CN204767507U - Distillation tower - Google Patents

Distillation tower Download PDF

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Publication number
CN204767507U
CN204767507U CN201520071334.8U CN201520071334U CN204767507U CN 204767507 U CN204767507 U CN 204767507U CN 201520071334 U CN201520071334 U CN 201520071334U CN 204767507 U CN204767507 U CN 204767507U
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China
Prior art keywords
exchange apparatus
distillation column
heat
pipeline
acetonitrile
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CN201520071334.8U
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Chinese (zh)
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熊瑾�
顾军民
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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Abstract

The utility model relates to a distillation tower, distillation tower includes: the distillation column, indirect heating equipment, it is used for the condensation by the configuration the gaseous phase commodity circulation of distilling off in the distillation column top, it is disposed does not congeal the gas outlet to and cooling water inlet pipeline and outlet line, the coolant outlet pipeline includes the control valve, indirect heating equipment lime set temperature controller, it is used for control by the configuration the control valve of coolant outlet pipeline is through adjusting indirect heating equipment lime set temperature is controlled to the control valve.

Description

Destilling tower
Technical field
The utility model relates to a kind of destilling tower.
Background technology
In the production process of ammoxidating propylene to prepare acrylonitrile, coproduct hydrogen cyanic acid and acetonitrile simultaneously, wherein the impurity such as aldehyde, Tong, oxazole, propionitrile and a small amount of hydrogen cyanide are extracted to acetonitrile solution in acrylonitrile extraction desorption process, through acetonitrile desorb or stripping in crude acetonitrile.Usually we adopt by the group technology of decyanation tower, chemical treatment, decompression, pressurization azeotropic distillation, reclaim continuously acetonitrile.Such as document CN1328994A discloses a kind of high-purity acetonitrile refining method, high-purity acetonitrile is reclaimed continuously from containing acetonitrile, water, HCN, oxazole and heavy organic crude acetonitrile, comprise the following steps successively: a) crude acetonitrile is separated through the first knockout tower, HCN and Light ends are discharged by tower top, part water and heavy organic matter are discharged by tower reactor, take out out oxazole in the first knockout tower rectifying section top side line liquid phase; B) being stripped of Light ends divides the water-acetonitrile that contains of oxazole to add alkali chemical treatment through chemical treatment still after the first knockout tower stripping section bottom side line gas phase is extracted out with large absolutely portion; C) through add alkali chemical treatment remove free HCN after enter the second knockout tower of decompression containing water-acetonitrile, remove heavy organic matter and water in tower reactor; D) be separated tower top from second and steam the 3rd knockout tower that the acetonitrile being stripped of most of water enters pressurization, the acetonitrile material that tower top steams containing oxazole and moisture content returns the first knockout tower charging, and in stripping section bottom, gas phase extracts to obtain high-purity acetonitrile out.The method, by increasing a liquid phase outlet port on the rectifying section top of the first knockout tower, makes Lei Ji oxazole be discharged system smoothly.But, because this strand of lateral line withdrawal function mass flow is little, and in order to ensure the high-recovery of final acetonitrile, this strand of material generally can not be extracted out continuously, extract pipeline out and very easily occur clogging, cause regular unavailable or parking maintenance, device can not long period steady and continuous run.For overcoming this problem, in current industrial production, by controlling the tower top temperature of the first knockout tower (removing hydrogen cyanide tower), top gaseous phase logistics is after condenser portion condensation, not solidifying gas sends to hydrogen cyanide incinerator or other emission-control equipments, lime set all passes back into dehydrogenation cyanic acid tower top, makes Lei Ji oxazole and hydrogen cyanide and a small amount of acetonitrile exclude system as Light ends, ensure that device stable operation.But, the method is adopted to create again new problem, because tower top temperature controls to rely on overhead condenser indirectly to control to realize, the sensitivity regulated is not high, easy generation is delayed, fluctuation is large, when the light component containing hydrogen cyanide and oxazole removes from top of tower, is difficult to effectively control the quantity of distillate of acetonitrile with light component.So prior art, by controlling the method for tower top temperature, is often difficult to reach the object effectively controlling acetonitrile loss.
Summary of the invention
The utility model aims to provide a kind of destilling tower.This destilling tower has the advantages that effectively control acetonitrile loss.
For achieving the above object, the technical scheme that the utility model is taked is as follows: a kind of destilling tower, comprising: distillation column; Heat-exchange apparatus, it is arranged to the gaseous stream that described in condensation, distillation column top distillates; It is configured with solidifying gas vent, and cooling water inlet pipeline and outlet line; Described coolant outlet pipeline comprises control valve; Heat-exchange apparatus lime set temperature controller, it is arranged to the control valve controlling described coolant outlet pipeline, controls heat-exchange apparatus lime set temperature by regulating described control valve.
In technique scheme, preferably, described distillation column is arranged to: accept the crude acetonitrile from acrylonitrile installation by the material inlet in the middle part of distillation column, and be arranged to acetonitrile of purifying further.
In technique scheme, preferably, described distillation column comprises top, middle part and bottom; Its top comprises the gaseous stream outlet being positioned at top, and is positioned at the phegma entrance of described gaseous stream outlet below; Middle part comprises the acetonitrile products export being positioned at side line; Bottom comprises heavy constituent outlet; Described heat-exchange apparatus is configured with gas access and condensate outlet.In technique scheme, preferably, described acetonitrile products export is positioned described distillation column height from top to bottom 60 ~ 90%.
In technique scheme, preferably, the first pipeline is connected with between described distillation column top gas phase stream outlet and described heat-exchange apparatus gas access; Described first pipeline is arranged to described distillation column top gas phase stream outlet effluent air and is circulated to described heat-exchange apparatus.
In technique scheme, preferably, second pipe is connected with between described distillation column phegma entrance and described heat-exchange apparatus condensate outlet; Described second pipe is arranged to the described distillation column that the lime set in described heat-exchange apparatus to be circulated back.
In technique scheme, preferably, the not solidifying of described heat-exchange apparatus is connected with the 3rd pipeline between gas vent and follow-up exhaust treatment system; Described 3rd pipeline is arranged to and the not solidifying gas flow in described heat-exchange apparatus is passed to follow-up exhaust treatment system.
In technique scheme, preferably, described heat-exchange apparatus comprises condenser and gas-liquid separator; The 4th pipeline is connected with between described condenser and gas-liquid separator.3
In technique scheme, preferably, by weight percentage, described crude acetonitrile raw material comprises 20 ~ 60% acetonitriles, 1 ~ 4%HCN, 0.1 ~ 0.3% acrylonitrile, 34 ~ 79% water, 0.1 ~ 0.7% oxazole, 0.1 ~ 1% heavy organic matter.
In technique scheme, preferably, described distillation column top operational pressure is 0.1 ~ 0.13MPa, and feedstock temperature is 30 ~ 70 DEG C, and the acetonitrile product outlet temperature that middle part is positioned at side line is 76 ~ 100 DEG C, and bottom temperature is 105 ~ 120 DEG C.
In technique scheme, preferably, condensate temperature control range is 45 ~ 60 DEG C; More preferably, condensate temperature control range is 46 ~ 58 DEG C; Most preferably, condensate temperature control range is 47 ~ 55 DEG C; Particularly preferably, condensate temperature control range is 48 ~ 53 DEG C.
The method that the utility model is controlled by the discharging and refluxer temperature cascade adopting heat-exchange apparatus cooling water, regulate heat-exchange apparatus cooling water inflow, control condensate temperature, control the entrainment rate that the removal efficiency of light component in lime set and heat-exchange apparatus discharge acetonitrile in solidifying gas phase, the loss of an acetonitrile that can effectively control to release at this.The boiling point of oxazole a little less than acetonitrile apparently higher than HCN, under existing equipment condition, process conditions, takes off and together distillates from decyanation column overhead with oxazole except having acetonitrile while oxazole.By controlling the lime set temperature of tower top heat-exchange apparatus, directly can control the vapor liquid equilibrium of heat-exchange apparatus, effectively the acetonitrile that tower top distillates being stayed in lime set to greatest extent and returning decyanation tower as backflow, effectively controlling the loss of acetonitrile.Adopt the utility model, than prior art direct control tower top operating temperature, control more direct, decyanation tower smooth operation, the loss late of decyanation tower acetonitrile can be controlled in less than 3 % by weight, thus ensures the rate of recovery of final acetonitrile product, achieves good technique effect.
Accompanying drawing explanation
Fig. 1 and Fig. 2 is the utility model schematic diagram.
In Fig. 1 and Fig. 2,1 is distillation column, and 2 is heat-exchange apparatus, and 3 is control valve, and 4 is heat-exchange apparatus lime set temperature controller.
Below by embodiment, the utility model is further elaborated.
Detailed description of the invention
Adopt equipment shown in Fig. 1 or Fig. 2, entered from the material inlet 5 be positioned in the middle part of distillation column by feed line 6 raw material crude acetonitrile.
Distillation column 1 comprises top, middle part and bottom.Its top comprises the gaseous stream outlet 7 being positioned at top, and is positioned at the phegma entrance 24 of gaseous stream outlet below.Comprise the acetonitrile products export 11 being positioned at side line in the middle part of it, by pipeline 12, the gas phase acetonitrile after purification is extracted out.Comprise heavy constituent outlet 13 bottom it, by pipeline 14, part water and heavy component are discharged.
Heat-exchange apparatus 2 is configured with gas access 15 and condensate outlet 22.
The first pipeline 8 is connected with between distillation column top gas phase stream outlet 7 and heat-exchange apparatus gas access 15; First pipeline 8 is arranged to distillation column top gas phase stream outlet 7 effluent air and is circulated to heat-exchange apparatus 2.
Second pipe 23 is connected with between distillation column phegma entrance 24 and heat-exchange apparatus condensate outlet 22; Second pipe 23 is arranged to the distillation column 1 that the lime set in heat-exchange apparatus 2 to be circulated back.
The not solidifying of heat-exchange apparatus is connected with the 3rd pipeline 10 between gas vent 9 and follow-up exhaust treatment system; 3rd pipeline 10 is arranged to and the not solidifying gas flow in described heat-exchange apparatus is passed to follow-up exhaust treatment system.
Heat-exchange apparatus 2 is configured with cooling water inlet 18 and coolant outlet 16, enters heat-exchange apparatus 2 by pipeline 19 cooling water, leaves heat-exchange apparatus 2 by the cooling water after pipeline 17 heat exchange.Coolant outlet pipeline 17 comprises control valve 3.Control valve 3 is configured to, by changing cooling water by the size of the aperture of valve 3, regulate the flow of cooling water in heat-exchange apparatus 2.Second pipeline 23 is configured with heat-exchange apparatus lime set temperature controller 4, it is arranged to the control valve 3 controlling described coolant outlet pipeline, controls heat-exchange apparatus 2 lime set temperature by adjusting control valve 3.When heat-exchange apparatus 2 lime set temperature controller 4 detects the scope of condensate temperature higher than predetermined temperature or temperature, heat-exchange apparatus 2 lime set temperature controller 4 activated valve 3 to open suitable amount more from its initial opening, and allows more cooling water to enter heat-exchange apparatus 2 by cooling water inlet pipeline 19.When heat-exchange apparatus 2 lime set temperature controller 4 detects the scope of condensate temperature lower than predetermined temperature or temperature, heat-exchange apparatus 2 lime set temperature controller 4 activated valve 3 to close suitable amount more from its initial opening, and allows the cooling water reduced to enter heat-exchange apparatus 2 by cooling water inlet pipeline 19.
Heat-exchange apparatus 2 is arranged to the gaseous stream that condensation distillation column 1 top gas outlet 7 distillates, and will not coagulate gas discharge.Its configuration meets above-mentioned functions.Both condensation and gas-liquid can be separated in same equipment and complete, such as, shown in Fig. 1, heat-exchange apparatus 2 top is tubular heat exchanger, and bottom is gas-liquid separator, and heat-exchange apparatus 2 is provided with not solidifying gas outlet 9, will not coagulate gas discharge by pipeline 10; Also condensation and gas-liquid can be separated in two equipment and carry out, such as shown in Fig. 2, heat-exchange apparatus 2 comprises condenser 20 and gas-liquid separator 21, gas-liquid separator 21 top is configured with not solidifying gas outlet 9, not solidifying gas discharges system by pipeline 10, be connected with between condenser 20 and gas-liquid separator 21 the 4th pipeline the 25, four pipeline 25 be arranged to by from distillation column top, with condenser 20 heat exchange after logistics be circulated to gas-liquid separator 21.
[embodiment 1]
Adopt destilling tower shown in Fig. 1, crude acetonitrile raw material containing acetonitrile 45%, HCN2%, acrylonitrile 0.1%, water 51.9%, oxazole 0.5%, heavy organic matter 0.5% adds from the middle part of distillation column 1, and feeding temperature is 40 DEG C, and tower top pressure is normal pressure, tower top temperature is 63 DEG C, and bottom temperature is 115 DEG C.Distillation column 1 highly from top to bottom 85% place (acetonitrile products export 11) side line concentration be the acetonitrile of 70 % by weight, extract out temperature be 92 DEG C.Distillation column top gas phase enters heat-exchange apparatus 2, and heat-exchange apparatus lime set is back to distillation column.Discharging and the refluxer temperature cascade of heat-exchange apparatus cooling water control, and regulating heat-exchange apparatus cooling water inflow to control heat-exchange apparatus condensate temperature is 45 DEG C.The solidifying gas outlet streams of heat-exchange apparatus consists of acetonitrile 5.9%, oxazole 11.7%, HCN71.7%, light component 7.2%, other are water.Acetonitrile loss late is 1%, decyanation tower smooth operation.
[embodiment 2]
Adopt destilling tower shown in Fig. 2, crude acetonitrile raw material containing acetonitrile 46%, HCN2.1%, acrylonitrile 0.2%, water 50.7%, oxazole 0.3%, heavy organic matter 0.7% adds from the middle part of distillation column 1, feeding temperature is 38 DEG C, tower top pressure is normal pressure, tower top temperature is 67 DEG C, and bottom temperature is 118 DEG C.Distillation column 1 highly from top to bottom 80% place (acetonitrile products export 11) side line concentration be the acetonitrile of 73 % by weight, extract out temperature be 90 DEG C.Distillation column top gas phase enters condenser 20, and the logistics after heat exchange is circulated to gas-liquid separator, and the lime set in gas-liquid separator 21 is back to distillation column.Discharging and the refluxer temperature cascade of condenser cooling water control, and regulating condenser cooling water amount to control reflux condensation mode liquid temp is 55 DEG C.The solidifying gas in gas-liquid separator 21 top exports that 9 logistics consist of acetonitrile 10.9%, oxazole 14.7%, HCN64.1%, light component 6.8%, other are water.Acetonitrile loss late is 2.1%, decyanation tower smooth operation.

Claims (8)

1. a destilling tower, comprising:
Distillation column;
Heat-exchange apparatus, it is arranged to the gaseous stream that described in condensation, distillation column top distillates; It is configured with solidifying gas vent, and cooling water inlet pipeline and outlet line; Described coolant outlet pipeline comprises control valve;
Heat-exchange apparatus lime set temperature controller, it is arranged to the control valve controlling described coolant outlet pipeline, controls heat-exchange apparatus lime set temperature by regulating described control valve.
2. destilling tower according to claim 1, is characterized in that described distillation column is arranged to: accept the crude acetonitrile from acrylonitrile installation by the material inlet in the middle part of distillation column, and be arranged to acetonitrile of purifying further.
3. destilling tower according to claim 1, is characterized in that described distillation column comprises top, middle part and bottom; Its top comprises the gaseous stream outlet being positioned at top, and is positioned at the phegma entrance of described gaseous stream outlet below; Middle part comprises the acetonitrile products export being positioned at side line; Bottom comprises heavy constituent outlet;
Described heat-exchange apparatus is configured with gas access and condensate outlet.
4. destilling tower according to claim 3, is characterized in that described acetonitrile products export is positioned described distillation column height from top to bottom 60 ~ 90%.
5. destilling tower according to claim 3, is characterized in that being connected with the first pipeline between described distillation column top gas phase stream outlet and described heat-exchange apparatus gas access; Described first pipeline is arranged to described distillation column top gas phase stream outlet effluent air and is circulated to described heat-exchange apparatus.
6. destilling tower according to claim 3, is characterized in that being connected with second pipe between described distillation column phegma entrance and described heat-exchange apparatus condensate outlet; Described second pipe is arranged to the described distillation column that the lime set in described heat-exchange apparatus to be circulated back.
7., according to destilling tower described in claim 1, it is characterized in that the not solidifying of described heat-exchange apparatus is connected with the 3rd pipeline between gas vent and follow-up exhaust treatment system; Described 3rd pipeline is arranged to and the not solidifying gas flow in described heat-exchange apparatus is passed to follow-up exhaust treatment system.
8., according to destilling tower described in claim 1, it is characterized in that described heat-exchange apparatus comprises condenser and gas-liquid separator; The 4th pipeline is connected with between described condenser and gas-liquid separator.
CN201520071334.8U 2015-01-31 2015-01-31 Distillation tower Active CN204767507U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105983244A (en) * 2015-01-31 2016-10-05 中国石油化工股份有限公司 Distillation tower and application thereof
CN112393619A (en) * 2020-11-10 2021-02-23 润泰化学(泰兴)有限公司 A safe type overhead condenser for producing hexadecanediester

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105983244A (en) * 2015-01-31 2016-10-05 中国石油化工股份有限公司 Distillation tower and application thereof
CN112393619A (en) * 2020-11-10 2021-02-23 润泰化学(泰兴)有限公司 A safe type overhead condenser for producing hexadecanediester

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