the second outlet 252.
The embodiment also provides a separation method of triethylene diamine and ethanolamine, which comprises the following steps:
firstly, adding an azeotrope of triethylene diamine and ethanolamine from the lower part of an extraction tower, adding an extracting agent from the upper part of the extraction tower, controlling the temperature to be 90-130 ℃, and then controlling a rotating rod 171 to rotate for stirring;
secondly, opening a valve 161 on the pipeline 160, and then controlling the electric lifting rod 130 to lift the sealing plate 120, so that the mixture of the triethylene diamine and the extractant flows into the processing chamber 211;
thirdly, the mixture of the triethylene diamine and the extractant falls into the space above the drawing plate 230, cold air is filled into the metal cylinder 220, and the mixture is cooled by the cold air and dry ice on the drawing plate 230 to generate triethylene diamine solid;
fourthly, after cooling, the drawing plate 230 is drawn out, the triethylene diamine solid falls into the first sieve plate 240 for filtering, the eccentric wheel 260 is controlled to rotate, the solid quickly falls into the collecting tank 250, and the residual liquid falls into the bottom of the treatment cavity 211 and then flows into the bottom of the collecting tank 250;
fifthly, the solids in the collecting tank 250 are blocked by the second sieve plate 251, and the liquid attached to the solids falls into the bottom of the collecting tank 250;
sixthly, the liquid at the bottom of the collecting tank 250 is circulated to the top of the processing cavity 211;
and seventhly, taking out the mixture of the extracting agent and the ethanolamine at the bottom of the extracting tower, and then carrying out rectification separation in a rectifying tower to obtain the ethanolamine.
Wherein the extractant is 1, 3-dimethyl imidazolidinone.
The method can conveniently separate the triethylene diamine and the ethanolamine, and has the advantages of less time consumption, high efficiency, less used equipment and low cost.
In this embodiment, the second motor 177 and the electric lifting rod 130 can be exchanged in position, and other related components are modified accordingly. Thus, the liquid is less likely to leak from the sealing plate 120 by gravity.
The present invention and its embodiments have been described above schematically, without limitation, and what is shown in the drawings is only one of the embodiments of the present invention, and the actual structure is not limited thereto. Therefore, if the person skilled in the art receives the teaching, without departing from the spirit of the invention, the person skilled in the art shall not inventively design the similar structural modes and embodiments to the technical solution, but shall fall within the scope of the invention.

Claims (9)

1. Triethylene diamine and ethanolamine's separator, its characterized in that: the extraction tower comprises an extraction tower (110), wherein an extraction cavity (111) is arranged in the extraction tower (110), a sealing plate (120) is arranged at the bottom of the extraction cavity (111), the bottom end of the sealing plate (120) is connected with a movable rod of an electric lifting rod (130), and a rod body of the electric lifting rod (130) penetrates out of the bottom of the extraction tower (110); a sleeve (140) is arranged on the bottom surface of the extraction cavity (111), the movable rod is positioned in the sleeve (140), the top surface of the sleeve (140) is connected with a bellows sleeve (150), and the top end of the bellows sleeve (150) is connected with the bottom surface of the sealing plate (120); the top of the extraction tower (110) is provided with a light-phase liquid outlet (112), the light-phase liquid outlet (112) is connected with a treatment device (210) through a pipeline (160), a treatment cavity (211) is arranged in the treatment device (210), the top of the treatment cavity (211) is provided with a plurality of horizontal metal cylinders (220), and two ends of each metal cylinder (220) are communicated with the outer side of the treatment device (210); a movable drawing plate (230) is arranged below the metal cylinder (220), one end of the drawing plate (230) penetrates out of the processing device (210), an accommodating cavity (231) with an upward opening is arranged in the drawing plate (230), dry ice blocks (232) are contained in the accommodating cavity (231), and a heat conducting plate (233) is arranged at the cavity opening of the accommodating cavity (231); a first sieve plate (240) is obliquely arranged below the drawing plate (230), one end of the first sieve plate (240) is hinged to the wall of the treatment cavity (211), and the other end of the first sieve plate (240) penetrates through the treatment cavity (211) and then corresponds to a collecting tank (250); the bottom surface of the first sieve plate (240) is attached with an eccentric wheel (260), and the eccentric wheel (260) is driven by a first motor (270).
2. The separation apparatus of triethylenediamine and ethanolamine according to claim 1, wherein: the top end of the extraction cavity (111) is rotatably connected with a rotating rod (171), the bottom end of the rotating rod (171) is connected with a supporting block (172), the supporting block (172) is positioned above the sealing plate (120), a reinforcing block (173) is rotatably sleeved on the rod body of the rotating rod (171), the supporting block (172) and the reinforcing block (173) are connected to the wall of the extraction cavity (111) through a plurality of connecting rods (174), a plurality of turntables (175) are arranged on the rotating rod (171), and the plurality of turntables (175) are positioned between the supporting block (172) and the reinforcing block (173); the turntable (175) is matched with a fixing ring (176), and the fixing ring (176) is connected to the wall of the extraction cavity (111); the rotating rod (171) is driven by a second motor (177), and the second motor (177) is positioned on the top surface of the extraction column (110).
3. The separation apparatus of triethylenediamine from ethanolamine according to claim 2, characterized in that: the pipeline (160) is provided with a valve (161).
4. The separation apparatus of triethylenediamine from ethanolamine according to claim 3, characterized in that: a plurality of supporting rods (113) are arranged at the bottom of the extraction tower (110), a supporting plate (114) is arranged among the supporting rods (113), and the bottom end of the electric lifting rod (130) is fixed on the supporting plate (114).
5. The separation apparatus of triethylenediamine from ethanolamine according to claim 4, wherein: the first liquid outlet (115) is arranged at the lowest part of the side surface of the extraction cavity (111).
6. The separation apparatus of triethylenediamine from ethanolamine according to claim 5, wherein: an outlet (212) is arranged on one side of the processing device (210), and one end of the first sieve plate (240) penetrates out of the outlet (212).
7. The separation apparatus of triethylenediamine from ethanolamine according to claim 6, wherein: a second sieve plate (251) is arranged in the collecting tank (250), and the bottom end of the collecting tank (250) is communicated with the bottom end of the processing cavity (211); the bottom end of the collecting tank (250) is also provided with a second liquid outlet (252).
8. A method for separating triethylene diamine from ethanolamine is characterized by comprising the following steps: the method comprises the following steps:
firstly, adding an azeotrope of triethylene diamine and ethanolamine from the lower part of an extraction tower, adding an extracting agent from the upper part of the extraction tower, controlling the temperature to be 90-130 ℃, and then controlling a rotating rod (171) to rotate for stirring;
secondly, opening a valve (161) on the pipeline (160), then controlling an electric lifting rod (130) to lift a sealing plate (120), and enabling a mixture of the triethylene diamine and the extractant to flow into the processing cavity (211);
thirdly, the mixture of the triethylene diamine and the extractant falls into a space above the drawing plate (230), cold air is filled into the metal cylinder (220), and the cold air and dry ice on the drawing plate (230) cool the mixture to generate triethylene diamine solid;
fourthly, after cooling, drawing out the drawing plate (230), enabling the triethylene diamine solid to fall into a first sieve plate (240) for filtering, controlling an eccentric wheel (260) to rotate, enabling the solid to fall into the collecting tank (250) quickly, enabling the residual liquid to fall into the bottom of the processing cavity (211), and then enabling the residual liquid to flow into the bottom of the collecting tank (250);
fifthly, the solids in the collecting tank (250) are blocked by a second sieve plate (251), and the liquid attached to the solids can fall into the bottom of the collecting tank (250);
sixthly, the liquid at the bottom of the collecting tank (250) is circulated to the top of the treatment cavity (211);
and seventhly, taking out the mixture of the extracting agent and the ethanolamine at the bottom of the extracting tower, and then carrying out rectification separation in a rectifying tower to obtain the ethanolamine.
9. The method for separating triethylenediamine from ethanolamine according to claim 8, wherein: the extractant is 1, 3-dimethyl imidazolinone.
CN201911377606.6A 2019-12-27 2019-12-27 Separation device and separation method for triethylene diamine and ethanolamine Pending CN111097192A (en)

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CN114084530A (en) * 2021-11-11 2022-02-25 天驰药业有限公司 Collection tank suitable for 2, 6-dichlorobenzonitrile

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