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CN112354205A - Multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources - Google Patents

Multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources Download PDF

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Publication number
CN112354205A
CN112354205A CN202011203660.1A CN202011203660A CN112354205A CN 112354205 A CN112354205 A CN 112354205A CN 202011203660 A CN202011203660 A CN 202011203660A CN 112354205 A CN112354205 A CN 112354205A
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China
Prior art keywords
rectifying tower
tank
rectification
pump
rectifying
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Inventor
宋太沧
唐斌
施健
卞艳飞
仲超
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Yabang Green Process And New Materials Research Institute Nanjing Co ltd
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Yabang Green Process And New Materials Research Institute Nanjing Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/143Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B01D3/146Multiple effect distillation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/10Vacuum distillation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/36Azeotropic distillation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/40Extractive distillation

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention relates to a multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources, belonging to the technical field of chemical rectification; the invention is composed of a first rectification system, a second rectification system and a third rectification system, and can realize conventional multi-tower atmospheric and vacuum rectification and special rectification through simple valve switching and operation pressure control: azeotropic distillation and extractive distillation can complete the recovery tasks of various waste organic solvents; the waste organic solvent is separated and purified by multistage rectification, and each rectifying tower is provided with four side discharge ports, so that the characteristic of complex components of the waste organic solvent is combined, the required components in the waste organic solvent can be recovered to the maximum extent, and the purity of the target components is ensured; under the condition of changing experimental tasks, the rectification experimental system has quick response and can quickly adjust the process flow so as to meet the experimental requirements of different processes.

Description

Multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources
Technical Field
The invention relates to the technical field of chemical rectification, in particular to a multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources.
Background
The organic solvent is widely used in the production process of industries such as coating, printing, automobile, electronics, pharmacy and the like, can be used as a cleaning agent, a diluting agent and an extracting agent, and can also be used as a raw material or an intermediate for chemical synthesis. The organic solvent generally generates waste organic solvent after being used, is often characterized by inflammability, fat solubility, volatility, toxicity and the like, and has strong harmfulness to human bodies and environment. Therefore, it is important to treat the waste organic solvent to be harmless or to recycle it. The treatment technology is different according to the specific situation of the waste organic solvent, and is mainly divided into three types: the waste organic solvent with high purity and single component or high relative volatility of each component is recycled mainly by adopting a distillation mode; waste organic solvent which is difficult to rectify and has more impurities or distillation residue after rectification is treated by adopting incineration and a cement kiln in a synergic way; solid semi-solid waste solvent sludge is safely buried. With the increasing severity of the problems of environmental pollution and resource waste, more and more enterprises recycle the waste organic solvent, thereby achieving the purposes of effectively utilizing resources, reducing environmental pollution and lowering production cost. The waste organic solvent is recycled mainly by means of a rectification technology, and components of the waste organic solvent are separated by means of the rectification technology, so that the purpose of refining and purifying target components is achieved, and recycling of the waste organic solvent is achieved to the maximum extent.
The waste organic solvent is generally a mixed solvent, the production links are various, the compositions of the waste organic solvents from different sources are different, and recyclable target components are different. Therefore, specific processes need to be designed for the waste organic solvents from different sources to meet the requirements of recycling the waste organic solvents. The process design of the waste organic solvent is required to be established on the basis of experiments, and for the specific waste organic solvent, the optimal process flow can be determined by experimental verification of different process flows and comparison of the advantages and disadvantages of different processes; on the other hand, the recovery process generally differs for different sources of waste organic solvents. Therefore, it is particularly important to develop a multifunctional rectification experimental system, which can flexibly change the process flow of the rectification system according to the specific situation of the waste organic solvent, and perform experimental verification on different process flows.
Disclosure of Invention
The technical problems actually solved by the invention are as follows: aiming at the experimental requirements of different processes for recycling the waste organic solvent, only a rectification experimental system with a single process flow is provided, and the maximum separation and purification of target components in the waste organic solvent are difficult to realize. The invention provides a multifunctional rectification experimental system for comprehensively utilizing waste organic solvent resources, which is used for verifying a waste organic solvent recovery process by switching and adjusting a process route of a rectification system through a valve under the conditions of normal pressure and reduced pressure according to experimental requirements of different separation tasks and arranging a plurality of side line discharge ports in each tower.
A multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources comprises: the device comprises a first rectification system, a second rectification system and a third rectification system.
The first rectification system comprises:
a raw material tank a for storing the waste organic solvent to be separated and purified;
the feeding pump a is connected with the raw material tank a and is used for conveying the waste organic solvent in the raw material tank a;
the preheater a is connected with the feeding pump a and is used for heating the waste organic solvent;
the rectifying tower a is used for carrying out primary separation on each component of the waste organic solvent;
the reboiler a is arranged at the bottom of the rectifying tower a and used for heating and gasifying the waste organic solvent in the rectifying tower a;
the condenser a is connected with the top of the rectifying tower a and is used for condensing the gas-phase components distilled from the top of the rectifying tower a;
the cooler a1 is connected with a side line discharge port at the upper part of the rectifying tower a through a valve and is used for cooling the side line extracted liquid at the top of the rectifying tower a;
the cooler a2 is connected with a side line discharge port at the lower part of the rectifying tower a through a valve and is used for cooling the side line extracted liquid at the top of the rectifying tower a;
the kettle bottom discharge pump a is connected with the reboiler a and is used for outputting the bottom liquid of the rectifying tower a;
the cooler a3 is connected with the reboiler a through a kettle bottom discharge pump a and is used for cooling the kettle bottom liquid of the rectifying tower a;
the reflux ratio controller a is connected with the condenser a and the top of the rectifying tower a and is used for distributing condensate of the condenser a to divide the condensate into reflux liquid and distillate;
a receiving tank a1, a receiving tank a2 and a receiving tank a3 which are connected with the reflux ratio controller a through valves and are used for receiving distillate of the reflux ratio controller a;
a receiving tank a4 connected with the cooler a1 through a valve for receiving the cooling liquid of the cooler a 1;
a receiving tank a5 connected with the cooler a2 through a valve for receiving the cooling liquid of the cooler a 2;
the receiving tank a6 is connected with the kettle bottom discharge pump a through a valve and is used for receiving the cooling liquid of the cooler a 3;
the discharge pump a1, the discharge pump a2, the discharge pump a3 and the discharge pump a4 are respectively connected with the receiving tank a3, the receiving tank a4, the receiving tank a5 and the receiving tank a6 through valves and are used for outputting feed liquid in the receiving tank;
the vacuum pump a and the vacuum buffer tank a form a vacuum system for providing negative pressure of the first rectification system.
The second rectification system comprises:
the raw material tank b is connected with a discharge pump a1, a discharge pump a2, a discharge pump a3 and a discharge pump a4 of the first rectification system and is used for storing the waste organic solvent to be separated and purified from the first rectification system;
the feeding pump b is connected with the raw material tank b through a valve and is used for conveying the waste organic solvent in the raw material tank b;
the preheater b is connected with the feed pump b and is used for heating the feed liquid from the feed tank b;
the extractant tank b is connected with a discharge pump c of the third rectification system and used for storing an extractant;
the extractant feeding pump b is connected with the extractant tank b and is used for conveying the extractant in the extractant tank b;
an extractant preheater b for heating extractant from storage;
the rectifying tower b is used for carrying out secondary separation on the waste organic solvent;
the reboiler b is positioned at the bottom of the rectifying tower b and used for heating and gasifying the waste organic solvent in the rectifying tower b;
the condenser b is connected with the top of the rectifying tower b and is used for condensing gas-phase components distilled out of the top of the rectifying tower b;
the cooler b1 is connected with a side line discharge port at the upper part of the rectifying tower b through a valve and is used for cooling the side line extracted liquid at the top of the rectifying tower b;
the cooler b2 is connected with a side line discharge port at the lower part of the rectifying tower b through a valve and is used for cooling the side line extracted liquid at the top of the rectifying tower b;
the kettle bottom discharge pump b is connected with the reboiler b and used for outputting tower bottom liquid of the rectifying tower b;
the cooler b3 is connected with the reboiler b through a kettle bottom discharge pump b and is used for cooling the kettle bottom liquid of the rectifying tower b;
the reflux ratio controller b is connected with the condenser b and the top of the rectifying tower b through a valve and is used for distributing condensate of the condenser b to divide the condensate into reflux liquid and distillate;
the delayer b is connected with the condenser b and the top of the rectifying tower b through a valve and is used for delaminating the heterogeneous condensate of the condenser b so that the condensate is divided into an upper layer light liquid and a lower layer heavy liquid;
the entrainer tank b is used for storing an entrainer;
the entrainer feeding pump b is connected with the entrainer tank b and is used for feeding the entrainer in the entrainer tank b into the delayer b;
the upper-layer discharging pump b is connected with the delayer b and used for sending the light liquid on the upper layer in the delayer b into the buffer tank b; meanwhile, the buffer tank b is connected with an upper discharge pump c of the third rectification system and receives light liquid on the upper layer of a delayer c of the third rectification system;
the lower-layer discharge pump b is connected with the delayer b and used for conveying the heavy liquid of the lower layer in the delayer b into a raw material tank c of a third rectification system;
the reflux pump b is connected with the buffer tank b and used for feeding the feed liquid in the buffer tank b to the top of the rectifying tower b;
a receiving tank b1, a receiving tank b2 and a receiving tank b3 which are connected with the reflux ratio controller b through valves and are used for receiving the distillate of the reflux ratio controller b;
a receiving tank b4 connected with the cooler b1 through a valve for receiving the cooling liquid of the cooler b 1;
a receiving tank b5 connected with the cooler b2 through a valve for receiving the cooling liquid of the cooler b 2;
the receiving tank b6 is connected with the kettle bottom discharge pump b through a valve and is used for receiving the cooling liquid of the cooler b 3;
the discharge pump b1, the discharge pump b2, the discharge pump b3 and the discharge pump b4 are respectively connected with the receiving tank b3, the receiving tank b4, the receiving tank b5 and the receiving tank b6 through valves and are used for outputting feed liquid in the receiving tank;
and the vacuum pump b and the vacuum buffer tank b form a vacuum system for providing negative pressure of the second rectification system.
The third rectification system comprises:
the raw material tank c is connected with a discharge pump b1, a discharge pump b2, a discharge pump b3 and a discharge pump b4 of the second rectification system and is used for storing the waste organic solvent to be separated and purified from the second rectification system;
the feeding pump c is connected with the raw material tank c through a valve and is used for conveying the waste organic solvent in the raw material tank c;
the preheater c is connected with the feed pump c and is used for heating the feed liquid from the feed tank c;
the rectifying tower c is used for carrying out secondary separation on the waste organic solvent;
the reboiler c is positioned at the bottom of the rectifying tower c and used for heating and gasifying the waste organic solvent in the rectifying tower c;
the condenser c is connected with the top of the rectifying tower c and is used for condensing gas-phase components distilled out of the top of the rectifying tower c;
the cooler c1 is connected with a side line discharge port at the upper part of the rectifying tower c through a valve and is used for cooling the side line extracted liquid at the top of the rectifying tower c;
the cooler c2 is connected with a side line discharge port at the lower part of the rectifying tower c through a valve and is used for cooling the side line extracted liquid at the top of the rectifying tower c;
the kettle bottom discharge pump c is connected with the reboiler c and used for outputting the bottom liquid of the rectifying tower c;
the cooler c3 is connected with the reboiler c through a kettle bottom discharge pump c and is used for cooling the kettle bottom liquid of the rectifying tower c;
the reflux ratio controller c is connected with the condenser c and the top of the rectifying tower c through valves and is used for distributing condensate of the condenser c to divide the condensate into reflux liquid and distillate;
the delayer c is connected with the condenser c and the top of the rectifying tower c through valves and is used for delaminating the heterogeneous condensate of the condenser c so that the condensate is divided into an upper layer light liquid and a lower layer heavy liquid;
the upper discharge pump c is connected with the delayer c and the second rectification system buffer tank c and is used for sending the light liquid on the upper layer in the delayer c into the buffer tank c of the second rectification system;
the lower layer discharge pump c is connected with the delayer c and the top of the rectifying tower c and is used for sending the heavy liquid of the lower layer in the delayer b into the rectifying tower c of the third rectifying system;
a receiving tank c3-1, a receiving tank c3-2 and a receiving tank c3-3 which are connected with the reflux ratio controller c through valves and used for receiving the distillate of the reflux ratio controller c;
a receiving tank c1-1 connected with the cooler c1 through a valve for receiving the cooling liquid of the cooler c 1;
a receiving tank c1-2 connected with the cooler c2 through a valve for receiving the cooling liquid of the cooler c 2;
the receiving tank c2 is connected with the kettle bottom discharge pump c through a valve and is used for receiving the cooling liquid of the cooler c 3;
the discharge pump c is connected with the receiving tank c2 and the second rectification system extractant tank b through valves, and feeds the feed liquid in the receiving tank c2 into the second rectification system extractant tank b;
and the vacuum pump c and the vacuum buffer tank c form a vacuum system for providing negative pressure of the third rectification system.
The rectifying tower a is provided with four feed inlets which are respectively positioned at 3/8, 1/2, 5/8 and a reboiler a from top to bottom of the rectifying tower a body;
the rectifying tower b is provided with four feed inlets which are respectively positioned at 3/8, 1/2, 5/8 and a reboiler b from top to bottom of the rectifying tower b;
the rectifying tower c is provided with four feed inlets which are respectively positioned at 3/8, 1/2, 5/8 and a reboiler c from top to bottom of the rectifying tower c;
the rectifying tower a is provided with four side line discharge ports which are respectively positioned at 1/8, 1/4, 3/4 and 7/8 from top to bottom of the rectifying tower a body;
the rectifying tower b is provided with four side line discharge ports which are respectively positioned at 1/8, 1/4, 3/4 and 7/8 from top to bottom of a tower body of the rectifying tower b;
the rectifying tower c is provided with four side line discharge ports which are respectively positioned at 1/8, 1/4, 3/4 and 7/8 from top to bottom of a tower body of the rectifying tower c;
the rectifying tower b is provided with two extractant inlets which are respectively positioned at 1/8 and 1/4 from top to bottom of the rectifying tower b;
a multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources comprises a first rectification system, a second rectification system and a third rectification system which are sequentially connected through pipelines; the first rectifying system comprises a raw material tank a, a preheater a, a rectifying tower a, a reboiler a, a cooler a, a receiving tank a, a discharge pump a and a first rectifying tower top system; the bottom end of the rectifying tower a is provided with a reboiler a, the raw material tank a is connected with a preheater a through a feed pump a, one end of the preheater a is connected with the reboiler a, and the other end of the preheater a is connected with the rectifying tower a; the rectifying tower a is sequentially connected with a receiving tank a, a discharge pump a and a second rectifying system through a cooler a; the reboiler a is sequentially connected with the cooler a, the receiving tank a, the discharge pump a and the second rectifying system through the kettle bottom discharge pump a, and the top end of the rectifying tower a is connected with the first rectifying tower top system.
Furthermore, the first rectifying tower top system comprises a condenser a, a reflux ratio controller a, a receiving tank a and a discharge pump a, the top end of the rectifying tower a is connected with the reflux ratio controller a through the condenser a, one end of the reflux ratio controller a is connected with the top end of the rectifying tower a, and the other end of the reflux ratio controller a is sequentially connected with the discharge pump a and the second rectifying system through the receiving tank a.
Furthermore, the first rectification system also comprises a first vacuum system, the first vacuum system comprises a vacuum pump a and a vacuum buffer tank a, the vacuum pump a is connected with the vacuum buffer tank a, one end of the vacuum buffer tank a is connected with the condenser a, and the other end of the vacuum buffer tank a is connected with the receiving tank a.
Further, the second rectification system comprises a raw material tank b, a preheater b, a rectification tower b, a reboiler b, a cooler b, a receiving tank b, a discharge pump b, an extractant tank b and a second rectification tower top system; a reboiler b is arranged at the bottom end of the rectifying tower b, one end of the raw material tank b is connected with the first rectifying system, the other end of the raw material tank b is connected with the preheater b through a feed pump b, one end of the preheater b is connected with the reboiler b, and the other end of the preheater b is connected with the rectifying tower b; the rectifying tower b is sequentially connected with a receiving tank b, a discharge pump b and a third rectifying system through a cooler b; the reboiler b is sequentially connected with the cooler b, the receiving tank b, the discharge pump b and the third rectification system through a kettle bottom discharge pump b; one end of the extractant tank b is connected with the third rectification system, and the other end of the extractant tank b is sequentially connected with the extractant preheater b and the rectification tower b through an extractant feeding pump b; the top end of the rectifying tower b is connected with a second rectifying tower top system.
Further, the second rectifying tower top system comprises a buffer tank b, an upper-layer discharging pump b, a delayer b, a discharging pump b, a condenser b, a reflux ratio controller b, a receiving tank b, an entrainer tank b and a lower-layer discharging pump b, wherein the top of the rectifying tower b is connected with the condenser b, one end of the condenser b is connected with the top of the rectifying tower b through the reflux ratio controller b, the other end of the condenser b is connected with the delayer b, one end of the delayer b is connected with a third rectifying system through the lower-layer discharging pump b, the other end of the delayer b is connected with the buffer tank b through the upper-layer discharging pump b, one end of the buffer tank b is connected with the third rectifying system, and the other end of the buffer tank b is connected with the top of the rectifying tower b through the reflux pump b; the entrainer tank b is connected with the delayer b through an entrainer feeding pump b; the reflux ratio controller b is connected with the discharge pump b and the third rectification system in sequence through the receiving tank b.
Furthermore, the second rectification system also comprises a second vacuum system, the second vacuum system comprises a vacuum pump b and a vacuum buffer tank b, the vacuum pump b is connected with the vacuum buffer tank b, one end of the vacuum buffer tank b is connected with a condenser b, and the other end of the vacuum buffer tank b is respectively connected with the delayer b and the receiving tank b.
Further, the third rectifying system comprises a raw material tank c, a preheater c, a rectifying tower c, a reboiler c, a cooler c, a receiving tank c1, a receiving tank c2, a discharge pump c and a first rectifying tower top system; a reboiler c is arranged at the bottom end of the rectifying tower c, one end of the raw material tank c is connected with the second rectifying system, the other end of the raw material tank c is connected with the preheater c through a feed pump c, one end of the preheater c is connected with the reboiler c, and the other end of the preheater c is connected with the rectifying tower c; the rectifying tower c is connected with a receiving tank c1 through a cooler c; the reboiler c is connected with the cooler c, the receiving tank c2, the discharge pump c and the second rectifying system in sequence through the kettle bottom discharge pump c, and the top end of the rectifying tower c is connected with the first rectifying tower top system.
Further, the tower top system of the third rectifying tower comprises a delayer c, a condenser c, a reflux ratio controller c, a receiving tank c3, an upper-layer discharging pump c and a lower-layer discharging pump c, wherein the tower top of the rectifying tower c is connected with the condenser c, one end of the condenser c is connected with the tower top of the rectifying tower c through the reflux ratio controller c, the other end of the condenser c is connected with the delayer c, one end of the delayer c is connected with the top end of the rectifying tower c through the lower-layer discharging pump c, and the other end of the rectifying tower c is connected with the second rectifying system through the upper-layer discharging pump c; the reflux ratio controller c is connected to the receiver tank c 3.
Further, the third rectification system also comprises a third vacuum system, the third vacuum system comprises a vacuum pump c and a vacuum buffer tank c, the vacuum pump c is connected with the vacuum buffer tank c, one end of the vacuum buffer tank c is connected with the condenser c, and the other end of the vacuum buffer tank c is respectively connected with the delayer c, the receiving tank c3, the receiving tank c2 and the receiving tank c 1.
The invention has the beneficial effects that:
1. the process flow is flexible and changeable, and the special rectification can be carried out through simple valve switching and operation pressure control besides the conventional multi-tower atmospheric and vacuum rectification: azeotropic distillation and extractive distillation, so that different process experiments for recovering the waste organic solvent can be completed;
2. the waste organic solvent is separated and purified by multistage rectification, and each rectifying tower is provided with a plurality of side line discharge ports, so that the characteristic of complex components of the waste organic solvent is combined, the requirement of recovering the required components in the waste organic solvent to the maximum extent can be met, and the purity of the target components is ensured to meet the recycling standard;
3. under the condition of changing experimental tasks, the rectification experimental system disclosed by the invention is quick in response and can be used for quickly adjusting the process flow so as to meet the experimental requirements of different recovery processes.
Drawings
FIG. 1 is a schematic view of a first rectification system in accordance with the present invention;
FIG. 2 is a schematic view of a second rectification system in accordance with the present invention;
FIG. 3 is a schematic view of a third rectification system in accordance with the present invention;
in fig. 1: 1. raw material tanks a, 2, feed pumps a, 3, preheaters a, 4, rectifying towers a, 5, reboilers a, 6, condensers a, 7, coolers a, 7-1, coolers a1, 7-2, coolers a2, 7-3, coolers a3, 8, bottom discharge pumps a, 9, reflux ratio controllers a, 10, receiving tanks a, 10-1, receiving tanks a1, 10-2, receiving tanks a2, 10-3, receiving tanks a3, 10-4, receiving tanks a4, 10-5 receiving tanks a5, 10-6, receiving tanks a6, 11, discharge pumps a, 11-1, discharge pumps a1, 11-2, discharge pumps a2, 11-3, discharge pumps a3, 11-4, discharge pumps a4, 12, vacuum pumps a, 13 and vacuum buffer tanks a.
In fig. 2: 14. raw material tanks b, 15, feed pumps b, 16, preheaters b, 17, extractant tanks b, 18, extractant feed pumps b, 19, extractant preheaters b, 20, rectifying towers b, 21, reboilers b, 22, condensers b, 23, coolers b, 23-1, coolers b1, 23-2, coolers b2, 23-3, coolers b3, 24, bottom discharge pumps b, 25, reflux ratio controllers b, 26, delayers b, 27, entrainer tanks b, 28, entrainer feed pumps b, 29, upper discharge pumps b, 30, buffer tanks b, 31, lower discharge pumps b, 32, reflux pumps b, 33, receiving tanks b, 33-1, receiving tanks b1, 33-2, receiving tanks b2, 33-3 receiving tanks b3, 33-4, receiving tanks 4, 33-5, receiving tanks b5, 33-6 and receiving tanks b6, 35. discharge pumps b, 35-1, discharge pumps b1, 35-2, discharge pumps b2, 35-3, discharge pumps b3, 35-4, discharge pumps b4, 36, vacuum pumps b, 37 and a vacuum buffer tank b.
In fig. 3: 38. raw material tanks c, 39, feed pumps c, 40, preheaters c, 41, rectifying towers c, 42, reboilers c, 43, condensers c, 44, coolers c, 44-1, coolers c1, 44-2, coolers c2, 44-3, coolers c3, 45, kettle bottom discharge pumps c, 46, reflux ratio controllers c, 47, delayers c, 48, upper discharge pumps c, 49, lower discharge pumps c, 50, receiving tanks c1, 50-1, receiving tanks c1-1, 50-2 receiving tanks c1-2, 51, receiving tanks c2, 52, receiving tanks c3, 52-1, receiving tanks c3-1, 52-2, receiving tanks c3-2, 52-3, receiving tanks c3-3, 53, vacuum pumps c, 54, vacuum buffer tanks c, 55 and discharge pumps c.
Detailed Description
The invention is further elucidated with reference to the drawings and the detailed description.
Example 1
A multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources comprises a first rectification system, a second rectification system and a third rectification system which are sequentially connected through pipelines; the first rectifying system comprises a raw material tank a1, a preheater a3, a rectifying tower a4, a reboiler a5, a cooler a 7, a receiving tank a 10, a discharge pump a 11 and a first rectifying tower top system; the bottom end of the rectifying tower a4 is provided with a reboiler a5, the raw material tank a1 is connected with a preheater a3 through a feed pump a2, one end of the preheater a3 is connected with the reboiler a5, and the other end of the preheater a3 is connected with the rectifying tower a 4; the rectifying tower a4 is sequentially connected with a receiving tank a 10, a discharge pump a 11 and a second rectifying system through a cooler a 7; the reboiler a5 is connected with a cooler a 7, a receiving tank a 10, a discharge pump a 11 and a second rectifying system in sequence through a kettle bottom discharge pump a8, and the top end of the rectifying tower a4 is connected with a first rectifying tower top system.
The first rectifying tower top system comprises a condenser a6, a reflux ratio controller a 9, a receiving tank a 10 and a discharge pump a 11, the top end of a rectifying tower a4 is connected with the reflux ratio controller a 9 through the condenser a6, one end of the reflux ratio controller a 9 is connected with the top end of the rectifying tower a4, and the other end of the reflux ratio controller a 9 is sequentially connected with the discharge pump a 11 and a second rectifying system through the receiving tank a 10.
The first rectification system further comprises a first vacuum system, the first vacuum system comprises a vacuum pump a 12 and a vacuum buffer tank a 13, the vacuum pump a 12 is connected with the vacuum buffer tank a 13, one end of the vacuum buffer tank a 13 is connected with the condenser a6, and the other end of the vacuum buffer tank a 13 is connected with the receiving tank a 10.
The second rectification system comprises a raw material tank b 14, a preheater b 16, a rectification tower b20, a reboiler b21, a cooler b 23, a receiving tank b 33, a discharge pump b 35, an extractant tank b 17 and a second rectification tower top system; a reboiler b21 is arranged at the bottom end of the rectifying tower b20, one end of a raw material tank b 14 is connected with the first rectifying system, the other end of the raw material tank b 14 is connected with a preheater b 16 through a feed pump b 15, one end of the preheater b 16 is connected with the reboiler b21, and the other end of the preheater b 16 is connected with the rectifying tower b 20; the rectifying tower b20 is sequentially connected with a receiving tank b 33, a discharge pump b 35 and a third rectifying system through a cooler b 23; the reboiler b21 is connected with the cooler b 23, the receiving tank b 33, the discharge pump b 35 and the third rectification system in sequence through a kettle bottom discharge pump b 24; one end of an extractant tank b 17 is connected with a third rectification system, and the other end of the extractant tank b 17 is sequentially connected with an extractant preheater b 19 and a rectification tower b20 through an extractant feeding pump b 18; the top end of the rectifying tower b20 is connected with a second rectifying tower top system.
The second rectifying tower top system comprises a buffer tank b 30, an upper discharging pump b 29, a delayer b 26, a discharging pump b 35, a condenser b 22, a reflux ratio controller b 25, a receiving tank b 33, an entrainer tank b 27 and a lower discharging pump b 31, the top of the rectifying tower b20 is connected with the condenser b 22, one end of the condenser b 22 is connected with the top of the rectifying tower b20 through the reflux ratio controller b 25, the other end of the condenser b 22 is connected with the delayer b 26, one end of the delayer b 26 is connected with a third rectifying system through the lower discharging pump b 31, the other end of the delayer b 26 is connected with the buffer tank b 30 through the upper discharging pump b 29, one end of the buffer tank b 30 is connected with the third rectifying system, and the other end of the buffer tank b 30 is connected with the top of the rectifying tower b20 through a reflux pump b 32; an entrainer tank b 27 is connected with the delayer b 26 through an entrainer feed pump b 28; the reflux ratio controller b 25 is connected with a discharge pump b 35 and a third rectification system in sequence through a receiving tank b 33.
The second rectification system also comprises a second vacuum system, the second vacuum system comprises a vacuum pump b 36 and a vacuum buffer tank b 37, the vacuum pump b 36 is connected with the vacuum buffer tank b 37, one end of the vacuum buffer tank b 37 is connected with the condenser b 22, and the other end of the vacuum buffer tank b 37 is respectively connected with the delayer b 26 and the receiving tank b 33.
The third rectifying system comprises a raw material tank c 38, a preheater c 40, a rectifying tower c 41, a reboiler c 42, a cooler c 44, a receiving tank c 150, a receiving tank c 251, a discharge pump c 55 and a first rectifying tower top system; a reboiler c 42 is arranged at the bottom end of the rectifying tower c 41, one end of the raw material tank c 38 is connected with the second rectifying system, the other end of the raw material tank c 38 is connected with the preheater c 40 through a feed pump c 39, one end of the preheater c 40 is connected with the reboiler c 42, and the other end of the preheater c 40 is connected with the rectifying tower c 41; the rectifying column c 41 is connected to the receiver tank c 150 through a cooler c 44; the reboiler c 42 is connected with the cooler c 44, the receiving tank c 251, the discharge pump c 55 and the second rectifying system in sequence through a kettle bottom discharge pump c 45, and the top end of the rectifying tower c 41 is connected with the first rectifying tower top system.
The tower top system of the third rectifying tower comprises a delayer c 47, a condenser c 43, a reflux ratio controller c 46, a receiving tank c352, an upper-layer discharging pump c 48 and a lower-layer discharging pump c 49, the tower top of the rectifying tower c 41 is connected with the condenser c 43, one end of the condenser c 43 is connected with the tower top of the rectifying tower c 41 through the reflux ratio controller c 46, the other end of the condenser c 43 is connected with the delayer c 47, one end of the delayer c 47 is connected with the top end of the rectifying tower c 41 through the lower-layer discharging pump c 49, and the other end of the rectifying tower c 41 is connected with the second rectifying system through the upper-layer discharging pump c 48; the reflux ratio controller c 46 is connected to the receiver tank c 352.
The third rectification system also comprises a third vacuum system, the third vacuum system comprises a vacuum pump c 53 and a vacuum buffer tank c54, the vacuum pump c 53 is connected with the vacuum buffer tank c54, one end of the vacuum buffer tank c54 is connected with the condenser c 43, and the other end of the vacuum buffer tank c54 is respectively connected with the delayer c 47, the receiving tank c352, the receiving tank c 251 and the receiving tank c 150.
The absolute pressure of the first vacuum system, the second vacuum system and the third vacuum system is 500 Pa-120 kPa.
Example 2
A process using the multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources is a recovery process of N-methylpyrrolidone waste liquid for a three-tower vacuum rectification system, and comprises the following steps:
the N-methyl pyrrolidone waste liquid is placed in a raw material tank a1, the N-methyl pyrrolidone waste liquid is sent to a preheater a3 for preheating by a feeding pump a2, and enters a rectifying tower a4 from 3/8 from top to bottom of a rectifying tower a4 for reduced pressure rectification, negative pressure is provided by a vacuum pump a 12, and a vacuum buffer tank a 13 is used as pump front protection of the vacuum pump a 12; after the water at the top of the rectifying tower a4 is condensed by a condenser a6, part of the water flows back to the rectifying tower a4 through a reflux ratio controller a 9, and part of the water enters a receiving tank a 310-3; n-methyl pyrrolidone containing a small amount of water and heavy components is enriched in a reboiler a5, heated by a reboiler a5 to be boiled, sent into a cooler a 37-3 through a kettle bottom discharge pump a8 to be cooled and collected in a receiving tank a 610-6.
The material in the receiving tank a 610-6 is transferred to a raw material tank b 14 for storage through a discharge pump a 411-4, the material is sent to a preheater b 16 for preheating by adopting a feed pump b 15, and enters a rectifying tower b20 from 1/2 from top to bottom of the rectifying tower b20 for reduced pressure rectification, the negative pressure is provided by a vacuum pump a 12, and a vacuum buffer tank a 13 is used for protecting the vacuum pump a 12 in front of the pump; after the water and the N-methyl pyrrolidone at the top of the rectifying tower b20 are condensed by a condenser b 22, part of the water and the N-methyl pyrrolidone flow back to a rectifying tower b20 through a reflux ratio controller b 25, and part of the water and the N-methyl pyrrolidone flow into a receiving tank b 333-3; n-methyl pyrrolidone containing a small amount of heavy components is enriched in a reboiler b21, heated by the reboiler b21 to be boiled, and simultaneously sent into a cooler b 323-3 through a kettle bottom discharge pump b 24 to be cooled and collected in a receiving tank b 633-6.
The material in the receiving tank b 633-6 is transferred to a raw material tank c 38 for storage through a discharge pump b 435-4, the material is sent to a preheater c 40 for preheating by adopting a feed pump c 39, and enters a rectifying tower c 41 from 5/8 from top to bottom of a rectifying tower c 41 for reduced pressure rectification, the negative pressure is provided by a vacuum pump a 12, and a vacuum buffer tank a 13 is used for protecting the vacuum pump a 12 in front of the pump; after the finished product of the N-methyl pyrrolidone at the top of the rectifying tower c 41 is condensed by a condenser c 43, part of the finished product flows back to the rectifying tower c 41 through a reflux ratio controller c 46, and part of the finished product enters a receiving tank c 352; heavy components and N-methyl pyrrolidone are enriched in a reboiler c 42, heated by the reboiler c 42 to be boiled, sent into a cooler c 344-3 through a kettle bottom discharge pump c 45 to be cooled, and collected in a receiving tank c 251.
Example 3
A process for using the multifunctional rectification experimental system for comprehensively utilizing waste organic solvent resources is a process for recovering ethanol waste liquid by using a heterogeneous azeotropic rectification system, and comprises the following steps:
the ethanol waste liquid is placed in a raw material tank a1, the ethanol waste liquid is sent to a preheater a3 for preheating by a feed pump a2, and enters a rectifying tower a4 from a 1/2 part from top to bottom of a rectifying tower a4 for normal pressure rectification; after the azeotrope of the water and the ethanol at the top of the rectifying tower a4 is condensed by a condenser a6, part of the azeotrope flows back to the rectifying tower a4 through a reflux ratio controller a 9, and part of the azeotrope enters a receiving tank a 310-3; the water and heavy components are enriched in the reboiler a5, heated by the reboiler a5 to be boiled, and simultaneously sent to the cooler a 37-3 through the kettle bottom discharge pump a8 to be cooled and collected in the receiving tank a 610-6.
The material in the receiving tank a 610-6 is transferred to a raw material tank b 14 for storage through a discharge pump a 411-4, the material is sent to a preheater b 16 for preheating through a feed pump b 15, and enters a rectifying tower b20 from 3/8 from top to bottom of a rectifying tower b20 body for heterogeneous azeotropic rectification under the normal pressure condition; the entrainer cyclohexane is stored in an entrainer tank b 27 and enters a delayer b 26 through an entrainer feed pump b 28; after the azeotrope of water, ethanol and cyclohexane at the top of the rectifying tower b20 is condensed by a condenser b 22, the azeotrope is divided into an upper organic phase and a lower aqueous phase by a delayer b 26; the upper organic phase is sent into a buffer tank b 30 through an upper discharge pump b 29; the lower water phase is sent to a raw material tank c 38 through a lower discharging pump b 31; the material in the buffer tank b 30 enters the top of the rectifying tower b20 through a reflux pump b32 to be used as reflux liquid of the rectifying tower b 20; the finished product of the ethanol is enriched in a reboiler b21, is heated by the reboiler b21 to be boiled, and is simultaneously sent into a cooler b 323-3 through a kettle bottom discharge pump b 24 to be cooled and collected in a receiving tank b 633-6.
The material in the raw material tank c 38 is sent into a preheater c 40 by a feed pump c 39 for preheating, and enters a rectifying tower c 41 from 5/8 from top to bottom of a rectifying tower c 41 for heterogeneous azeotropic rectification under the normal pressure condition; after the azeotrope of water, ethanol and cyclohexane at the top of the rectifying tower c 41 is condensed by a condenser c 43, the azeotrope is divided into an upper organic phase and a lower aqueous phase by a delayer c 47; the upper organic phase is sent into a buffer tank b 30 through an upper discharge pump c 48; the lower water phase reflows to the top of the rectifying tower c 41 through a lower discharge pump c 49 and is used as a reflux of the rectifying tower c 41; the waste water containing a small amount of ethanol is enriched in the reboiler c 42, heated by the reboiler c 42 to be boiled, and simultaneously sent into the cooler c 344-3 through the kettle bottom discharge pump c 45 to be cooled and collected in the receiving tank c 251.
Example 4
A process for using the multifunctional rectification experimental system for comprehensively utilizing waste organic solvent resources is a process for recovering ethanol waste liquid by an extractive rectification system, which comprises the following steps:
the ethanol waste liquid is placed in a raw material tank a1, the ethanol waste liquid is sent to a preheater a3 for preheating by a feed pump a2, and enters a rectifying tower a4 from a 1/2 part from top to bottom of a rectifying tower a4 for normal pressure rectification; after the azeotrope of the water and the ethanol at the top of the rectifying tower a4 is condensed by a condenser a6, part of the azeotrope flows back to the rectifying tower a4 through a reflux ratio controller a 9, and part of the azeotrope enters a receiving tank a 310-3; the water and heavy components are enriched in the reboiler a5, heated by the reboiler a5 to be boiled, and simultaneously sent to the cooler a 37-3 through the kettle bottom discharge pump a8 to be cooled and collected in the receiving tank a 610-6.
The material in the receiving tank a 610-6 is transferred to a raw material tank b 14 for storage through a discharge pump a 411-4, the material is sent to a preheater b 16 for preheating through a feed pump b 15, and enters a rectifying tower b20 from 5/8 from top to bottom of the rectifying tower b20 for decompression, extraction, boiling and rectification, the negative pressure is provided by a vacuum pump b 36, and a vacuum buffer tank b 37 is used for protecting the vacuum pump b 36 in front of the pump; the extractant ethylene glycol is stored in an extractant tank b 17, is sent into an extractant preheater b 19 by an extractant feeding pump b 18 for preheating, and enters a rectifying tower b20 from the 1/8 position from top to bottom of the tower body of the rectifying tower b 20; after an ethanol finished product at the top of the rectifying tower b20 is condensed by a condenser b 22, part of the ethanol finished product flows back to the rectifying tower b20 through a reflux ratio controller b 25, and part of the ethanol finished product enters a receiving tank b 333-6; water and glycol are enriched in a reboiler b21, heated by the reboiler b21 to be boiled, and simultaneously sent into a cooler b 323-3 through a kettle bottom discharge pump b 24 to be cooled and collected in a receiving tank b 633-6.
The material in the receiving tank b 633-6 is transferred to a raw material tank c 38 for storage through a discharge pump b 435-4, the material is sent to a preheater c 40 for preheating by adopting a feed pump c 39, and enters a rectifying tower c 41 from 5/8 from top to bottom of a rectifying tower c 41 for reduced pressure rectification, the negative pressure is provided by a vacuum pump c 53, and a vacuum buffer tank c54 is used for protecting the vacuum pump c 53; after the wastewater at the top of the rectifying tower c 41 is condensed by a condenser c 43, part of the wastewater flows back to the rectifying tower c 41 through a reflux ratio controller c 46, and part of the wastewater enters a receiving tank c 352; ethylene glycol containing a small amount of water is enriched in a reboiler c 42, heated by the reboiler c 42 to be boiled, and simultaneously sent into a cooler c 344-3 through a kettle bottom discharge pump c 45 to be cooled and collected in a receiving tank c 251; finally, the material in the receiving tank c 251 is sent to the extracting agent tank b 17 by the discharging pump c 55, and the ethylene glycol can be recycled.
The above-mentioned embodiments are merely preferred embodiments of the present invention, and should not be construed as limiting the present invention, and the scope of the present invention should be defined by the claims, and equivalents including technical features of the claims, i.e., equivalent modifications within the scope of the present invention.

Claims (10)

1. A multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources is characterized by comprising a first rectification system, a second rectification system and a third rectification system which are sequentially connected through pipelines; the first rectifying system comprises a raw material tank a, a preheater a, a rectifying tower a, a reboiler a, a cooler a, a receiving tank a, a discharge pump a and a first rectifying tower top system; the bottom end of the rectifying tower a is provided with a reboiler a, the raw material tank a is connected with a preheater a through a feed pump a, one end of the preheater a is connected with the reboiler a, and the other end of the preheater a is connected with the rectifying tower a; the rectifying tower a is sequentially connected with a receiving tank a, a discharge pump a and a second rectifying system through a cooler a; the reboiler a is sequentially connected with the cooler a, the receiving tank a, the discharge pump a and the second rectifying system through the kettle bottom discharge pump a, and the top end of the rectifying tower a is connected with the first rectifying tower top system.
2. The multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources as claimed in claim 1, wherein: the first rectifying tower top system comprises a condenser a, a reflux ratio controller a, a receiving tank a and a discharge pump a, the top end of the rectifying tower a is connected with the reflux ratio controller a through the condenser a, one end of the reflux ratio controller a is connected with the top end of the rectifying tower a, and the other end of the reflux ratio controller a is sequentially connected with the discharge pump a and the second rectifying system through the receiving tank a.
3. The multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources as claimed in claim 2, wherein: the first rectification system further comprises a first vacuum system, the first vacuum system comprises a vacuum pump a and a vacuum buffer tank a, the vacuum pump a is connected with the vacuum buffer tank a, one end of the vacuum buffer tank a is connected with the condenser a, and the other end of the vacuum buffer tank a is connected with the receiving tank a.
4. The multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources as claimed in claim 1, wherein: the second rectifying system comprises a raw material tank b, a preheater b, a rectifying tower b, a reboiler b, a cooler b, a receiving tank b, a discharge pump b, an extractant tank b and a second rectifying tower top system; a reboiler b is arranged at the bottom end of the rectifying tower b, one end of the raw material tank b is connected with the first rectifying system, the other end of the raw material tank b is connected with the preheater b through a feed pump b, one end of the preheater b is connected with the reboiler b, and the other end of the preheater b is connected with the rectifying tower b; the rectifying tower b is sequentially connected with a receiving tank b, a discharge pump b and a third rectifying system through a cooler b; the reboiler b is sequentially connected with the cooler b, the receiving tank b, the discharge pump b and the third rectification system through a kettle bottom discharge pump b; one end of the extractant tank b is connected with the third rectification system, and the other end of the extractant tank b is sequentially connected with the extractant preheater b and the rectification tower b through an extractant feeding pump b; the top end of the rectifying tower b is connected with a second rectifying tower top system.
5. The multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources as claimed in claim 4, wherein: the second rectifying tower top system comprises a buffer tank b, an upper discharging pump b, a delayer b, a discharging pump b, a condenser b, a reflux ratio controller b, a receiving tank b, an entrainer tank b and a lower discharging pump b, wherein the top of the rectifying tower b is connected with the condenser b, one end of the condenser b is connected with the top of the rectifying tower b through the reflux ratio controller b, the other end of the condenser b is connected with the delayer b, one end of the delayer b is connected with a third rectifying system through the lower discharging pump b, the other end of the delayer b is connected with the buffer tank b through the upper discharging pump b, one end of the buffer tank b is connected with the third rectifying system, and the other end of the buffer tank b is connected with the top of the rectifying tower b through the reflux pump b; the entrainer tank b is connected with the delayer b through an entrainer feeding pump b; the reflux ratio controller b is connected with the discharge pump b and the third rectification system in sequence through the receiving tank b.
6. The multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources as claimed in claim 5, wherein: the second rectification system also comprises a second vacuum system, the second vacuum system comprises a vacuum pump b and a vacuum buffer tank b, the vacuum pump b is connected with the vacuum buffer tank b, one end of the vacuum buffer tank b is connected with the condenser b, and the other end of the vacuum buffer tank b is respectively connected with the delayer b and the receiving tank b.
7. The multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources as claimed in claim 1, wherein: the third rectifying system comprises a raw material tank c, a preheater c, a rectifying tower c, a reboiler c, a cooler c, a receiving tank c1, a receiving tank c2, a discharging pump c and a first rectifying tower top system; a reboiler c is arranged at the bottom end of the rectifying tower c, one end of the raw material tank c is connected with the second rectifying system, the other end of the raw material tank c is connected with the preheater c through a feed pump c, one end of the preheater c is connected with the reboiler c, and the other end of the preheater c is connected with the rectifying tower c; the rectifying tower c is connected with a receiving tank c1 through a cooler c; the reboiler c is connected with the cooler c, the receiving tank c2, the discharge pump c and the second rectifying system in sequence through the kettle bottom discharge pump c, and the top end of the rectifying tower c is connected with the first rectifying tower top system.
8. The multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources as claimed in claim 7, wherein: the tower top system of the third rectifying tower comprises a delayer c, a condenser c, a reflux ratio controller c, a receiving tank c3, an upper-layer discharge pump c and a lower-layer discharge pump c, the tower top of the rectifying tower c is connected with the condenser c, one end of the condenser c is connected with the tower top of the rectifying tower c through the reflux ratio controller c, the other end of the condenser c is connected with the delayer c, one end of the delayer c is connected with the top end of the rectifying tower c through the lower-layer discharge pump c, and the other end of the rectifying tower c is connected with the second rectifying system through the upper-layer discharge pump c; the reflux ratio controller c is connected to the receiver tank c 3.
9. The multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources as claimed in claim 7, wherein: the third rectification system also comprises a third vacuum system, the third vacuum system comprises a vacuum pump c and a vacuum buffer tank c, the vacuum pump c is connected with the vacuum buffer tank c, one end of the vacuum buffer tank c is connected with the condenser c, and the other end of the vacuum buffer tank c is respectively connected with the delayer c, the receiving tank c3, the receiving tank c2 and the receiving tank c 1.
10. The multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources as claimed in claim 3, 6 or 9, wherein: the rectifying tower a, the rectifying tower b and the rectifying tower c are provided with at least 2 feed inlets; and at least 2 lateral line discharge holes are formed in the rectifying tower a, the rectifying tower b and the rectifying tower c.
CN202011203660.1A 2020-11-02 2020-11-02 Multifunctional rectification experimental system for comprehensive utilization of waste organic solvent resources Pending CN112354205A (en)

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Application publication date: 20210212