CN105693585A - System and method for separating N-methylpyrrolidone/chloroform - Google Patents
System and method for separating N-methylpyrrolidone/chloroform Download PDFInfo
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- CN105693585A CN105693585A CN201610221714.4A CN201610221714A CN105693585A CN 105693585 A CN105693585 A CN 105693585A CN 201610221714 A CN201610221714 A CN 201610221714A CN 105693585 A CN105693585 A CN 105693585A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C19/00—Acyclic saturated compounds containing halogen atoms
- C07C19/01—Acyclic saturated compounds containing halogen atoms containing chlorine
- C07C19/03—Chloromethanes
- C07C19/04—Chloroform
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
- C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/24—Oxygen or sulfur atoms
- C07D207/26—2-Pyrrolidones
- C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
- C07D207/267—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to the ring nitrogen atom
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The invention belongs to the technical field of chemical engineering and particularly relates to a system and method for separating N-methylpyrrolidone(NMP)/chloroform. The system for separating N-methylpyrrolidone/chloroform has the advantages that a falling film evaporator, a forced circulation evaporator and a rectifying column are combined organically, supporting technical operating means is also in connection with them, the separated chloroform never deteriorates, and recycled NMP has high purity.
Description
Technical field
The invention belongs to technical field of chemical engineering, particularly to the system and method for one separation N-Methyl pyrrolidone (NMP)/chloroform。
Background technology
N-Methyl pyrrolidone (NMP) is a kind of important industrial chemicals, is widely used as many fields such as polymer solvent, extractant。And NMP is separated from mixture and purification Posterior circle to use be a difficult problem through being commonly encountered in NMP use procedure。It is current industrial conventional a kind of separation method with chloroform by NMP extract and separate from various mixed systems, such as in producing many product process such as para-aramid fiber, polyphenylene sulfide fibre, is all adopt chloroform extraction method to separate NMP。Utilizing the advantage that chloroform extracts NMP is that extraction efficiency is high, and NMP residual quantity is low, but shortcoming is it is also obvious that one is totally can use substantial amounts of chloroform to be extracted as far as possible by NMP, and two is that chloroform is relatively difficult with separating again of NMP。Due to the effumability of chloroform, when high chloroform content, it is difficult to condition of high vacuum degree condition。And improve separation temperature and can cause that chloroform generation side reaction decomposites hydrogen chloride。The generation meeting severe corrosion equipment of hydrogen chloride, and cause that the purity of NMP declines。
The problem decomposing acidifying for chloroform, has two kinds of solutions at present。One is add stabilizer slow down or stop the decomposition of chloroform。Such as the stabilizer of chloroform makes in patent US4980031 of low-molecular-weight amine (such as triethylamine) in E.I.Du Pont Company。But the addition of stabilizer makes separation system more complicated, and stabilizer there is also the risk polluting NMP。Two is pass into enhanced water NMP to separate with chloroform, such as accelerates the elimination of NMP in patent CN101550233A by passing into the mode of steam in NMP/ chloroform system, but follow-up dehydration makes production procedure elongated, and cost raises。In order to improve the vacuum of separation, it is possible to use chloroform is forced sub-cooled by cold-trap, reduce chloroform volatile quantity and improve vacuum, but if having a small amount of water to deposit the risk having again ice blockage condenser or vacuum pipe in case。
Summary of the invention
It is an object of the invention to for the chloroform acidifying occurred in NMP/ chloroform separation process and separation efficiency problem, a kind of system and method separating NMP/ chloroform is proposed, avoid the series of problems that chloroform side reaction brings on the one hand, and the purity of NMP organic efficiency and NMP can be improved。
A kind of system separating N-Methyl pyrrolidone/chloroform of the present invention, including falling-film evaporating unit, forced-circulation evaporation unit, rectification cell and vacuum unit；
Described falling-film evaporating unit includes falling film evaporator, separator I, normal-temperature water condenser I, low-temperature condenser I and chloroform storage tank I；Connect with bottom separator I bottom falling film evaporator；Separator I top has been sequentially communicated normal-temperature water condenser I, low-temperature condenser I and chloroform storage tank I by pipeline；Chloroform storage tank I top connection vacuum unit, bottom connection chloroform collecting；
Described forced-circulation evaporation unit includes preheater, separator II, forced circulation pump, heater, normal-temperature water condenser II, low-temperature condenser II, chloroform storage tank II, discharging pump；Preheater top connects with separator II bottom；Separator II top has been sequentially communicated normal-temperature water condenser II, low-temperature condenser II and chloroform storage tank II by pipeline；Chloroform storage tank I top connection vacuum unit, bottom connection chloroform collecting；Be connected with in turn forced circulation pump and heater bottom separator II by pipeline, heater top is connected with separator II by pipeline；Connect with discharging pump bottom separator II；
Described rectification cell includes reboiler, rectifying column, normal-temperature water condenser III, low-temperature condenser III, chloroform storage tank III, normal-temperature water condenser IV, N-Methyl pyrrolidone storage tank；Rectifying column, normal-temperature water condenser III, low-temperature condenser III and chloroform storage tank III are sequentially communicated formation Guan Bi pipeline and chloroform storage tank III top connects vacuum unit, bottom connection chloroform collecting；Rectifying column connects formation Guan Bi pipeline with reboiler；Normal-temperature water condenser IV and N-Methyl pyrrolidone storage tank it is connected with in turn in the middle part of rectifying column and by pipeline, N-Methyl pyrrolidone storage tank top connection vacuum unit, bottom connection N-Methyl pyrrolidone collecting；
Preheater is connected with falling film evaporator and separator I by pipeline；Pipeline connection is passed through bottom rectifier and separator II。
In a kind of system separating N-Methyl pyrrolidone/chloroform of the present invention, there is filler on separator I and separator II top, to improve gas-liquid separation effect, reduce the amount of the NMP carried secretly away by chloroform vapor；Described rectifying column is plate column, and described reboiler is vertical or horizontal reboiler。It addition, system of the present invention is additionally provided with the measuring instruments such as relevant valve, temperature, pressure transducer and liquidometer, it is the conventional design of this area。
The feature of native system is: vaporizer two kinds different combines and uses, and operating flexibility is big, and separation efficiency is high, and is cascade raising temperature separation chloroform, and acidifying spoilage problems will not occur chloroform, and capacity usage ratio is high。Being NMP and chloroform for key component, the another system containing a small amount of other components (such as water), native system is still suitable for。
Applying the described system separating N-Methyl pyrrolidone/chloroform of the present invention, present invention also offers the method separating N-Methyl pyrrolidone/chloroform accordingly, it concretely comprises the following steps:
(1) chloroform content is that 30-99%N-methyl pyrrolidone/chloroform mixed liquor enters falling film evaporator, in control falling film evaporator and separator I, temperature of charge is less than 80 DEG C, vacuum is at below-0.06MPa, controlling capacity of returns is the 5-20% of produced quantity, controls chloroform concentration in the N-Methyl pyrrolidone of extraction/chloroform mixed liquor at 20-50%；In order to ensure vacuum, chloroform temperature is controlled below 20 DEG C by the chloroform of separator I (2) extraction by condensed in two stages；
(2) N-Methyl pyrrolidone of falling-film evaporating unit extraction/chloroform mixed liquor is heated to 60-100 DEG C by preheater, part chloroform is removed subsequently into separator II, leftover materials pump into heater through forced circulation pump, and material enters back into separator II and separates after heating at this；So chloroform content is repeatedly further decreased to 1-20% by circulation；This process control temperature of charge is less than 120 DEG C, and vacuum is at below-0.085MPa；In order to ensure vacuum, chloroform temperature is controlled below 10 DEG C by the chloroform of separator II extraction by condensed in two stages；In this process, in extraction material, chloroform concentration is by controlling produced quantity, or cycle-index and technological parameter (temperature, vacuum) regulate and control, if namely chloroform content exceeds standard in material, then can reduce produced quantity, or increase cycle-index, or raising temperature of charge, or improve vacuum, so that chloroform content in the material of extraction is controlled in scope of design；
(3) N-Methyl pyrrolidone of forced-circulation evaporation unit extraction/chloroform mixed liquor is pumped directly into rectifying column, at the remaining chloroform of rectifying column overhead extraction, extraction NMP in the middle part of tower；The temperature of reboiler is less than 140 DEG C, and within rectifying column tower top temperature controls 100 DEG C, top vacuum degree is at below-0.09MPa；Chloroform temperature is controlled below 10 DEG C by the chloroform of rectifying column overhead extraction by condensed in two stages；The NMP of extraction controls within 40 DEG C through condensation temperature。
Adopting method of the present invention, the NMP purity of final rectifying column extraction can up to 99.99%。
In sum, the present invention utilizes a falling film evaporator will to remove (slightly steaming) under the chloroform low temperature coarse vacuum in the NMP/ chloroform mixed liquor of high chloroform content, then under higher temperatures and high vacuum, chloroform (essence is steamed) is removed further with a forced-circulation evaporator again, finally enter rectifying column under high temperature fine vacuum, remove remaining a small amount of chloroform, and rectification goes out high purity N MP (rectification)。Utilize this system and auxiliary in corresponding manner, it is possible to being prevented effectively from the acidifying problem of NMP/ chloroform separation process, energy consumption is low, and separation efficiency is high, and is conducive to keeping the purity of NMP, thus improving NMP to reclaim the efficiency and quality that use。The method have simple to operate, cost is low and safety advantages of higher。
Accompanying drawing explanation
Fig. 1 is the structural representation of the system of separation N-Methyl pyrrolidone (NMP)/chloroform of the present invention；
In figure: 1, falling film evaporator, 2, separator I, 3, normal-temperature water condenser I, 4, low-temperature condenser I, 5, chloroform storage tank I, 6, preheater, 7, separator II, 8, forced circulation pump, 9, heater, 10, normal-temperature water condenser II, 11, low-temperature condenser II, 12, chloroform storage tank II, 13, discharging pump, 14, reboiler, 15, rectifying column, 16, normal-temperature water condenser III, 17, low-temperature condenser III, 18, chloroform storage tank III, 19, normal-temperature water condenser IV, 20, N-Methyl pyrrolidone storage tank。
Detailed description of the invention
Below by example, the present invention is further described, but content not thereby limiting the invention。
Embodiment 1
A kind of system separating N-Methyl pyrrolidone/chloroform, this system includes falling-film evaporating unit, forced-circulation evaporation unit, rectification cell and vacuum unit；
Described falling-film evaporating unit includes falling film evaporator 1, separator I2, normal-temperature water condenser I3, low-temperature condenser I4 and chloroform storage tank I5；Connect with bottom separator I2 bottom falling film evaporator 1；Separator I2 top has been sequentially communicated normal-temperature water condenser I3, low-temperature condenser I4 and chloroform storage tank I5 by pipeline；Chloroform storage tank I5 top connection vacuum unit, bottom connection chloroform collecting；
Described forced-circulation evaporation unit includes preheater 6, separator II7, forced circulation pump 8, heater 9, normal-temperature water condenser II10, low-temperature condenser II11, chloroform storage tank II12, discharging pump 13；Preheater 6 top connects with separator II7 bottom；Separator II7 top has been sequentially communicated normal-temperature water condenser II10, low-temperature condenser II11 and chloroform storage tank II12 by pipeline；Chloroform storage tank II12 top connection vacuum unit, bottom connection chloroform collecting；Be connected with in turn forced circulation pump 8 and heater 9 bottom separator II7 by pipeline, heater 9 top is connected with separator II7 by pipeline；Connect with discharging pump 13 bottom separator II7；
Described rectification cell includes reboiler 14, rectifying column 15, normal-temperature water condenser III16, low-temperature condenser III17, chloroform storage tank III18, normal-temperature water condenser IV19, N-Methyl pyrrolidone storage tank 20；Rectifying column 15, normal-temperature water condenser III16, low-temperature condenser III17 and chloroform storage tank III18 are sequentially communicated formation Guan Bi pipeline and chloroform storage tank III18 top connects vacuum unit, bottom connection chloroform collecting；Rectifying column 15 connects formation Guan Bi pipeline with reboiler 14；Normal-temperature water condenser IV19 and N-Methyl pyrrolidone storage tank 20 it is connected with in turn in the middle part of rectifying column 15 and by pipeline, N-Methyl pyrrolidone storage tank 20 top connection vacuum unit, bottom connection N-Methyl pyrrolidone collecting；
Preheater 6 is connected with falling film evaporator 1 and separator I2 by pipeline；Pipeline connection is passed through bottom rectifying column 15 top and separator II7。
The method applying the above-mentioned system separation N-Methyl pyrrolidone/chloroform separating N-Methyl pyrrolidone/chloroform, it concretely comprises the following steps:
Chloroform content 70%, the mixed liquor of NMP content 30% enters falling film evaporator 1 with the flow of 5.5 tons/h, and in control falling film evaporator 1 and separator I2, temperature of charge is at 60 DEG C, and vacuum degree control is at-0.08MPa。Temperature is controlled at 15 DEG C by the chloroform of extraction through condensed in two stages。By controlling capacity of returns, chloroform concentration in the NMP/ chloroform mixed liquor of extraction is controlled 30%；Capacity of returns is the 5% of produced quantity。
By preheater, the NMP/ chloroform mixed liquor of falling-film evaporating unit extraction being heated to 80 DEG C, removes part chloroform subsequently into separator II7, leftover materials pump into heater 9 through forced circulation pump 8, and material enters back into separator II7 and separates after heating at this。So chloroform content is further decreased to 5% by circulation。Controlling temperature of charge 100 DEG C, vacuum is at-0.085MPa。Chloroform temperature is controlled at 5 DEG C by the chloroform of extraction by condensed in two stages。
Material after concentration is up to standard is pumped directly into rectifying column 15。At the rectifying column 15 remaining chloroform of overhead extraction, extraction NMP in the middle part of tower。The temperature of reboiler 14 controls at 120 DEG C, and tower top temperature is by regulating control of reflux ratio at 80 DEG C, and top vacuum degree controls at-0.094MPa。In order to ensure vacuum, chloroform temperature is controlled at 5 DEG C by the chloroform of overhead extraction by condensed in two stages。The NMP of extraction controls at 20 DEG C through condensation temperature。Above-mentioned technical process can ensure that chloroform not acidifying in During Process of Long-term Operation, and the NMP purity of rectifying column extraction is 99.96%。
Embodiment 2
A kind of described in this embodiment separates the system of N-Methyl pyrrolidone/chloroform with embodiment 1。
The method applying the above-mentioned system separation N-Methyl pyrrolidone/chloroform separating N-Methyl pyrrolidone/chloroform, it concretely comprises the following steps:
Chloroform content 50%, the mixed liquor of NMP content 50% enters falling film evaporator with the flow of 5.5 tons/h, and in control falling film evaporator and separator I, temperature of charge is at about 80 DEG C, and vacuum degree control is at-0.08MPa。Temperature is controlled at 15 DEG C by the chloroform of extraction through condensed in two stages。By controlling capacity of returns, chloroform concentration in the NMP/ chloroform mixed liquor of extraction is controlled 20%。Capacity of returns is the 20% of produced quantity。
By preheater, the NMP/ chloroform mixed liquor of falling film evaporator extraction being heated to 90 DEG C, removes part chloroform subsequently into separator II, leftover materials pump into heater through forced circulation pump, and material enters back into separator II and separates after heating at this。So chloroform content is further decreased to 3% by circulation。Controlling temperature of charge 100 DEG C, vacuum is at-0.085MPa。Chloroform temperature is controlled at 5 DEG C by the chloroform of extraction by condensed in two stages。
Material after concentration is up to standard is pumped directly into rectifying column。At the remaining chloroform of rectifying column overhead extraction, extraction NMP in the middle part of tower。The temperature of reboiler controls at 130 DEG C, and tower top temperature is by regulating control of reflux ratio at 70 DEG C, and top vacuum degree controls at-0.096MPa。In order to ensure vacuum, chloroform temperature is controlled at 0 DEG C by the chloroform of overhead extraction by condensed in two stages。The NMP of extraction controls at 10 DEG C through condensation temperature。Above-mentioned technical process can ensure that chloroform not acidifying in During Process of Long-term Operation, and the NMP purity of rectifying column extraction is 99.99%。
Embodiment 3
A kind of described in this embodiment separates the system of N-Methyl pyrrolidone/chloroform with embodiment 1。
The method applying the above-mentioned system separation N-Methyl pyrrolidone/chloroform separating N-Methyl pyrrolidone/chloroform, it concretely comprises the following steps:
Chloroform content 60%, NMP content 35%, the mixed liquor of water content 5% enters falling film evaporator with the flow of 5.5 tons/h, and in control falling film evaporator and separator I, temperature of charge is at 70 DEG C, and vacuum degree control is at-0.083MPa。Most water (about 90%) is carried over along with chloroform, and temperature is controlled at 20 DEG C by the chloroform/water of extraction through condensed in two stages。By controlling capacity of returns, chloroform concentration in the NMP/ chloroform mixed liquor of extraction is controlled 40%。Capacity of returns is the 15% of produced quantity。
By preheater, the NMP/ chloroform mixed liquor of falling film evaporator extraction being heated to 80 DEG C, removes part chloroform subsequently into separator II, leftover materials pump into heater through forced circulation pump, and material enters back into separator II and separates after heating at this。So chloroform content is further decreased to 3% by circulation。Controlling temperature of charge 110 DEG C, vacuum is at-0.085MPa。Chloroform temperature is controlled at 5 DEG C by the chloroform of extraction by condensed in two stages。
Material after concentration is up to standard is pumped directly into rectifying column。At the remaining chloroform of rectifying column overhead extraction, extraction NMP in the middle part of tower。The temperature of the reboiler of rectifying column controls at 120 DEG C, and tower top temperature is by regulating control of reflux ratio at 80 DEG C, and top vacuum degree controls at-0.095MPa。In order to ensure vacuum, chloroform temperature is controlled at 5 DEG C by the chloroform of overhead extraction by condensed in two stages。The NMP of extraction controls at 30 DEG C through condensation temperature。Above-mentioned technical process can ensure that chloroform not acidifying in During Process of Long-term Operation, and the NMP purity of rectifying column extraction is 99.95%。
Claims (2)
1. the system separating N-Methyl pyrrolidone/chloroform, it is characterised in that: this system includes falling-film evaporating unit, forced-circulation evaporation unit, rectification cell and vacuum unit；
Described falling-film evaporating unit includes falling film evaporator (1), separator I (2), normal-temperature water condenser I (3), low-temperature condenser I (4) and chloroform storage tank I (5)；Falling film evaporator (1) bottom connects with separator I (2) bottom；Separator I (2) top has been sequentially communicated normal-temperature water condenser I (3), low-temperature condenser I (4) and chloroform storage tank I (5) by pipeline；Chloroform storage tank I (5) top connection vacuum unit, bottom connection chloroform collecting；
Described forced-circulation evaporation unit includes preheater (6), separator II (7), forced circulation pump (8), heater (9), normal-temperature water condenser II (10), low-temperature condenser II (11), chloroform storage tank II (12), discharging pump (13)；Preheater (6) top connects with separator II (7) bottom；Separator II (7) top has been sequentially communicated normal-temperature water condenser II (10), low-temperature condenser II (11) and chloroform storage tank II (12) by pipeline；Chloroform storage tank II (12) top connection vacuum unit, bottom connection chloroform collecting；Separator II (7) bottom is connected with forced circulation pump (8) and heater (9) in turn by pipeline, and heater (9) top is connected with separator II (7) by pipeline；Separator II (7) bottom connects with discharging pump (13)；
Described rectification cell includes reboiler (14), rectifying column (15), normal-temperature water condenser III (16), low-temperature condenser III (17), chloroform storage tank III (18), normal-temperature water condenser IV (19), N-Methyl pyrrolidone storage tank (20)；Rectifying column (15), normal-temperature water condenser III (16), low-temperature condenser III (17) is sequentially communicated formation Guan Bi pipeline with chloroform storage tank III (18) and chloroform storage tank III (18) top connects vacuum unit, bottom connection chloroform collecting；Rectifying column (15) connects formation Guan Bi pipeline with reboiler (14)；Normal-temperature water condenser IV (19) and N-Methyl pyrrolidone storage tank (20) it is connected with in turn in the middle part of rectifying column (15) and by pipeline, N-Methyl pyrrolidone storage tank (20) top connection vacuum unit, bottom connection N-Methyl pyrrolidone collecting；
Preheater (6) is connected with falling film evaporator (1) and separator I (2) by pipeline；Pipeline connection is passed through with separator II (7) bottom in rectifying column (15) top。
2. the method for the system separation N-Methyl pyrrolidone/chloroform separating N-Methyl pyrrolidone/chloroform described in application claim 1, it is characterised in that: it concretely comprises the following steps:
(1) chloroform content is that 30-99%N-methyl pyrrolidone/chloroform mixed liquor enters falling film evaporator (1), in control falling film evaporator (1) and separator I (2), temperature of charge is less than 80 DEG C, vacuum is at below-0.06MPa, controlling capacity of returns is the 5-20% of produced quantity, controls chloroform concentration in the N-Methyl pyrrolidone of extraction/chloroform mixed liquor at 20-50%；Chloroform temperature is controlled below 20 DEG C by the chloroform of separator I (2) extraction by condensed in two stages；
(2) N-Methyl pyrrolidone of falling-film evaporating unit extraction/chloroform mixed liquor is heated to 60-100 DEG C by preheater, part chloroform is removed subsequently into separator II (7), leftover materials pump into heater (9) through forced circulation pump (8), and material enters back into separator II (7) and separates after heating at this；So chloroform content is repeatedly further decreased to 1-20% by circulation；This process control temperature of charge is less than 120 DEG C, and vacuum is at below-0.085MPa；Chloroform temperature is controlled below 10 DEG C by the chloroform of separator II (7) extraction by condensed in two stages；
(3) N-Methyl pyrrolidone of forced-circulation evaporation unit extraction/chloroform mixed liquor is pumped directly into rectifying column (15), at the remaining chloroform of rectifying column (15) overhead extraction, extraction NMP in the middle part of tower；The temperature of reboiler (14) is less than 140 DEG C, and within rectifying column (15) tower top temperature controls 100 DEG C, top vacuum degree is at below-0.09MPa；Chloroform temperature is controlled below 10 DEG C by the chloroform of rectifying column (15) overhead extraction by condensed in two stages；The NMP of extraction controls within 40 DEG C through condensation temperature。
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| CN201610221714.4A CN105693585B (en) | 2016-04-11 | 2016-04-11 | A kind of separation N-Methyl pyrrolidone/chloroform system and method |
| PCT/CN2017/073851 WO2017177763A1 (en) | 2016-04-11 | 2017-02-17 | System and method for separating n-methyl-2-pyrrolidone/chloroform |
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| WO2017177763A1 (en) | 2017-10-19 |
| CN105693585B (en) | 2018-11-20 |
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