CN111991851A - Xylene-brine separation method - Google Patents
Xylene-brine separation method Download PDFInfo
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- CN111991851A CN111991851A CN202010753603.4A CN202010753603A CN111991851A CN 111991851 A CN111991851 A CN 111991851A CN 202010753603 A CN202010753603 A CN 202010753603A CN 111991851 A CN111991851 A CN 111991851A
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- xylene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0208—Separation of non-miscible liquids by sedimentation
- B01D17/0214—Separation of non-miscible liquids by sedimentation with removal of one of the phases
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/12—Auxiliary equipment particularly adapted for use with liquid-separating apparatus, e.g. control circuits
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
Abstract
The invention discloses a xylene-brine separation method, which comprises the following steps: firstly, introducing brine, ethanol and xylene waste liquor generated in the production of Polydimethylsilane (PDMS) into a separation tank for standing; after standing and layering, discharging the brine with ethanol dissolved in the brine through a brine discharge valve of the separation tank, and simultaneously discharging the dimethylbenzene in the separation tank through a dimethylbenzene discharge valve of the separation tank. After the technical scheme is adopted, the method can efficiently separate a large amount of xylene-saline waste liquid generated in the process of preparing the Polydimethylsilane (PDMS), and recover ethanol and xylene in the waste liquid, so that the recycling of a solvent is realized, the waste liquid treatment capacity is reduced, and the cost for producing the PDMS is reduced.
Description
Technical Field
The invention relates to the chemical industry, in particular to a xylene-brine separation method.
Background
Polydimethylsilane (PDMS) is a raw material for synthesizing Polycarbosilane (PCS) [ songyancai, yao, von chunxiang, lou. 753-757]. The synthesis of the Polydimethylsilane (PDMS) is that monomer dichlorodimethylsilane reacts with metallic sodium for dechlorination and polycondensation, and after the polycondensation reaction is finished, unreacted metallic sodium and dichlorodimethylsilane monomers need to be digested by absolute ethyl alcohol; then respectively washing with pure water to remove sodium chloride and sodium ethoxide; the by-products are removed by washing with xylene. And finally drying to obtain Polydimethylsiloxane (PDMS) [ Happy pine Min, Chenyiluo ] organic silicon synthesis process and product application [ M ]. Beijing: chemical industry Press, 2001.793-815 ]. A large amount of waste liquid is generated in the processes of reaction, washing and drying. The waste liquid mainly consists of xylene, brine, ethanol and byproducts washed off in the washing process. The brine in which the ethanol is dissolved is deposited at the bottom and the xylene at the top, and the washed byproducts form an emulsion layer between the xylene layer and the brine layer. If the waste liquid is treated as waste chemical liquid, the production of Polydimethylsilane (PDMS) is greatly cost-effectively and environmental pressure is generated; if the waste liquid is kept stand for layering and separated, the saline water dissolved with the ethanol and the xylene respectively recover the ethanol and the xylene, the recovered ethanol and the xylene can be used for producing the Polydimethylsilane (PDMS) again, the recycling of the solvent is realized, the treatment capacity of the waste liquid can be reduced, and the cost for producing the Polydimethylsilane (PDMS) is further reduced. Therefore, xylene and brine in the waste liquid can be effectively separated, which is a problem to be solved urgently in the production of Polydimethylsilane (PDMS).
Because the existence of the emulsion layer, can't form clear interface between xylol and the salt solution, can't use traditional interface detector as detecting the layering position, and traditional conductivity measurement device antipollution is poor, runs into the emulsion layer and breaks down easily, and how differentiate xylol or salt solution is also the difficult problem that awaits a diligent solution in the waste liquid separation.
Disclosure of Invention
In order to solve the problems, the invention provides a xylene-brine separation method, which can be used for efficiently separating a large amount of xylene-brine waste liquid generated in the process of preparing Polydimethylsilane (PDMS), and recovering ethanol and xylene in the waste liquid, so that the solvent is recycled, the waste liquid treatment capacity is reduced, and the cost for producing the Polydimethylsilane (PDMS) is reduced.
In order to achieve the purpose, the invention adopts the following technical scheme:
a xylene-brine separation process comprising the steps of:
(1) firstly, introducing brine, ethanol and xylene waste liquor generated in the production of Polydimethylsilane (PDMS) into a separation tank for standing;
(2) after standing and layering, discharging the brine with ethanol dissolved in the brine through a brine discharge valve of the separation tank, and simultaneously discharging the dimethylbenzene in the separation tank through a dimethylbenzene discharge valve of the separation tank.
By adopting the structure, the brine and the xylene waste liquid in the production process of the Polydimethylsilane (PDMS) are collected to a separation tank in a centralized manner and are kept stand for layering, the brine with ethanol dissolved after layering is deposited at the bottom of the separation tank, and the xylene is positioned above the brine; discharging the saline water with the ethanol dissolved in the separation tank to an ethanol distillation device through a saline water discharge valve at the bottom to recover the ethanol; xylene discharges the valve through the xylol of knockout drum side and discharges to the xylene distillation plant in the recovery xylene of distilling, and the ethanol and the xylene of retrieving can be used for Polydimethylsilane (PDMS) production again, adopted promptly with distillation collocation, realized the recovery of xylene and ethanol in the PDMS production, reduced PDMS manufacturing cost, degree of automation is high, safe and reliable.
Preferably, in the step (2), each discharge valve is provided with a corresponding determination electrode for determining whether the liquid at the position of the discharge valve is brine or xylene, and the interlocking control of the discharge valves is realized to prevent xylene from being discharged from the brine discharge valve or to discharge brine from the xylene discharge valve.
Preferably, the brine discharge valve is arranged on the bottom of the separation tank, and a discrimination electrode matched with the brine discharge valve is arranged near the upper part of the brine discharge valve.
By adopting the structure, the brine dissolving the ethanol in the separation tank can be discharged to the ethanol distillation device through the brine discharge valve to recover the ethanol. And a distinguishing electrode is arranged on the brine discharge valve close to the brine discharge valve and used for distinguishing xylene or brine in the liquid at the electrode mounting position and realizing the linkage control of the brine discharge valve. When the liquid at the installation position of the electrode is judged to be saline, the liquid discharged by the saline discharge valve at the bottom is certainly saline, and saline can be discharged; when the liquid for distinguishing the installation position of the electrode is xylene, the liquid discharged from the bottom brine discharge valve can be xylene, the discharged liquid can be xylene, and the brine discharge valve is locked and closed to prevent the xylene from being discharged to the ethanol distillation device.
Preferably, a plurality of xylene discharging valves are arranged on the side edge of the separation tank along the length direction of the separation tank, each xylene discharging valve is provided with a distinguishing electrode, and the corresponding distinguishing electrode is arranged near the lower part of the xylene discharging valve.
By adopting the structure, the xylene in the separating tank can be discharged to the xylene distilling device through the xylene discharging valve to recover the xylene. And a discrimination electrode is arranged below the xylene discharge valve and close to the xylene discharge valve, and is used for discriminating whether the liquid at the electrode mounting position is xylene or brine and realizing the linkage control of the xylene discharge valve. When the liquid at the position where the electrodes are installed is the dimethylbenzene, the liquid discharged by the dimethylbenzene discharge valve is definitely the dimethylbenzene and can be discharged; when the liquid at the position of the discriminating electrode is brine, the liquid discharged from the xylene discharging valve may be brine, and the discharged liquid may be brine, and the xylene discharging valve is locked to be closed to prevent the brine from being discharged to the xylene distillation apparatus.
Preferably, the control system is used for performing interlock control, and the control system can detect and display the judging state of the judging electrode and the opening and closing state of the valve.
By adopting the structure, the control system can detect and display the judging state of the judging electrode and the opening and closing state of the valve, open and close the valve through the control system and complete the linkage locking function.
Preferably, the distinguishing electrode comprises an electrode rod, an insulating assembly, an electrode fixing flange, a separating tank mounting flange, a low-voltage power frequency power supply, a voltage division inductor and a voltage detection meter; the motor rod is fixedly arranged on the mounting flange of the separation tank by the electrode fixing flange through the insulating assembly; the electrode rod is electrically insulated from the electrode fixing flange and the separating tank mounting flange and keeps the sealing property; the alternating voltage output by the low-voltage power frequency power supply is 12-36V, one end of the output voltage of the low-voltage power frequency power supply is connected with the separation tank and is grounded, and the other end of the low-voltage power frequency power supply is connected with the electrode rod after being connected with a voltage division inductor in series; the voltage detection meter is used for detecting the voltage between the separation tank and the electrode rod of the distinguishing electrode, can measure the voltage to judge whether the liquid at the position where the electrode rod of the distinguishing electrode is located is dimethylbenzene or saline water, and displays the liquid through the indicator lamp and feeds the liquid back to the control system.
Adopt this structure, electrode rod is close to the cover of knockout drum mounted position and is had the insulating tube promptly, avoids the pollution of emulsion layer granule to the judgement electrode, and the voltage detection table has high limit output lamp and low limit output lamp to with voltage signal output to control system in order to realize coordinated control. When the electrode rod is soaked in brine, the conductivity of the brine is good, the electrode rod and the separation tank are in a short-circuit state, the voltage of the low-voltage power frequency power supply is almost loaded on the voltage-dividing inductor, the voltage detected by the voltage detection meter is lower than a set lower limit value, and the low-voltage limit output lamp is turned on; when the electrode rod is soaked in xylene or exposed in air, due to poor conductivity of the xylene and the air, the electrode rod and the separation tank are in an open circuit state, the voltage of the low-voltage power frequency power supply is almost loaded between the electrode rod and the separation tank, the voltage detected by the voltage detection meter is higher than a set upper limit value, and the high-voltage output lamp is on; because the emulsion layer is provided with mixed liquid of dimethylbenzene and saline water, the electrode rod has certain conductivity, when the electrode rod is positioned in the emulsion layer, the voltage of the low-voltage power frequency power supply can be distributed among the distinguishing electrode, the separating tank and the voltage-dividing inductor according to a certain proportion, the voltage of the voltage detection meter is lower than a set upper limit and higher than a set lower limit, and the voltage high-limit output lamp and the voltage low-limit output lamp are not on.
Preferably, the number of the discriminating electrodes is 3, and the discriminating electrodes are respectively an upper discriminating electrode, a middle discriminating electrode and a lower discriminating electrode which are sequentially arranged on one side of the separating tank from top to bottom; the xylene discharge valve is 2, and is respectively an upper xylene discharge valve and a lower xylene discharge valve.
By adopting the structure, a plurality of sets of xylene discharge valves and corresponding discrimination electrodes can be arranged in the separation tank at different heights, and the xylene discharge valves can be flexibly selected to discharge xylene according to different xylene positions.
Preferably, a waste liquid inlet valve is further arranged on the top of the separation tank and connected with a radar liquid level meter.
Adopt this structure, the waste liquid that produces Polydimethylsilane (PDMS) promptly enters into the knockout drum through the waste liquid feed valve, and the radar level gauge that detects total liquid level height is installed at the top of knockout drum, and the radar level gauge realizes the linkage with the waste liquid feed valve, and when total liquid level height was higher than the upper limit, the waste liquid feed valve was closed by the locking to prevent that the knockout drum liquid from spilling over.
Preferably, the separating tank is far away from one side of the middle discrimination electrode, and is further connected with an emulsion layer discharge valve for discharging an emulsion layer in the separating tank, wherein the emulsion layer discharge valve is at the same height as the middle discrimination electrode.
Adopt this structure, when the liquid of distinguishing electrode position department is the emulsion layer promptly, the liquid that the emulsion layer blow-off valve was located also is the emulsion layer, and the accessible is opened the emulsion layer blow-off valve and is discharged the emulsion layer to prevent the emulsion layer constantly accumulation in the knockout drum.
From the above description of the structure of the present invention, compared with the prior art, the present invention has the following advantages:
1. the invention provides a xylene-brine separation method, which is characterized in that brine and xylene waste liquid in the production process of Polydimethylsilane (PDMS) are collected to a separation tank in a centralized manner and are kept stand for layering, the brine with ethanol dissolved after layering is deposited at the bottom of the separation tank, and xylene is located above the brine; discharging the saline water with the ethanol dissolved in the separation tank to an ethanol distillation device through a saline water discharge valve at the bottom to recover the ethanol; xylene discharges the valve through the xylol of knockout drum side and discharges to the xylene distillation plant in the recovery xylene of distilling, and the ethanol and the xylene of retrieving can be used for Polydimethylsilane (PDMS) production again, adopted promptly with distillation collocation, realized the recovery of xylol and ethanol in the production of Polydimethylsilane (PDMS), reduced Polydimethylsilane (PDMS) manufacturing cost, degree of automation is high, safe and reliable.
2. The xylene-brine separation method provided by the invention has the advantages that the adopted brine discrimination electrode has good pollution resistance and is simple to realize, and the problem that the existing device cannot discriminate the xylene-brine interface is solved.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic diagram of a xylene-brine separation process provided by the present invention;
FIG. 2 is a schematic diagram of a discriminating electrode structure of a xylene-brine separation method provided by the present invention;
FIG. 3 is a schematic diagram of the connection of the control system of the xylene-brine separation method provided by the invention with each valve and the discrimination electrode
In the figure: a separation tank 1; an upper xylene discharge valve 11; an upper discrimination electrode 11 a; a lower xylene discharge valve 12; a discrimination electrode 12 a; a brine discharge valve 13; a lower discrimination electrode 13 a; an emulsion layer discharge valve 14; a waste liquid inlet valve 15; a radar level gauge 15 a; an electrode rod 2; an insulating member 21; an electrode fixing flange 22; a separation tank mounting flange 18; a low-voltage power frequency power supply 23; a voltage dividing inductor 24; a voltage detection table 25; 1x of xylene; 1w of saline; and an emulsion layer 1 r.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
Examples
In a xylene-brine separation method as shown in FIGS. 1 to 3, an upper xylene discharge valve 11 is installed at a separation tank 1; an upper discrimination electrode 11 a; a lower xylene discharge valve 12; the middle discrimination electrode 12 a; a brine discharge valve 13; a lower discrimination electrode 13 a; an emulsion layer discharge valve 14; a waste liquid inlet valve 15; a radar level gauge 15 a.
Waste liquid inlet valve 15, radar level gauge 15a all adorn the top at knockout drum 1, and salt water, the xylene that produce in the production Polydimethylsilane (PDMS) enter into knockout drum 1 through waste liquid inlet valve 15. An upper xylene discharge valve 11 is respectively arranged at the side edge of the separation tank 1 from top to bottom; an upper discrimination electrode 11 a; a lower xylene discharge valve 12; the middle discrimination electrode 12 a; a lower discrimination electrode 13 a; a brine discharge valve 13; the xylene in the separation tank 1 is discharged to the xylene distillation apparatus through an upper xylene discharge valve 11 or a lower xylene discharge valve 12; and xylene dissolved with brine is discharged to the ethanol distillation apparatus through a brine discharge valve 13.
The distinguishing electrode comprises an electrode rod 2; an insulating member 21; an electrode fixing flange 22; a separation tank mounting flange 18; a low-voltage power frequency power supply 23; a voltage dividing inductor 24; and a voltage detection table 25. The electrode rod 2 is fixedly arranged on the separation tank mounting flange 18 through an insulating assembly 21 by an electrode fixing flange 22, and the electrode rod 2 is electrically insulated from the electrode fixing flange 22 and the separation tank mounting flange 18 and keeps a sealed state. The low-voltage power frequency power supply 26 outputs 12-36V alternating-current voltage, one end of the output voltage is grounded, and the output voltage is connected with the separation tank 1; the other end is connected with a voltage division inductor 27 in series and then is connected with the electrode rod 2. The voltage between the electrode rod 2 and the separation tank 1 is measured by a voltage meter 28. The voltage measuring meter 28 feeds back the measured voltage feedback signal 3 to the control system; if the measured voltage is lower than the set low-limit voltage value, the measured voltage is output through a green lamp to indicate that the electrode rod 2 is immersed in the saline water 1 w; if the measured voltage is higher than the set upper limit voltage value, the red light is output to indicate that the central electrode rod 2 is immersed in xylene 1x or exposed in gas; neither indicator light is on, indicating that the central electrode rod 2 is in the emulsion layer 1 r.
In the control system, voltage signals detected by the upper discrimination electrode 11a, the middle discrimination electrode 12a and the lower discrimination electrode 13a and liquid level signals of the radar liquid level meter 15a are all fed back to the control system, and the control system displays the state; the upper xylene discharge valve 11, the lower xylene discharge valve 12, the brine discharge valve 13 and the waste liquid inlet valve 15 are opened or closed through a control system; the control system has a valve opening interlocking function, wherein when the radar liquid level meter 15a reaches a preset high limit liquid level, the control system closes the waste liquid inlet valve 15 and cannot be opened; when the upper discrimination electrode 11a detects saline water or an emulsion layer, the control system closes the upper xylene discharge valve 11 and cannot open the upper xylene discharge valve; when the middle discrimination electrode 12a detects the saline water or the emulsion layer, the control system closes the lower xylene discharge valve 12 and cannot open the lower xylene discharge valve; when the lower discrimination electrode 13a detects an emulsion layer or xylene, the control system closes the brine discharge valve 13 and cannot open; thus, the liquid discharged by the upper xylene discharge valve 11 and the lower xylene discharge valve 12 is xylene, and an emulsion layer and saline water cannot be mixed; the liquid discharged from the brine discharge valve 13 is brine without mixing the emulsion layer and xylene.
The upper xylene discharging valve 11 and the lower xylene discharging valve 12 are positioned at different positions above and below the separation tank 1, and the upper xylene discharging valve 11 or the lower xylene discharging valve 12 can be selected to discharge xylene according to different xylene liquid levels.
The emulsion layer in the separator tank accumulates more and more with prolonged use. The emulsion layer discharge valve 14 is at the same height as the medium discrimination electrode 12a, and when the medium discrimination electrode 12a detects the emulsion layer, the emulsion layer discharge valve 14 can be opened to discharge the emulsion layer.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A xylene-brine separation process, characterized in that it comprises the steps of:
(1) firstly, introducing brine, ethanol and xylene waste liquor generated in the production of Polydimethylsilane (PDMS) into a separation tank for standing;
(2) after standing and layering, discharging the brine with ethanol dissolved in the brine through a brine discharge valve of the separation tank, and simultaneously discharging the dimethylbenzene in the separation tank through a dimethylbenzene discharge valve of the separation tank.
2. The xylene-brine separation process according to claim 1, characterized in that: in the step (2), each discharge valve is provided with a corresponding judging electrode which is used for judging whether the liquid at the position of the discharge valve is saline water or xylene and realizing the interlocking control of the discharge valve so as to prevent the xylene from being discharged from the saline water discharge valve or discharge the saline water from the xylene discharge valve.
3. The xylene-brine separation process according to claim 2, characterized in that: the saline water discharge valve is arranged on the bottom of the separation tank, and a discrimination electrode matched with the saline water discharge valve is arranged near the upper part of the saline water discharge valve.
4. The xylene-brine separation process according to claim 2, characterized in that: a plurality of xylene discharging valves are arranged on the side edge of the separating tank along the length direction of the separating tank, each xylene discharging valve is provided with a distinguishing electrode, and the corresponding distinguishing electrode is arranged near the lower part of the xylene discharging valve.
5. The xylene-brine separation process according to claim 2, characterized in that: and a control system is adopted for linkage control, and the control system can detect and display the judging state of the judging electrode and the opening and closing state of the valve.
6. The xylene-brine separation process according to claim 5, wherein: the discriminating electrode comprises an electrode rod, an insulating assembly, an electrode fixing flange, a separating tank mounting flange, a low-voltage power frequency power supply, a voltage division inductor and a voltage detection meter; the motor rod is fixedly arranged on the mounting flange of the separation tank by the electrode fixing flange through the insulating assembly; the electrode rod is electrically insulated from the electrode fixing flange and the separating tank mounting flange and keeps the sealing property; one end of the output voltage of the low-voltage power frequency power supply is connected with the separating tank and is grounded, and the other end of the low-voltage power frequency power supply is connected with the electrode rod after being connected with the voltage-dividing inductor in series; the voltage detection meter is used for detecting the voltage between the separation tank and the electrode rod of the distinguishing electrode, can measure the voltage to judge whether the liquid at the position where the electrode rod of the distinguishing electrode is located is dimethylbenzene or saline water, and displays the liquid through the indicator lamp and feeds the liquid back to the control system.
7. The xylene-brine separation process of claim 6 wherein: the number of the distinguishing electrodes is 3, and the distinguishing electrodes are an upper distinguishing electrode, a middle distinguishing electrode and a lower distinguishing electrode which are sequentially arranged on one side of the separation tank from top to bottom; the xylene discharge valve is 2, and is respectively an upper xylene discharge valve and a lower xylene discharge valve.
8. The xylene-brine separation process according to claim 1, characterized in that: still be provided with a waste liquid feed valve on the top of knockout drum, waste liquid feed valve is connected with a radar level gauge.
9. The xylene-brine separation process of claim 6 wherein: the knockout drum is kept away from still be connected with one on one side of well judgement electrode and be arranged in the emulsion layer discharge valve of the emulsion layer discharge in the knockout drum, wherein the emulsion layer discharge valve with in judge the electrode equal height.
10. The xylene-brine separation process of claim 6 wherein: and the alternating voltage output by the low-voltage power frequency power supply is 12-36V.
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| CN202010753603.4A CN111991851A (en) | 2020-07-30 | 2020-07-30 | Xylene-brine separation method |
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2020
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| US20130082005A1 (en) * | 2011-09-29 | 2013-04-04 | Gary W. Sams | Method to Process Effluent Brine and Interface Rag from an Oil Dehydration/Desalting System |
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