CN106699599A - Heads column pump circulation - Google Patents
Heads column pump circulation Download PDFInfo
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- CN106699599A CN106699599A CN201510782236.XA CN201510782236A CN106699599A CN 106699599 A CN106699599 A CN 106699599A CN 201510782236 A CN201510782236 A CN 201510782236A CN 106699599 A CN106699599 A CN 106699599A
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- column
- head fraction
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- effluent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0208—Separation of non-miscible liquids by sedimentation
- B01D17/0214—Separation of non-miscible liquids by sedimentation with removal of one of the phases
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
- B01D3/4211—Regulation; Control of columns
- B01D3/4261—Side stream
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a process and a system used for recycling of acrylonitrile and HCN. The system comprises a heads column system. According to the system, loading of a heads column condenser is reduced, equipment is reduced, and the needed purity and standards are maintained under the minimum increasing of reboiler loading. The process comprises following steps: a reactant flow containing acrylonitrile, HCN, and water is delivered into a heads column; distillation of the reactant flow is carried out in the heads column so as to obtain heads column tower top distillate flow containing HCN and a bottom liquid flow containing acrylonitrile; side flow is removed from side-cut distillate of heads column containing water and organic matters; at least a part of water and the organic matters are separated from the side flow so as to provide organic flow; the organic flow is recycled back to the heads column; the ratio of the amount of the side flow separated from the side-cut distillate of the heads column to the amount of the organic flow recycled back to the heads column under the side-cut distillate is adjusted, and 500ppm or less HCN is provided for bottom liquid flow.
Description
Technical field
There is provided a kind of process and system reclaimed for acrylonitrile and HCN.More specifically, head fraction column (heads
Column) system operatio is into reduction head fraction column condenser duty, and reduces equipment requirement, while being increased come the pureness specifications needed for maintaining with the minimum of reboiler duty.
Background technology
Acrylonitrile manufacturing process produces HCN.HCN must be removed from acrylonitrile in the process, to meet final acrylonitrile specification.HCN can be valuable accessory substance, to expect that the process reclaims the HCN of purification.In order that Human body package is minimized, system reduces the exposure to HCN in position to remove HCN during equipment operation or maintenance.In certain aspects, equipment of the manufacture system using HCN can be processed with low risk of leakage.For example, the need for contributing to elimination in HCN treatment to pump using the system of gravity stream.(particularly column plate (tray)) is typically the problem in acrylonitrile equipment however, fouling.The polymerization of HCN can be the problem in acrylonitrile process.
An important system for removing HCN in acrylonitrile manufacturing process is directed to use with head fraction column.Head fraction column 30 includes multiple column plates.In one embodiment, head fraction column 30 include 50 (50) and 75 (75) it is individual between column plates, it is alternatively individual 55 (55) to 65 (65) between column plate.In embodiment, head fraction column 30 includes 62 (62) individual column plates, alternatively 60 (60) or 65 (65) column plates.Head fraction column 30 may be configured to the reception crude product nitrile at column plate 28 and enter stream 1.In embodiment, column plate 28 can be all located between the 35th and the 48th column plate since the bottom of head fraction column 30 in all cases, preferably between 40 to four ten four four ten column plates.Head fraction column 30 may be configured to remove effluent 44 from side stream (sidedraw) of head fraction column, side stream including being located between the 15th and the 28th column plate since the bottom of head fraction column 30 in all cases, water and organic matter between preferably 18 and 25 column plates.In an alternative embodiment, column plate 28 can be the 42nd or the 38th column plate since the bottom of head fraction column 12.
In an alternative embodiment, column plate 28 can be the 47th column plate since the bottom of head fraction column 30, and head fraction column 30 may include 67 column plates.In embodiment, the first to two ten bottom trays of head fraction column 30 dry acrylonitrile product.In embodiment, the 21st to the 42nd column plate since the bottom of head fraction column 30 is removed and purification HCN.In embodiment, head fraction column 30 includes 40 (40) and 65 (65) column plates between individual.In embodiment, and feed tray 28 can be between the 20th and the 30th column plate since head fraction tower bottom, and including them.
In some designs, head fraction column includes stacking two tower sections on top of each other.In this design, bottom section is referred to as drying tower/section, and including between 15 and 30 column plates, between preferably 18 and 25, between more preferably 18 and 22.In another aspect, head fraction column includes column plate 1 to 20, and wherein column plate 1 is the column plate of bottom.Head tower section is the position that HCN distills in tower top, and it is referred to as head fraction column/section or HCN towers/section, and in an aspect, including the column plate between 30 and 50, between preferably 32 and 48, and the column plate between more preferably 38 and 48.In another aspect, tower includes column plate 21 to 62, and wherein column plate 62 is highest column plate.These numbers can be different in different head fraction columns.
In order to help to reduce fouling, conventional head fraction drying tower is operated in the case where pressure (vacuum) operation is reduced.The operator scheme sharp reduces fouling, and extends the operating time between HCN or the cleaning of head fraction column.The operation of HCN or head fraction column in the case where pressure is reduced needs to distill at a lower temperature.Generation makes the polymerization rate of the solid of process device fouling greatly reduce at a lower temperature.However, used as trading off, lower temperature distillation needs to provide relatively low condensation temperature.This needs the cooling agent of freezing, for example, the ethene-ethylene glycol-water mixture of cooling, commonly referred to " bittern (brine) ".Bittern may need about 0 DEG C of temperature for head fraction column condenser, and about -10 DEG C of temperature is needed at relief condenser.
The content of the invention
It is a kind of to include that offer provides to head fraction column the stream of entering for including acrylonitrile, HCN and water for the process that acrylonitrile is reclaimed；This is distilled in head fraction column to enter stream to produce head fraction column overhead (overhead) stream including HCN and the bottom liquid stream including acrylonitrile；From the removal effluent that sides stream including water and the head fraction column of organic matter；At least some water and organic matter are separated from effluent to provide organic streams；Organic streams are made to return to head fraction column；With adjustment from the amount and the ratio of the amount of the organic streams that head fraction column is returned in lower section of sideing stream of the effluent of the removal of sideing stream of head fraction column, 500ppm or less HCN is provided with to bottom liquid stream.
It is a kind of to include that the stream of entering that include acrylonitrile, HCN and water is provided to head fraction column for the process that acrylonitrile is reclaimed；This is distilled in head fraction column to enter stream to produce the head fraction column column overhead stream including HCN and the bottom liquid stream including acrylonitrile；From the removal effluent that sides stream including water and the head fraction column of organic matter；At least some water and organic matter are separated from effluent；It is divided at least two plumes with by organic matter, and the stream is returned at least two points of positions opened on head fraction column.
A kind of process for operating head fraction column includes that the stream of entering that will include acrylonitrile, HCN and water is provided to head fraction column；This is distilled in head fraction column to enter stream to produce head fraction column column overhead stream and the head fraction column overhead is streamed into head fraction column condenser；Include the effluent of water and organic matter from the removal of sideing stream of head fraction column, and effluent be sent into effluent heat exchanger providing the effluent of cooling；At least some water and organic matter are separated from the effluent of cooling；Organic streams are made to return to head fraction column；With adjustment from the amount of the effluent of the removal of sideing stream of head fraction column and the ratio of the amount of the organic streams that head fraction column is returned in lower section of sideing stream, to provide the ratio between heat load and heat load in effluent heat exchanger in about 2.5 or smaller head fraction column condenser.
It is a kind of to include that the stream of entering that include acrylonitrile, HCN and water is provided to head fraction column for the process that acrylonitrile is reclaimed；This is distilled in head fraction column to enter stream to produce the head fraction column column overhead stream including HCN, the bottom liquid stream including acrylonitrile, and the effluent for sideing stream from head fraction column including water and organic matter；Wherein, the vapor/liquid ratio that the vapor/liquid mol ratio of the top of sideing stream of tower is of about 0.25 to the lower section of sideing stream of tower in about 0.55, and tower in tower is of about 0.50 to about 0.65.
It is a kind of to include that the stream of entering that include acrylonitrile, HCN and water is provided to head fraction column for the process that acrylonitrile is reclaimed；This is distilled in head fraction column to enter stream to produce the head fraction column column overhead stream including HCN, the bottom liquid stream including acrylonitrile, and the effluent for sideing stream from head fraction column including water and organic matter；Wherein, the ratio between vapor/liquid mol ratio for lower section of sideing stream of tower is of about 0.40 to about 1 in the vapor/liquid mol ratio and tower of the top of sideing stream of tower in tower.
A kind of head fraction column system includes：Head fraction column, it is configured to receive includes the stream of entering of acrylonitrile, HCN and water, and is also configured to be distilled in head fraction column into stream, and the head fraction column column overhead stream of HCN and bottom liquid stream including acrylonitrile are included with generation；Side stream, its be configured to from head fraction column remove water and organic matter admixture and before decanter is entered cooling water and organic matter the admixture；The decanter is configured to the admixture of the water and organic matter in separated flow and organic streams；Current divider, it is configured to receive organic streams from decanter and organic streams are divided into at least two plumes；It is configured to for one in organic streams to be sent at least one reflux pipeline of head fraction column in top of sideing stream；Be configured to for one in organic streams to be sent at least one reflux pipeline of head fraction column in lower section of sideing stream.
Brief description of the drawings
According to the following drawings, if the above and other aspects, features and advantages of the drying method of the process will become apparent.
Fig. 1 shows head fraction column system.
Fig. 2 shows the head fraction column system with pump circulation (pump around).
Fig. 3 shows the another aspect of the head fraction column system with pump circulation.
Corresponding reference number represents the counterpart member of some views through accompanying drawing.It will be recognized that the element in accompanying drawing shows in order to simple and clear, and be not necessarily drawn to scale.For example, the big I of some elements in accompanying drawing is exaggerated relative to other elements, to contribute to the understanding of improvement various aspects.In addition, the useful or required common but well-understood element of the aspect in commericially feasible is not drawn generally, hinder less in order to the observation to these various aspects.
Specific embodiment
Hereinafter describe not consider in a limiting sense, be only used for describing the General Principle of example embodiment and making.The scope of the present invention should determine with reference to claim.
A kind of process and equipment include head fraction column.Head fraction column receives crude product nitrile and enters stream (it includes acrylonitrile, HCN and water).Distillation in head fraction column is there is provided the head fraction column column overhead stream including hydrogen cyanide (HCN) at head fraction column top, and the head fraction column bottom liquid including acrylonitrile product at head fraction column bottom.Column distillation causes both hydrogen cyanide and water to be removed from acrylonitrile.
Head fraction column column overhead stream is sent to head fraction column condenser, here, a part is condensed using cooling agent.Uncooled steam from head fraction column condenser is sent to head fraction column relief condenser, here, a part is condensed using cooling agent.The process includes two kind condensate liquid streams of the combination from head fraction column condenser and head fraction column relief condenser, and those are streamed into head fraction column reflux pump.A part for the liquid flow of the combination is back to the top of head fraction column as backflow, and remainder is used as product or throws aside.
The process is included in and whole liquid distillates is removed at the centre portion of head fraction column, and the cut is delivered into effluent cooler and decanter is then sent to.Before, liquid distillate will first go to heat exchanger, here, the colder organic streams from decanter will cool down whole liquid distillate streams.Then whole liquid distillate stream will advance to head fraction column decanter, be separated herein.The water of the water side from decanter mutually can go to recovery tower feed manifold.The acrylonitrile of the organic matter side from decanter mutually returns to head fraction column.
In one aspect, the process include providing head fraction column include acrylonitrile, HCN and water enter stream.As shown in figure 1, entering stream 34 enters head fraction column 30 at the upper curtate of head fraction column 30 at head fraction column feed stream 36.In one aspect, feed stream 36 may correspond to any one in the number of plates 40 to 45 of head fraction column 30, and in another aspect, corresponding to the number of plates 42 of head fraction column 30.Entering stream 34 may include about 82 to about 90 acrylonitrile and about 5 to about 13 HCN of percentage by weight of percentage by weight.
The process is distilled into stream 34 in being included in head fraction column 30, and the head fraction column column overhead stream 51 of HCN and bottom liquid stream 58 including acrylonitrile are included to produce.The process includes the 44 removal effluents 46 that side stream from head fraction column 30.In one aspect, 44 are sideed stream at the centre portion of head fraction column 30.In another aspect, side stream 44 any one that may correspond in the number of plates 18 to 23 of head fraction column 30 (it includes 62 column plates), and in another aspect, corresponding to the number of plates 21 of head fraction column 30.Effluent 46 includes water and organic matter.
In one aspect, 44 allowing in tower of sideing stream are taken out at the height of effluent 46, effluent 46 includes about 90 to about 95 acrylonitrile of percentage by weight, and in another aspect, about 92 to about 93 acrylonitrile of percentage by weight, and about 5 to about 10 water of percentage by weight, and in another aspect, about 7 to about 8 water of percentage.
As shown in figure 1, the process may include continuously to remove effluent 46 from head fraction column 30 using effluent pump 39.The process includes cooling effluent 46 to provide the effluent 49 of cooling.Process shown in Fig. 1 includes making effluent 46 pass through first heat exchanger 35 and second heat exchanger 37.The process provides the effluent 49 of cooling, and the effluent 49 of the cooling had about 35 DEG C to about 45 DEG C, and about 38 DEG C to about 42 DEG C of temperature in another aspect before decanter 33 is entered.The separation of water and organic matter is improved to the effluent 49 that decanter 33 provides the cooling.
Water and organic material are separated in decanter 33.Pump (not shown) removes water phase 42 from decanter 33.Organic streams pump 31 removes organic streams 48 from decanter 33.In decanter 33, a phase is mainly water (about 93%), and another is mutually acrylonitrile (about 95%).Water is pumped to recovery tower feed manifold (not shown) from the water side of decanter 33.The acrylonitrile of the organic matter side from decanter 33 is mutually pumped back head fraction column 30.
Decanter discharge stream 47 can be sent to washer (not shown).Organic streams 48 are transferred into first heat exchanger 35, and it provides cooling stream herein.Organic streams 48 enter head fraction column 30 at organic streams entrance 54.Organic streams entrance 54 can be at the centre portion of head fraction column 30.In this aspect, organic streams entrance 54 is sideing stream below 44.
In another aspect, the process includes for head fraction column column overhead stream 51 being sent to head fraction column condenser 55.Head fraction column column overhead stream 51 is condensed using condenser coolant stream 53 in head fraction column condenser 55.In in this regard, condenser coolant stream 53 is antifreezing agent or chilled water.Condenser coolant stream 53 has about -10 DEG C to about+10 DEG C of temperature, in another aspect, about -10 DEG C to about+5 DEG C.Vapor/liquid stream 92 is sent to vapour/liquid separator 94.Uncooled steam 58 from vapour/liquid separator 94 is sent to head fraction column relief condenser 90.Uncooled steam 58 is condensed in the head fraction column relief condenser 90 cooled down by discharge coolant flow 61.In in this regard, discharge coolant flow 61 can be antifreezing agent or chilled water.Discharge coolant flow 61 has about -10 DEG C to about+10 DEG C of temperature, in another aspect, about -10 DEG C to about+5 DEG C.Vapor/liquid stream 96 is sent to second liquid/vapour separator 98.
In another aspect, the process includes combination head fraction column condenser condensate 63 and head fraction column relief condenser condensate 65, to form the condensate flow 67 of combination.The condensate flow 67 of combination is also sent to the process top section of head fraction column 30 using condensate pump 71.The process may include a part for the condensate flow 67 for extracting combination out at outlet port 74.The condensate flow 67 of combination can return to the top section of head fraction column 30 at head fraction column condensate entrance 76.
As shown in Fig. 2 and similar to Fig. 1, the process include providing head fraction column include acrylonitrile, HCN and water enter stream.As shown in Fig. 2 enter entering head fraction column 30 at the upper curtate of head fraction column 30 of the stream 34 at head fraction column feed stream 36.In one aspect, feed stream 36 may correspond to any one in the number of plates 40 to 45 of head fraction column 30 (it includes 62 column plates), and in one aspect, corresponding to the number of plates 42 of head fraction column 30.The process is distilled into stream 34 in being included in head fraction column 30, and the head fraction column column overhead stream 51 of HCN and bottom liquid stream 58 including acrylonitrile are included to produce.In in this regard, bottom liquid stream 58 includes about 500ppm or less HCN, in another aspect, about 0 to about 500ppm HCN, in another aspect, about 1 to about 400ppm HCN, in another aspect, about 1 to about 250ppm HCN, and in another aspect, about 1 to about 100ppm HCN.Bottom liquid stream 58 may also comprise about 0.1 to about 0.5 water of percentage by weight, in another aspect, about 0.1 to about 0.25 water of percentage by weight.
Head fraction column column overhead stream 51 includes about 100ppm or less acrylonitrile, in another aspect, about 0 to about 100ppm acrylonitrile, in another aspect, about 1 to about 90ppm acrylonitrile, in another aspect, about 5 to about 50ppm acrylonitrile, in another aspect, about 5 to about 25ppm acrylonitrile, and in another aspect, about 1 to about 10ppm acrylonitrile.Head fraction column column overhead stream 51 may include about 0.25 to about 0.75 water of percentage by weight, in another aspect, about 0.4 to about 0.6 water of percentage by weight.
The process includes the 44 removal effluents 46 that side stream from head fraction column 30.In one aspect, 44 are sideed stream at the centre portion of head fraction column 30.In another aspect, side stream 44 any one that may correspond in the number of plates 18 to 23 of head fraction column 30, and in one aspect, corresponding to the number of plates 21 of head fraction column 30.Effluent 46 includes water and organic matter.
In an aspect, and different from the process of Fig. 1, the process shown in Fig. 2 includes for effluent 46 being sent to heat exchanger 38.In in this regard, effluent 46 can be fed using gravity and flow to heat exchanger 38.The process was provided before decanter 33 is entered has about 35 DEG C to about 45 DEG C and the in another aspect effluent 49 of the cooling of about 38 DEG C to about 42 DEG C of temperature.In the aspect of the process shown in Fig. 2, the process does not need pump that effluent 46 is sent into heat exchanger 38, and only needs single heat exchanger before entering in decanter 33.
In another aspect, water and organic material are separated in decanter 33.Pump (not shown) removes water phase 42 from decanter 33.Organic streams pump 31 removes organic streams 48 from decanter 33.Different from Fig. 1, the process shown in Fig. 2 includes for organic streams 48 being sent to current divider 71.Organic streams 48 are divided into the first organic streams 73 and the second organic streams 75 by current divider.In in this regard, current divider 71 provides about 40 to about 60 weight % of organic streams 48 to the first organic streams 73 or the second organic streams 75.
In another aspect, the process includes making the first organic streams 73 and the second organic streams 75 return to head fraction column 30 at two separate positions of head fraction column 30.In in this regard, the process includes making the first organic streams 73 return to the first organic streams of head fraction column entrance 77, and the second organic streams 75 is returned to the second organic streams of head fraction column entrance 79.In one aspect, the process includes making the first organic streams 73 return to the first organic streams entrance 77, it is about 5 to about 1 column plates of 44 tops of sideing stream of head fraction column 30, in another aspect, about 4 to about 1 column plate, in another aspect, about 3 to about 1 column plates, in another aspect, about 2 to about 1 column plates, and in another aspect, about 1 column plate of 44 tops of sideing stream of head fraction column 30.In another aspect, the process includes making the second organic streams 75 return to the second organic streams entrance 79, it is about 5 to about 1 column plate of 44 lower sections of sideing stream of head fraction column 30, about 4 to about 1 column plate, in another aspect, about 3 to about 1 column plate, in another aspect, about 2 to about 1 column plate, and in another aspect, about 1 column plate of 44 lower sections of sideing stream of head fraction column 30.
In another aspect and different from Fig. 1, the process shown in Fig. 2 includes for decanter discharge stream 47 being sent to head fraction column 30.In in this regard, decanter discharge stream 47 can enter head fraction column 30 at decanter discharge inflow entrance 81.Decanter discharge inflow entrance 81 may correspond to the position on head fraction column with the 44 identical column plates that side stream.Decanter discharge stream 47 can liquid from side stream 44 removal when be used as balanced line.
Heat load between Fig. 1 and the process of Fig. 2 is compared as follows.
The comparing of the process of Fig. 1 and Fig. 2 shows that the shunting shown in fig. 2 of the condenser duty of head fraction column reduces about 13% in the case of returning.The change of heat load changes into the saving of refrigeration.The change of heat load is substantially transferred to effluent heat exchanger 38, and effluent heat exchanger 38 uses cooling water, and cooling water is more cheap public things.Although the thermal balance around head fraction column significantly changes due to processing equipment and operation change, the overall net change of cooling and reboiler duty between Fig. 1 and Fig. 2 is smaller, it is expected to be 0.62% and 0.43%.In in this regard, effluent heat exchanger 38 has 3165kw or smaller heat load, and in another aspect, about 1410 arrive about 2350kw, and in another aspect, about 2350 to about 3165kw (the acrylonitrile yield based on 260-350kta).In another aspect, the ratio between heat load in the heat load in head fraction column condenser 55 and effluent heat exchanger 38 is of about 4.7 or smaller, in another aspect, about 2.5 or smaller, in another aspect, about 2 to about 3, and in another aspect, about 2.5 to about 4.7.
In one aspect, the process shown in Fig. 2 provides the removal of a heat exchanger and pump, and the reduction that refrigeration communal facility is required.The practical example of the benefit can manifest during fouled condition.When overhead tower starts fouling, the operation of tower tends to needing increasing backflow to maintain identical pureness specifications, must shut off to be cleaned until final tower.Because the pump circulation to column plate 22 is to increase the source of backflow, therefore which results in the relatively low condenser duty related to the fouled condition in head fraction column.
In another aspect, the process operates head fraction column under being included in certain vapor/liquid mol ratio.In in this regard, sideed stream in head fraction column 30 44 top vapor/liquid mol ratio be of about 0.25 to about 0.55, in another aspect, about 0.26 to about 0.51, in another aspect, 0.26 to about 0.48, in another aspect, about 0.45 to about 0.55, in another aspect, about 0.46 to about 0.51, and in another aspect, about 0.49 to about 0.51.In one aspect, including the vapor/liquid mol ratio of the top of sideing stream of process that returns of shunting is of about 0.25 to about 0.50, and in another aspect, about 0.26 to about 0.48.In another aspect, including single return process side stream top vapor/liquid mol ratio be of about 0.49 to about 0.51.
Sideed stream in head fraction column 30 44 lower section vapor/liquid mol ratio be of about 0.4 to about 1, in another aspect, about 0.5 to about 0.65, in another aspect, about 0.55 to about 0.65, in another aspect, about 0.54 to 0.61, in another aspect, about 0.56 to about 0.62, and in another aspect, about 0.58 to about 0.61.On the one hand, including the vapor/liquid mol ratio of the lower section of sideing stream of process that returns of shunting is of about 0.5 to about 0.65, and in another aspect, about 0.54 to about 0.61.In another aspect, including single return process side stream lower section vapor/liquid mol ratio be of about 0.58 to about 0.61.
In another aspect, the process operates head fraction column under being included in certain vapor/liquid mol ratio.In in this regard, side stream the ratio between the vapor/liquid mol ratio of 44 lower sections in vapor/liquid mol ratio and the head fraction column 30 of 44 tops of being sideed stream in head fraction column 30 is of about 0.4 to about 0.9, in another aspect, about 0.44 to about 0.88, in another aspect, about 0.75 to about 0.90, in another aspect, about 0.77 to about 0.82, and in another aspect, about 0.82 to about 0.87.In another aspect, during being returned including shunting, side stream the ratio between the vapor/liquid mol ratio of 44 lower sections in vapor/liquid mol ratio and the head fraction column 30 of 44 tops of being sideed stream in head fraction column 30 is of about 0.4 to about 0.85, and in another aspect, about 0.44 to about 0.83.In another aspect, during including single return, side stream the ratio between the vapor/liquid mol ratio of 44 lower sections in vapor/liquid mol ratio and the head fraction column 30 of 44 tops of being sideed stream in head fraction column 30 is of about 0.8 to about 0.9, and in another aspect, about 0.81 to about 0.83.
Sideed stream in head fraction column 30 44 top vapor/liquid ratio can calculate as follows：
Flow velocity/(flow velocity entered in stream 34)+(flow velocity of the combined condensates stream 67 at head fraction column entrance 76) in head fraction column column overhead stream 51
Sideed stream in head fraction column 30 44 lower section vapor/liquid ratio can calculate as follows：
The flow velocity of flow velocity/the second organic streams 75 in head fraction column column overhead stream 51.
Fig. 3 includes additional heat exchanger 99 similar to Fig. 1, simply Fig. 3.
Although, by means of specific embodiment, example and its application description, those skilled in the art can various modifications may be made and modification to it, without deviating from the scope of the present invention illustrated in claim for present invention disclosed herein.
Claims (111)
1. it is a kind of for acrylonitrile reclaim process, it includes：
The stream of entering for including acrylonitrile, HCN and water is provided to head fraction column；
Enter stream described in being distilled in the head fraction column to produce the head fraction column column overhead stream including HCN and the bottom liquid stream including acrylonitrile；
From the removal effluent that sides stream including water and the head fraction column of organic matter；
At least some water and organic matter are separated from the effluent to provide organic streams；
The organic streams are made to return to the head fraction column；With
The amount and the ratio of the amount of the organic streams that the head fraction column is returned in the lower section of sideing stream from the effluent of the removal of sideing stream of the head fraction column are adjusted, 500ppm or less HCN is provided with to the bottom liquid stream.
2. process according to claim 1, it is characterised in that the organic streams were divided at least two plumes before its described head fraction column of return.
3. process according to claim 2, it is characterised in that one in organic streams returns to the head fraction column in the top of sideing stream of the head fraction column, and one is returned in the lower section of sideing stream of the head fraction column.
4. process according to claim 3, it is characterised in that one in organic streams returns to the head fraction column from about 5 to about 1 column plates of the top of sideing stream of the head fraction column.
5. process according to claim 3, it is characterised in that one in organic streams returns to the head fraction column from about 1 column plate of the lower section of sideing stream of the head fraction column.
6. process according to claim 2, it is characterised in that one returned in two strands of organic streams of the head fraction column includes about 40 to about 60 weight % of organic matter.
7. process according to claim 1, it is characterised in that the effluent is cooled down from after head fraction column removal.
8. process according to claim 7, it is characterised in that the effluent is cooled down at least one heat exchanger.
9. process according to claim 8, it is characterised in that the effluent is cooled down at least two heat exchangers.
10. process according to claim 8, it is characterised in that the effluent is fed by gravity and is transferred into the heat exchanger.
11. processes according to claim 1, it is characterised in that it is described side stream in water and organic matter separated in decanter.
12. processes according to claim 11, it is characterised in that the discharge stream from the decanter returns to the head fraction column.
13. processes according to claim 8, it is characterised in that the head fraction column column overhead stream is transferred into head fraction column condenser.
14. processes according to claim 13, it is characterised in that the ratio between heat load in heat load in the head fraction column condenser and effluent heat exchanger is of about 2.5 or smaller.
15. processes according to claim 1, it is characterised in that the head fraction column column overhead stream has 100ppm or less acrylonitrile.
A kind of 16. processes reclaimed for acrylonitrile, it includes：
The stream of entering for including acrylonitrile, HCN and water is provided to head fraction column；
Enter stream described in being distilled in the head fraction column to produce the head fraction column column overhead stream including HCN and the bottom liquid stream including acrylonitrile；
From the removal effluent that sides stream including water and the head fraction column of organic matter；
At least some water and organic matter is set to be separated with the effluent；With
The organic matter is divided at least two plumes, and the stream is returned at least two points of positions opened on the head fraction column.
17. processes according to claim 16, it is characterised in that one in organic streams returns to the head fraction column in the top of sideing stream of the head fraction column, and one is returned in the lower section of sideing stream of the head fraction column.
18. processes according to claim 17, it is characterised in that one in organic streams returns to the head fraction column from about 5 to about 1 column plates of the top of sideing stream of the head fraction column.
19. processes according to claim 17, it is characterised in that one in organic streams returns to the head fraction column from about 1 column plate of the lower section of sideing stream of the head fraction column.
20. processes according to claim 17, it is characterised in that return to one of two plumes of the head fraction column including organic matter about 40 to about 60 weight %.
21. processes according to claim 16, it is characterised in that the effluent is cooled down from after head fraction column removal.
22. processes according to claim 21, it is characterised in that the effluent is cooled down at least one heat exchanger.
23. processes according to claim 22, it is characterised in that the effluent is cooled down at least two heat exchangers.
24. processes according to claim 22, it is characterised in that the effluent is fed by gravity and is transferred into the heat exchanger.
25. processes according to claim 16, it is characterised in that water and organic matter are separated in decanter.
26. processes according to claim 25, it is characterised in that the discharge stream from the decanter returns to the head fraction column.
27. processes according to claim 22, it is characterised in that the head fraction column column overhead stream is transferred into head fraction column condenser.
28. processes according to claim 27, it is characterised in that the ratio between heat load in heat load in the head fraction column condenser and effluent heat exchanger is of about 2.5 or smaller.
29. processes according to claim 16, it is characterised in that the bottom liquid stream has 500ppm or less HCN.
30. processes according to claim 16, it is characterised in that the head fraction column column overhead stream has 100ppm or less acrylonitrile.
A kind of 31. processes for operating head fraction column, it includes：
The stream of entering for including acrylonitrile, HCN and water is provided to the head fraction column；
Enter stream described in being distilled in the head fraction column to produce head fraction column column overhead stream, and the head fraction column overhead is streamed to head fraction column condenser；
Include the effluent of water and organic matter from the removal of sideing stream of the head fraction column, and the effluent be sent into effluent heat exchanger providing the effluent of cooling；
At least some water and organic matter are separated from the effluent of the cooling；
Organic streams are made to return to the head fraction column；With
The amount of the organic streams returned in the top of sideing stream of the head fraction column and the ratio of the amount of the organic streams that head fraction column is returned in the lower section of sideing stream are adjusted, to provide the ratio between heat load in heat load and effluent heat exchanger in about 2.5 or smaller head fraction column condenser.
32. processes according to claim 31, it is characterised in that the organic streams were divided at least two plumes before its described head fraction column of return.
33. processes according to claim 31, it is characterised in that the tower includes about 15 to about 30 column plates of the lower section of sideing stream.
34. processes according to claim 33, it is characterised in that the tower includes about 18 to about 25 column plates of the lower section of sideing stream.
35. processes according to claim 34, it is characterised in that the tower includes about 18 to about 22 column plates of the lower section of sideing stream.
36. processes according to claim 31, it is characterised in that the tower includes about 30 to about 50 column plates of the top of sideing stream.
37. processes according to claim 36, it is characterised in that the tower includes about 32 to about 48 column plates of the top of sideing stream.
38. process according to claim 37, it is characterised in that the tower includes about 38 to about 44 column plates of the top of sideing stream.
39. processes according to claim 32, it is characterised in that one in organic streams returns to the head fraction column in the top of sideing stream of the head fraction column, and one is returned in the lower section of sideing stream of the head fraction column.
40. process according to claim 39, it is characterised in that one in organic streams returns to the head fraction column from about 5 to about 1 column plates of the top of sideing stream of the head fraction column.
41. process according to claim 39, it is characterised in that one in organic streams returns to the head fraction column from about 1 column plate of the lower section of sideing stream of the head fraction column.
42. processes according to claim 32, it is characterised in that return to one about 40 to the about 60 weight % including organic matter in two strands of organic streams of the head fraction column.
43. processes according to claim 31, it is characterised in that the effluent is cooled down at least one heat exchanger.
44. processes according to claim 43, it is characterised in that the effluent is cooled down at least two heat exchangers.
45. processes according to claim 43, it is characterised in that the effluent is fed by gravity and is transferred into the heat exchanger.
46. processes according to claim 31, it is characterised in that it is described side stream in water and organic matter separated in decanter.
47. processes according to claim 46, it is characterised in that the discharge stream from the decanter returns to the head fraction column.
48. processes according to claim 31, it is characterised in that the head fraction column column overhead stream is transferred into head fraction column condenser.
49. processes according to claim 31, it is characterised in that the bottom liquid stream has 500ppm or less HCN.
50. processes according to claim 31, it is characterised in that the head fraction column column overhead stream has 100ppm or less acrylonitrile.
A kind of 51. processes reclaimed for acrylonitrile, it includes：
The stream of entering for including acrylonitrile, HCN and water is provided to head fraction column；
Enter stream described in being distilled in the head fraction column to produce the head fraction column column overhead stream including HCN, the bottom liquid stream including acrylonitrile, and the effluent for sideing stream from head fraction column including water and organic matter；
Wherein, the vapor/liquid mol ratio of the top of sideing stream of tower described in the tower is of about 0.25 to about 0.55, and the vapor/liquid mol ratio of the lower section of sideing stream of tower described in tower is of about 0.50 to about 0.65.
52. processes according to claim 51, it is characterised in that the tower includes about 15 to about 30 column plates of the lower section of sideing stream.
53. processes according to claim 52, it is characterised in that the tower includes about 18 to about 25 column plates of the lower section of sideing stream.
54. processes according to claim 53, it is characterised in that the tower includes about 18 to about 22 column plates of the lower section of sideing stream.
55. processes according to claim 51, it is characterised in that the tower includes about 30 to about 50 column plates of the top of sideing stream.
56. processes according to claim 55, it is characterised in that the tower includes about 32 to about 48 column plates of the top of sideing stream.
57. processes according to claim 56, it is characterised in that the tower includes about 38 to about 44 column plates of the top of sideing stream.
58. processes according to claim 51, it is characterised in that the process includes the cooling effluent to provide the effluent of cooling.
59. processes according to claim 58, it is characterised in that the process includes the effluent separation water and organic matter from the cooling.
60. processes according to claim 51, it is characterised in that the organic streams are divided at least two plumes and return to the head fraction column.
61. processes according to claim 60, it is characterised in that one in organic streams returns to the head fraction column in the top of sideing stream of the head fraction column, and one is returned in the lower section of sideing stream of the head fraction column.
62. processes according to claim 61, it is characterised in that one in organic streams returns to the head fraction column from about 5 to about 1 column plates of the top of sideing stream of the head fraction column.
63. processes according to claim 61, it is characterised in that one in organic streams returns to the head fraction column from about 1 column plate of the lower section of sideing stream of the head fraction column.
64. processes according to claim 60, it is characterised in that return to one about 40 to the about 60 weight % including organic matter in two strands of organic streams of the head fraction column.
65. processes according to claim 58, it is characterised in that the effluent is cooled down at least one heat exchanger.
66. processes according to claim 65, it is characterised in that the effluent is cooled down at least two heat exchangers.
67. processes according to claim 65, it is characterised in that the effluent is fed by gravity and is transferred into the heat exchanger.
68. processes according to claim 59, it is characterised in that it is described side stream in water and organic matter separated in decanter.
69. processes according to claim 68, it is characterised in that the discharge stream from the decanter returns to the head fraction column.
70. processes according to claim 65, it is characterised in that the head fraction column column overhead stream is transferred into head fraction column condenser.
71. processes according to claim 70, it is characterised in that the ratio between heat load in heat load in the head fraction column condenser and effluent heat exchanger is of about 2.5 or smaller.
72. processes according to claim 51, it is characterised in that the bottom liquid stream has 500ppm or less HCN.
73. processes according to claim 51, it is characterised in that the head fraction column column overhead stream has 100ppm or less acrylonitrile.
A kind of 74. processes reclaimed for acrylonitrile, it includes：
The stream of entering for including acrylonitrile, HCN and water is provided to head fraction column；
Enter stream described in being distilled in the head fraction column to produce the head fraction column column overhead stream including HCN, the bottom liquid stream including acrylonitrile, and the effluent for sideing stream from head fraction column including water and organic matter；
Wherein, the ratio between vapor/liquid mol ratio for lower section of sideing stream of tower described in the vapor/liquid mol ratio of the top sideed stream of tower described in tower and tower is of about 0.40 to about 1.0.
75. process according to claim 74, it is characterised in that the tower includes about 15 to about 30 column plates of the lower section of sideing stream.
76. process according to claim 75, it is characterised in that the tower includes about 18 to about 25 column plates of the lower section of sideing stream.
77. process according to claim 76, it is characterised in that the tower includes about 18 to about 22 column plates of the lower section of sideing stream.
78. process according to claim 74, it is characterised in that the tower includes about 30 to about 50 column plates of the top of sideing stream.
79. process according to claim 78, it is characterised in that the tower includes about 32 to about 48 column plates of the top of sideing stream.
80. process according to claim 79, it is characterised in that the tower includes about 38 to about 44 column plates of the top of sideing stream.
81. process according to claim 74, it is characterised in that the process includes the cooling effluent to provide the effluent of cooling.
82. process according to claim 81, it is characterised in that the process includes the effluent separation water and organic matter from the cooling.
83. process according to claim 82, it is characterised in that the organic streams are divided at least two plumes and return to the head fraction column.
84. process according to claim 83, it is characterised in that one in organic streams returns to the head fraction column in the top of sideing stream of the head fraction column, and one is returned in the lower section of sideing stream of the head fraction column.
85. process according to claim 84, it is characterised in that one in organic streams returns to the head fraction column from about 5 to about 1 column plates of the top of sideing stream of the head fraction column.
86. process according to claim 84, it is characterised in that one in organic streams returns to the head fraction column from about 1 column plate of the lower section of sideing stream of the head fraction column.
87. process according to claim 83, it is characterised in that return to one about 40 to the about 60 weight % including organic matter in two strands of organic streams of the head fraction column.
88. process according to claim 81, it is characterised in that the effluent is cooled down at least one heat exchanger.
89. process according to claim 88, it is characterised in that the effluent is cooled down at least two heat exchangers.
90. process according to claim 89, it is characterised in that the effluent is fed by gravity and is transferred into the heat exchanger.
91. process according to claim 74, it is characterised in that it is described side stream in water and organic matter separated in decanter.
92. process according to claim 91, it is characterised in that the discharge stream from the decanter returns to the head fraction column.
93. process according to claim 88, it is characterised in that the head fraction column column overhead stream is transferred into head fraction column condenser.
94. process according to claim 93, it is characterised in that the ratio between heat load and heat load in the effluent heat exchanger are of about 2.5 or smaller in the head fraction column condenser.
95. process according to claim 74, it is characterised in that the bottom liquid stream has 500ppm or less HCN.
96. process according to claim 74, it is characterised in that the head fraction column column overhead stream has 100ppm or less acrylonitrile.
A kind of 97. head fraction column systems, including：
Head fraction column, it is configured to receive includes the stream of entering of acrylonitrile, HCN and water, and is also configured to enter stream described in distillation in the head fraction column, and the head fraction column column overhead stream of HCN and bottom liquid stream including acrylonitrile are included with generation；
Side stream, its be configured to from the head fraction column remove water and organic matter admixture and before decanter is entered cooling water and organic matter the admixture；
The decanter is configured to the admixture of the water and organic matter in separated flow and organic streams；
Current divider, it is configured to receive organic streams from the decanter and the organic streams are divided into at least two plumes；
It is configured to for one in organic streams to be sent at least one return line of the head fraction column in the top of sideing stream；With
It is configured to for one in organic streams to be sent at least one return line of the head fraction column in the lower section of sideing stream.
98. system according to claim 97, it is characterised in that one in organic streams returns to the head fraction column from about 5 to about 1 column plates of the top of sideing stream of the head fraction column.
99. system according to claim 97, it is characterised in that one in organic streams returns to the head fraction column from about 1 column plate of the lower section of sideing stream of the head fraction column.
100. system according to claim 97, it is characterised in that return to one about 40 to the about 60 weight % including organic matter in two plumes of the head fraction column.
101. system according to claim 97, it is characterised in that described sideing stream is cooled down at least one heat exchanger.
102. system according to claim 101, it is characterised in that the effluent point is fed by gravity and is transferred into the heat exchanger.
103. system according to claim 97, it is characterised in that the discharge stream from the decanter returns to the head fraction column.
104. system according to claim 101, it is characterised in that the head fraction column column overhead stream is transferred into head fraction column condenser.
105. system according to claim 104, it is characterised in that the ratio between heat load and heat load in the heat exchanger that sides stream are of about 2.5 or smaller in the head fraction column condenser.
106. system according to claim 97, it is characterised in that the tower includes about 15 to about 30 column plates of the lower section of sideing stream.
107. system according to claim 106, it is characterised in that the tower includes about 18 to about 25 column plates of the lower section of sideing stream.
108. system according to claim 107, it is characterised in that the tower includes about 18 to about 22 column plates of the lower section of sideing stream.
109. system according to claim 97, it is characterised in that the tower includes about 30 to about 50 column plates of the top of sideing stream.
110. system according to claim 109, it is characterised in that the tower includes about 32 to about 48 column plates of the top of sideing stream.
111. system according to claim 110, it is characterised in that the tower includes about 38 to about 44 column plates of the top of sideing stream.
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510782236.XA CN106699599A (en) | 2015-11-16 | 2015-11-16 | Heads column pump circulation |
| CN202210464254.3A CN114870421A (en) | 2015-11-16 | 2015-11-16 | Head fraction column pump cycle |
| PCT/US2016/060252 WO2017087175A1 (en) | 2015-11-16 | 2016-11-03 | Hcn heads column pump around for acrylonitrile recovery |
| RU2018120739A RU2721779C2 (en) | 2015-11-16 | 2016-11-03 | Circulatory reflux of overhead tower |
| TR2018/06463T TR201806463T1 (en) | 2015-11-16 | 2016-11-03 | Head column with pump around. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510782236.XA CN106699599A (en) | 2015-11-16 | 2015-11-16 | Heads column pump circulation |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210464254.3A Division CN114870421A (en) | 2015-11-16 | 2015-11-16 | Head fraction column pump cycle |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106699599A true CN106699599A (en) | 2017-05-24 |
Family
ID=57389524
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510782236.XA Pending CN106699599A (en) | 2015-11-16 | 2015-11-16 | Heads column pump circulation |
| CN202210464254.3A Pending CN114870421A (en) | 2015-11-16 | 2015-11-16 | Head fraction column pump cycle |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210464254.3A Pending CN114870421A (en) | 2015-11-16 | 2015-11-16 | Head fraction column pump cycle |
Country Status (4)
| Country | Link |
|---|---|
| CN (2) | CN106699599A (en) |
| RU (1) | RU2721779C2 (en) |
| TR (1) | TR201806463T1 (en) |
| WO (1) | WO2017087175A1 (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1545499A (en) * | 2001-08-21 | 2004-11-10 | 标准石油公司 | Improved operation of head fraction column in acrylonitrile production |
| CN104922923A (en) * | 2014-03-21 | 2015-09-23 | 英尼奥斯欧洲股份公司 | Inhibitor adding head fraction tower operation |
| CN104922926A (en) * | 2014-03-21 | 2015-09-23 | 英尼奥斯欧洲股份公司 | Head fraction tower tower-top system |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU373271A1 (en) * | 1969-12-08 | 1973-03-12 | METHOD OF ACRYLONITRILE REGENERATION | |
| RU2263108C1 (en) * | 2001-08-21 | 2005-10-27 | Дзе Стэндард Ойл Компани | Method for extraction of acrylonitrile, methacrylonitrile or hydrogen cyanide |
| KR101528986B1 (en) * | 2010-12-27 | 2015-06-15 | 아사히 가세이 케미칼즈 가부시키가이샤 | Method for purifying acrylonitrile |
| WO2013146609A1 (en) * | 2012-03-26 | 2013-10-03 | 旭化成ケミカルズ株式会社 | Method for purifying acetonitrile |
-
2015
- 2015-11-16 CN CN201510782236.XA patent/CN106699599A/en active Pending
- 2015-11-16 CN CN202210464254.3A patent/CN114870421A/en active Pending
-
2016
- 2016-11-03 RU RU2018120739A patent/RU2721779C2/en active
- 2016-11-03 WO PCT/US2016/060252 patent/WO2017087175A1/en active Application Filing
- 2016-11-03 TR TR2018/06463T patent/TR201806463T1/en unknown
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1545499A (en) * | 2001-08-21 | 2004-11-10 | 标准石油公司 | Improved operation of head fraction column in acrylonitrile production |
| CN104922923A (en) * | 2014-03-21 | 2015-09-23 | 英尼奥斯欧洲股份公司 | Inhibitor adding head fraction tower operation |
| CN104922926A (en) * | 2014-03-21 | 2015-09-23 | 英尼奥斯欧洲股份公司 | Head fraction tower tower-top system |
Non-Patent Citations (1)
| Title |
|---|
| 张平: "21.2万吨／年丙烯腈生产装置回收和精制过程的模拟分析", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| RU2721779C2 (en) | 2020-05-22 |
| RU2018120739A (en) | 2019-12-18 |
| RU2018120739A3 (en) | 2020-01-30 |
| TR201806463T1 (en) | 2018-07-23 |
| WO2017087175A1 (en) | 2017-05-26 |
| CN114870421A (en) | 2022-08-09 |
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