CN104107559A - Pollution reduction in acetonitrile removing step in acrylonitrile recovery - Google Patents

Pollution reduction in acetonitrile removing step in acrylonitrile recovery Download PDF

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Publication number
CN104107559A
CN104107559A CN201410256722.3A CN201410256722A CN104107559A CN 104107559 A CN104107559 A CN 104107559A CN 201410256722 A CN201410256722 A CN 201410256722A CN 104107559 A CN104107559 A CN 104107559A
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China
Prior art keywords
stream
tower
acid
acetonitrile
fractionator
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CN201410256722.3A
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Chinese (zh)
Inventor
T.R.麦克唐奈
J.R.库奇
D.R.瓦纳
P.T.瓦赫滕多夫
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Ineos Europe AG
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Ineos Europe AG
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Priority to CN201410256722.3A priority Critical patent/CN104107559A/en
Priority to CN201811122752.XA priority patent/CN109499085A/en
Publication of CN104107559A publication Critical patent/CN104107559A/en
Priority to JP2016572412A priority patent/JP6761758B2/en
Priority to TR2016/17300T priority patent/TR201617300T1/en
Priority to PCT/US2015/034826 priority patent/WO2015191528A1/en
Priority to EA201692339A priority patent/EA034228B1/en
Priority to TW104118782A priority patent/TWI715532B/en
Priority to SA516380473A priority patent/SA516380473B1/en
Pending legal-status Critical Current

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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
    • B01D3/42Regulation; Control
    • B01D3/4211Regulation; Control of columns
    • B01D3/4216Head stream
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C253/00Preparation of carboxylic acid nitriles
    • C07C253/32Separation; Purification; Stabilisation; Use of additives
    • C07C253/34Separation; Purification

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

A method is provided. The method includes adding an acid to a refluxing material stream, and conveying the refluxing material stream to an acetonitrile fractionator, wherein the acid reduces pollution in the acetonitrile fractionator.

Description

The pollution that the acetonitrile that acrylonitrile reclaims removes in step alleviates
Technical field
The disclosure is directed to improved process and the system for manufacturing acrylonitrile or methacrylonitrile.Especially, the disclosure is directed to the acetonitrile that acrylonitrile reclaims and removes improved pollution in step and alleviate.
Background technology
The various processes and the system that are used for manufacturing acrylonitrile and methacrylonitrile are known; Referring to for example U.S. Patent No. 3,936,360, No.3,433,822, No.3,399,120 and No.3,535,849.Propylene, ammonia and oxygen (as constituent of air) are fed to acrylonitrile reactor, and acrylonitrile reactor comprises catalyst and moves as fluid bed.Conventional way is to carry out operant response device with respect to the propylene amount that is fed into reactor with excess of ammonia in charging.Some in extra ammonia burnt in reactor, and this is owing to being combined with propylene at it with the extreme condition before formation acrylonitrile.All the other extra ammonia, are commonly referred to as " excess ammonia " and in eluting gas, leave reactor.This gas then conventionally through cooler and then to quencher to remove excess ammonia.Referring to for example U.S. Patent No. 3,936,360, No.4,166,008, No. 4,334,965, No.4,341,535, No.5,895,635 and No.6,793,776.
Conventional process is usually directed to comprise propane by being selected from, hydrocarbon in the group of propylene or isobutene, there is recovery and the purifying of acrylonitrile/methacrylonitrile that the direct reaction in situation produces at catalyst in ammonia and oxygen, realize by following steps: the reactor effluent that comprises acrylonitrile/methacrylonitrile is transported to the first tower (chilling), in the first tower, utilize the first aqueous stream cooling reactor effluent, the cooling effluent that comprises acrylonitrile/methacrylonitrile is transported in the second tower (absorber), in the second tower, cooling effluent contacts acrylonitrile/methacrylonitrile to be absorbed in the second aqueous stream with the second aqueous stream, the second aqueous stream that comprises acrylonitrile/methacrylonitrile is transported to the first destilling tower (recovery tower) for separating crude acetonitrile/methacrylonitrile and the second aqueous stream from the second tower, and, crude acetonitrile/the methacrylonitrile of separation is transported to after-fractionating tower (head fraction column) to remove at least some impurity from crude acetonitrile/methacrylonitrile, and, partially purified acrylonitrile/methacrylonitrile is transported to the 3rd destilling tower (product tower) to obtain product acrylonitrile/methacrylonitrile.Referring to for example, U.S. Patent No. 4,334,295 and No.4,238,295, it discloses conventional process, wherein in single extraction distillation column, carries out separating of acetonitrile and acrylonitrile.In this conventional process, at the bottom of the tower of acetonitrile fractionator, distillate material stream and be sent to recovery tower or extraction distillation column.
The problem running in conventional process and system is hydrogen cyanide gathering in higher-boiling compound, and higher-boiling compound required temperature in acetonitrile fractionator is decomposed.The decomposition of higher-boiling compound discharges the hydrogen cyanide that is radical form, hydrogen cyanide polymerization and polluting in acetonitrile fractionator.Pollution may cause the poor operation of acetonitrile fractionator, and causes unit shut down to clean acetonitrile fractionating column and remove pollution.In addition, a small amount of ammonia is through quencher, because chilling reaction is not 100% efficient.This ammonia tends to gather.
Summary of the invention
Therefore, one side of the present disclosure is to provide a kind of and alleviates and/or remove pollute in acetonitrile fractionating column safe, effectively and have cost-benefit process and equipment.
On the one hand, provide a kind of process, it comprises: add acid to reflux stream; And reflux stream is transported to acetonitrile fractionator.
On the other hand, a kind of process comprise by the bottom of the tower of acetonitrile fractionating column, distillate material stream be transported to quench tower.In this regard, at the bottom of tower, distillate material stream and comprise at least some acid.
On the other hand, a kind of equipment comprises: acetonitrile fractionator, and it is configured to produce the tower top that comprises acetonitrile and distillates material stream; Reflux pipeline, it is configured to reflux stream to be transported to acetonitrile fractionator; And pipeline is added in acid, it is configured to add acid to reflux stream.
Read by reference to the accompanying drawings, by the detailed description of the application's illustrated embodiment below, above-mentioned and other side, feature and advantage of the present disclosure will be apparent.
Brief description of the drawings
In consideration of the drawings by reference to the following description, can obtain the understanding more comprehensively to the application's exemplary embodiment and its advantage, in the accompanying drawings, similar Reference numeral is indicated similar feature and in the accompanying drawings:
Fig. 1 is the schematic flow diagram according at least one aspect of the present disclosure.
Fig. 2 is the schematic flow diagram according at least one aspect of the present disclosure.
Fig. 3 is according to the flow chart of the method 300 of aspect of the present disclosure.
Detailed description of the invention
On the one hand, provide a kind of method or process, it comprises the step of the acid in reflux stream being added to acetonitrile fractionator.On the one hand, this process comprises reflux stream is transported to acetonitrile fractionator, acetonitrile fractionator comprises top tray and the multiple tower trays below top tray, and wherein supplying step comprises reflux stream is transported to top tray, and wherein acid has alleviated the pollution in acetonitrile fractionator.
On the one hand, this process comprises and spreads and deliver to quencher distillating material at the bottom of the tower of acetonitrile fractionator.In one embodiment, the acid of adding acetonitrile fractionator in reflux stream is acetic acid.On the one hand, transmit and distillate material stream at the bottom of tower and can comprise at the bottom of obtaining the acetonitrile fractionator column that is sent to recovery tower originally and distillate at least a portion of material stream from acetonitrile fractionator, and make at least a portion change route to be sent to quencher.On the one hand, acid can be added in reflux stream to prevent or to alleviate the polymer formation in acetonitrile fractionator and reduce cleaning cost and the operation of prolongation acetonitrile fractionator by LDR.
The transmission that the tower bed material that can carry out acetonitrile fractionator flows to quencher makes the pH value of the lower section of recovery tower maintain predeterminated level or scope, for example, lower than pH neutral 7, on the other hand, 5 to 7.5 pH value, and 6 to 7.5 pH on the other hand.Adding sour step to the lower section of recovery tower can excessively reduce the pH in recovery tower and upset the chemical balance that is present in the higher-boiling compound of this position in this process.
On the one hand, when the bottomsstream of acetonitrile fractionator turns back to quench tower and turn back to the recoverer section in recovery tower unlike conventional acrylonitrile process time, the top tray that is back to acetonitrile fractionator by acid is added to has solved the problem that hydrogen cyanide pollutes.
Acid by pH is remained on the hydrogen cyanide that makes to be present in material stream and acetonitrile fractionator not in acetonitrile fractionating column polymerization and the scope that pollutes be used as polymerization inhibitor.Then acid get back to quencher, and wherein, pH has maintained the neutral range lower than approximately 4 to approximately 6, and can drift except ammonia with the outflow material of helping the reactor from acrylonitrile facility.
Fig. 1 and Fig. 2 are the schematic flow diagram according at least one aspect of the present disclosure.Especially, Fig. 1 and Fig. 2 are the schematic diagram of the embodiment of the present disclosure in acrylonitrile removal process.
The rich water or the aqueous solution that comprise acrylonitrile, acetonitrile, HCN, water and impurity from absorber 300 are delivered to heat exchanger 4 by pipeline 2, and wherein rich water is by poor-water/aqueous solvent 222 preheatings from pipeline 223 to heat exchanger 4.After preheating, Fu Shui leaves interchanger 4 and is delivered to recovery tower 7 via pipeline 6.Utilize and add the aqueous solvent that is delivered to recovery tower by pipeline 8, in recovery tower 7, carry out extractive distillation.When heat exchanger 4 transmits or after transmitting, poor-water/aqueous solvent 222 can split into aqueous solvent material stream and poor-water material stream, and aqueous solvent material circulation over-heat-exchanger 236 and pipeline 8 are to the top 207 of recovery tower 7, and poor-water material stream passes through pipeline 224.Poor-water/aqueous solvent 222 can provide from heat recovery equipment 226.Heat recovery equipment 226 can receive material stream 228 from recovery tower 7 via pipeline 230.Material stream 228 precalculated positions that can take from recovery tower 7, such as above the summary of the tower tray 232 in the bottom 227 of recovery tower 7 or tower tray 232 places.Tower tray 232 can be the tower tray of bottommost in recovery tower 7, is also known as the first tower tray of recovery tower 7.Material stream 228 can be transferred to heat recovery equipment 226 from recovery tower 7 by pump 229.
Poor-water material stream by pipeline 224 can be sent to absorber 300.Heat exchange can occur at heat exchanger 234 places, before the poor-water material stream by pipeline 224 is sent to absorber 300.Heat can be supplied for distilling in recovery tower 7 by interchanger 210.Remove three kinds of material streams from recovery tower 7.First, the tower top of acrylonitrile, HCN, water and some impurity distillates material and flows through and removed from recovery tower 7 by pipeline 212.Sidepiece material stream 214 can remove and be delivered to elutriator (stripper) or acetonitrile fractionator 215 from recovery tower 7.The tower top that comprises acetonitrile distillate material stream 203 can be via pipeline 216 top removal from acetonitrile fractionator 215.Liquid column bottoms distillate from the bottom 205 of acetonitrile fractionator 215 can turn back to recovery tower 7 by pipeline 218.Pump 219 can be for making liquid turn back to like this recovery tower 7 by pipeline 218.But, find that it can be preferred by pipeline 221, the bottomsstream from bottom 205 209 being transported to quencher 10.At the bottom of tower from recovery tower 7, distillating material stream can remove via pipeline 51, and transfers to chilling tower 10 or waste disposal unit by pipeline 220 by pump 53.
In one embodiment, comprise that at pipeline 216 the material stream of acetonitrile can be transported to condenser 235 and leave as condenser tower bottoms stream 245.Condenser tower bottoms stream 245 can split at 247 places, junction surface the reflux stream 251 in reflux pipeline 217 and the stream of the crude acetonitrile material in crude acetonitrile pipeline 237 253.On the one hand, the reflux stream 251 in reflux pipeline 217 can turn back to the top tray 241 of acetonitrile fractionator 215.A part for material stream 215 can offer pipeline 216 via pipeline 239.
On the one hand, extract the gas phase that comprises acetonitrile, water and trace HCN as sidepiece material stream 214 and be transported to acetonitrile fractionator 215 from recovery tower 7.Acetonitrile fractionator 215 can be the tower that comprises multiple tower trays.Pump 225 can be used for pumped back stream by reflux pipeline 217 and/or crude acetonitrile pipeline 237.
On the one hand, process comprises to reflux stream interpolation acid.As further describe, " adding sour to reflux stream " can comprise to reflux pipeline 217 and add acid, the overhead in pipeline 216 adds acid, and to reflux pipeline 239 interpolation acid, and the combination of each.On the other hand, acid can be in the upstream of condenser 235 or downstream add.Add acid to condenser 235 upstreams the more acid concentration of dilution is provided.Add acid in the downstream of condenser the acid of higher concentration will be provided to acetonitrile fractionator 215.
On the other hand, acid is provided for condenser 235 to reduce the pollution in condenser.In this regard, in the time that the acid of the tube sheet in condenser is sprayed completely by acid injection covering, the acid that is transported to condenser 235 is the most effective.Acid can be transported to the tube sheet in condenser 235 by injection nozzle (such as wholecircle conical jet nozzle).Injection nozzle can angledly cover with the injection that realizes tube sheet.For example, nozzle can be perpendicular to tube sheet and with respect to becoming the angle up to approximately 60 ° perpendicular to tube sheet.
On the one hand, organic acid or organic acid derivatives, can add reflux pipeline 217 to via pipeline 213 such as acetic acid or glycol acid.On the other hand, organic acid or organic acid derivatives, can add overhead pipeline 216 to from acetonitrile fractionator 215 via pipeline 233 such as acetic acid or glycol acid.On the other hand.Organic acid or organic acid derivatives can add reflux pipeline 239 to via pipeline 243 such as acetic acid or glycol acid.On the other hand, before overhead enters condenser 235, via pipeline 213 to reflux pipeline 217 and/or via pipeline 233 and/or via pipeline 243 to reflux pipeline 239, it can be useful to reduce polymerization and the pollution in acetonitrile fractionator 215, condenser 235 and/or miscellaneous equipment adding organic acid or for example acetic acid of organic acid derivatives or glycol acid to pipeline 216, such as being sent to quencher when the bottomsstream of acetonitrile fractionator 215, instead of during to recovery tower 7.Acetonitrile fractionator 215 can be designed or be configured to concentrated dilution water/acetonitrile material that may send to miscellaneous equipment and flow to be further purified and/or to reclaim acetonitrile.In one embodiment, the bottomsstream 211 of acetonitrile fractionator 215 can be transferred to quencher 10 by pipeline 221 by pump 55.In one embodiment, the bottomsstream 211 of acetonitrile fractionator 215 can engage with the recovery tower the bottomsstream in pipeline 51 via pipeline 9, and wherein the bottomsstream of combination can be transferred to quencher 10 by pipeline 220 by pump 53 or to waste disposal unit.
As shown in Figure 2, quencher 10 is configured to receive reactor eluting gas or gaseous stream 12 by pipeline 14.Reactor eluting gas 12 can comprise acrylonitrile and ammonia.Reactor eluting gas 12 can be cooling in reactor effluent cooler before entering quencher 10.In quencher 10, comprise the quench liquid contact and the quench reactor eluting gas 12 that distillate material stream at the bottom of the tower of acetonitrile fractionator.
Acid 36(for example, 98% sulfuric acid) can add quench liquid 16 to via pipeline 38.Due to the acid in the bottomsstream 211 that is sent to quencher 10, can reduce the acid amount of adding by pipeline 38.Quench liquid 16 comprises the liquid that leaves the bottom 42 of quencher 10 by pipeline 44.Water can add quencher 10 to by entrance 48 via pipeline 46, or otherwise can add quench liquid 16 to or flow other position in 17, the 44 and 65 liquid recirculation loops that form by material.Quench liquid 16 is recycled and uses pump 50 to get back to pipeline 65 and 17 by pipeline 44.Material stream 67 can be used as the extracting section of the liquid efflunent leaving by pipeline 44, to maintain the relative constant-quality flow in liquid recirculation loops by making up via pipeline 38,46,220 with 221 liquid that add.Material stream 57 removes formed neutralization reaction product (for example, ammonium sulfate) and is also applicable to prevent that undesired product from gathering in liquid recirculation loops, such as corrosion product.The effluent that leaves quencher 10 bottoms 42 can be put 52 places in siphon and extract from pipeline 44.
Tower top distillates material stream 13 can flow to chilling aftercooler 240 from quencher 10 by pipeline 15.Cold water can distillate material stream 13 chilling aftercooler condensate liquids with cooling tower top for chilling aftercooler 240.Rich water can be transferred to by pump 242 rich water pipeline 2 and/or to recirculation line 248 and get back to the top 252 of chilling aftercooler 240 from the bottom 250 of chilling aftercooler 240.After cooling by chilling aftercooler 340, tower top distillates expects that stream 13 can be used as material stream 244 and leaves chilling aftercooler 240.Material stream 244 can be transported to absorber 300 via pipeline 246.Can enter the top 254 of absorber 300 from the poor-water of pipeline 224.Can be sent to incinerator (not shown) from the waste gas 256 of absorber 300.Material stream 258 from absorber 300 bottoms 262 can comprise rich water as described earlier.This rich water can be transferred to pipeline 2 via pump 260.Material stream 258 can with the rich water combination from chilling aftercooler 240, such as at joint 264.
On the one hand, controller 11 can be configured to process the one or more signals corresponding to measured parameter, the pH of for example pH of the acetonitrile fractionator the bottomsstream 209 in the bottom 205 of acetonitrile fractionator 215 or the acetonitrile fractionator the bottomsstream 211 in pipeline 221 or pipeline 9, as measured by pH sensor (not shown in Fig. 1).Controller 11 can be configured to judge that whether determined parameter is higher or lower than predefined parameter scope.Those skilled in the art will recognize that according to the disclosure, the parameter of measuring can be any proper parameter that is applicable to operate acetonitrile fractionator, for example, the pH of acetonitrile fractionator the bottomsstream 209 or 211 of previously having discussed, or by the fluid level controller in the bottom 205 of acetonitrile fractionator 215 (not shown in Fig. 1) or flow controller (among Fig. 1 not shown) the measured liquid level associated with fluid mobile phase in one or more pipelines discussed in this article.Controller 11 can be configured to adjust via order wire or radio communication (not shown in Fig. 1) operation of one or more devices, if the parameter of measuring is below or above predefined parameter scope.For example, the acid that controller 11 can be configured to adjust by pipeline 213 or 233 interpolations measures to realize desirable pH in reflux stream 251 to alleviate the pollution in acetonitrile fractionator 215.Those skilled in the art will recognize that according to the disclosure, controller 11 can be configured to control with (multiple) that are associated by pipeline 213 and/or 233 interpolation acid thereby the operation of pump and/or valve meets (multiple) preset range.Those skilled in the art can be arranged in identification controller 11 or similar control device from fluid level controller or flow controller (not shown at Fig. 1) at a distance or can be positioned at and comprise fluid level controller or flow controller.Those skilled in the art will recognize that according to the disclosure, controller 11 can be configured to the device shown in Fig. 2 and the operation of (multiple) pump/valve of being associated with those devices.
Carry out the advantage of test to prove to add acid and acetonitrile fractionator the bottomsstream is sent to quencher 10 instead of according to conventional way, acetonitrile fractionator the bottomsstream is sent to recovery tower 7 and acid is not added to acetonitrile fractionator 215 to acetonitrile fractionator 215.Obtain following test data.
The facility 1 of test data-the comprise quencher shown in Fig. 1 is operated to illustrate that the ammonia in the overhead pipeline 216 of acetonitrile fractionator 215 forms according to the disclosure.Ammonia in overhead pipeline 216 be hydrogen cyanide polymerisation accessory substance and therefore indicate in acetonitrile fractionator 215 improperly/undesirable polymer forms.The facility 1 of " add acid/possess acid " operates to the top tray of acetonitrile fractionator 215 to add as described above acetic acid, and acetonitrile fractionator the bottomsstream sends to quencher 10 via pipeline 211.The facility 1 that " does not add acid/anacidity " is not to add acetic acid or other acid operates, and wherein acetonitrile fractionator the bottomsstream sends back to recovery tower 7 via pipeline 18.
The result that the facility 1 that operation as described above " is added acid " and the facility 1 of operation " not adding acid " obtain is shown in following table.
Above given test data shows the effect of adding acetic acid to acetonitrile fractionator overhead distillate, and wherein the pH of material stream is reduced to 6.4 pH from 8.9 pH.On the one hand, the pH reducing in recovery tower has reduced improper polymerization.This is the corresponding reduction of the ammonia concentration in acetonitrile fractionator overhead distillate, when adding when acetic acid from 188ppm to 9ppm.The reduction of ammonia in this acetonitrile fractionator overhead distillate, that is, be considered to acetic acid by the mobile material stream of pipeline 216 and catch ammonia and in material stream 211, remove to chilling 10 as the result of ammonium acetate and by it.It may be partly also that hydrogen cyanide is stayed in solution as cyanalcohol and do not resolve into its original components and the result of then polymerization (it discharges ammonia).Ammonia is the accessory substance of the polymerisation of hydrogen cyanide.Adding acetic acid to material stream has reduced significantly the ammonia amount existing and has proved effect of the present disclosure.
On the one hand, selecting pH level is to reduce to pollute and use the balance between desirable building material.In this regard, use pH level as described above to allow to use carbon steel structure.
Fig. 3 is according to the flow chart of the method 300 of aspect of the present disclosure.Can carry out manner of execution 300 with previous described equipment.Step 301 comprises: expect to spread to deliver to quencher by distillating at the bottom of the tower of acetonitrile fractionating column.Step 302 comprises: add acid to reflux stream to acetonitrile fractionator.On the one hand, acetonitrile fractionator comprises multiple tower trays, and adds acid to reflux stream and comprise the top tray that acid is added to multiple tower trays of acetonitrile fractionator to the step of acetonitrile fractionating column.On the one hand, acid being added to reflux stream comprises to reflux stream and adds acetic acid to the step of acetonitrile fractionator.On the one hand, carry out and add the pH of sour step with the overhead of reduction acetonitrile fractionator to refluxing.
On the one hand, adding sour step to refluxing causes the pH of the overhead of acetonitrile fractionating column from higher than 7.0 pH that are reduced to lower than 7.0.On the one hand, adding sour step to refluxing causes the pH of the overhead of acetonitrile fractionating column from higher than 8.0 pH that are reduced to lower than 6.5.On the one hand, add to refluxing sour step by the pH of the overhead of acetonitrile fractionating column from being reduced to approximately 6.4 pH higher than 7.0.
On the one hand, spread the step of delivering to quencher and also comprise and change route transmission and make the tower bottoms stream of acetonitrile fractionating column flow to quencher from flowing to recovery tower distillating material stream at the bottom of the tower of acetonitrile fractionator distillating material at the bottom of the tower of acetonitrile fractionator.
The application is applicable to any process of recover acrylonitrile, and the process of recover acrylonitrile has recovery tower and one or more extra destilling tower.Extra destilling tower generally includes HCN tower, be used for removing the drying tower of water and be used for reclaiming the product tower of product quality acrylonitrile.But these independent operations can be combined as shown in drawings, wherein, destilling tower remove HCN and water the two.
Although some preferred embodiment about the application has been described the disclosure, and many details are described for purpose of explanation, for those skilled in the art obviously the disclosure be easy to have in extra embodiment and details described herein some can change significantly, and do not depart from general principle of the present disclosure.Should be appreciated that feature of the present disclosure to be easy to make amendment, change, to change or to substitute and do not depart from the scope of spirit or scope of the present disclosure or claim.For example, the size of various parts, quantity, size and shape can change to adapt to concrete application.Therefore, diagram and specific embodiment described herein are just for purpose of explanation.

Claims (37)

1. a process, comprising:
Add acid to reflux stream; And
Described reflux stream is transported to acetonitrile fractionator.
2. process according to claim 1, is characterized in that, described acid has reduced the pollution in described acetonitrile fractionator.
3. process according to claim 1, is characterized in that, described acetonitrile fractionator comprises top tray and the multiple tower trays below described top tray, and wherein said supplying step comprises described reflux stream is transported to described top tray.
4. process according to claim 1, is characterized in that, described acid comprises organic acid, organic acid derivatives and its mixture, and wherein said organic acid is selected from the group of acetic acid, glycol acid and its mixture.
5. process according to claim 1, is characterized in that, adds tower top that sour step reduced described acetonitrile fractionator and distillate the pH of material stream to described reflux stream.
6. process according to claim 1, is characterized in that, the described step of adding acid to described reflux stream comprises that the tower top that maintains described acetonitrile fractionator distillates the pH that expects stream in preset range.
7. process according to claim 5, is characterized in that, to described backflow add pH that tower top that sour step reduced described acetonitrile fractionating column distillates material stream from higher than 7.0 to the pH lower than 7.0.
8. process according to claim 5, is characterized in that, to described reflux stream add pH that tower top that sour step reduced described acetonitrile fractionating column distillates material stream from higher than 8.0 to the pH lower than 6.5.
9. process according to claim 5, is characterized in that, adds pH that tower top that sour step reduced described acetonitrile fractionating column distillates material stream from the pH higher than 7.0 to approximately 6.4 to described reflux stream.
10. process according to claim 6, is characterized in that, the tower top that maintains described acetonitrile fractionator to the described step of described reflux stream interpolation acid distillates the pH that expects stream lower than approximately 7.0.
11. processes according to claim 6, is characterized in that, the tower top that maintains described acetonitrile fractionator to the described step of described reflux stream interpolation acid distillates the pH that expects stream lower than approximately 6.5.
12. processes according to claim 6, is characterized in that, the tower top that maintains described acetonitrile fractionator to the described step of described reflux stream interpolation acid distillates the pH that expects stream lower than approximately 6.4.
13. processes according to claim 1, is characterized in that, it also comprises: described in condensation, tower top distillates material stream so that described reflux stream to be provided.
14. processes according to claim 13, is characterized in that, add sour step comprise that distillating material stream to the tower top of described acetonitrile fractionator adds acid to described reflux stream.
15. processes according to claim 14, is characterized in that, it also comprises: expect to spread to deliver to quencher by distillating at the bottom of the tower of described acetonitrile fractionator.
16. processes according to claim 15, is characterized in that, distillate material stream and be included in to described reflux stream and add at least some acid of adding to described reflux stream during sour step at the bottom of the described tower of described acetonitrile fractionator.
17. processes according to claim 16, it is characterized in that, it also comprises: provide gaseous stream to described quencher, described gaseous stream comprises acrylonitrile and ammonia, and described gaseous stream is contacted with quench liquid, described quench liquid distillates material stream at the bottom of comprising the tower of described acetonitrile fractionator.
18. processes according to claim 15, it is characterized in that, described transfer step comprises that at least a portion that distillates material stream at the bottom of the tower that makes the described acetonitrile fractionator that is transported to recovery tower changes route transmission and makes the described tower bottoms stream of described acetonitrile fractionator be transported to described quencher.
19. processes according to claim 1, is characterized in that, it also comprises: the tower top that at least a portion of described reflux stream is transported to the acetonitrile fractionator of condenser upstream distillates material stream.
Expect that by distillating at the bottom of the tower of acetonitrile fractionating column stream is transported to the process of quench tower, at the bottom of wherein said tower, distillate material stream and comprise at least some acid for 20. 1 kinds.
21. processes according to claim 20, is characterized in that, distillate material stream and have approximately 7 or less pH at the bottom of described tower.
22. processes according to claim 20, is characterized in that, distillate material stream and have approximately 5 to approximately 7.5 pH at the bottom of described tower.
23. processes according to claim 20, is characterized in that, distillate material stream and have approximately 6 to approximately 7 pH at the bottom of described tower.
24. 1 kinds of equipment comprise:
Acetonitrile fractionator, it is configured to produce and comprises that the tower top of acetonitrile distillates material stream;
Reflux pipeline, it is configured to reflux stream to be transported to acetonitrile fractionator; And
Pipeline is added in acid, and it is configured to add acid to described reflux stream.
25. equipment according to claim 24, is characterized in that, it also comprises: condenser, and it is configured to the crude acetonitrile product that cooling described tower top distillates material stream and generates condensation, and wherein said reflux stream comprises at least a portion of described condensation acetonitrile product.
26. equipment according to claim 24, is characterized in that, described acetonitrile fractionator comprises top tray and the multiple tower trays below described top tray, and described reflux pipeline is configured to described reflux stream to be transported to described top tray.
27. equipment according to claim 24, is characterized in that, described acid comprises acetic acid.
28. equipment according to claim 24, is characterized in that, it comprises controller, and it is configured to control to the acid interpolation of described reflux stream.
29. equipment according to claim 28, is characterized in that, described controller is configured to control acid and adds the pH that distillates material stream to reduce described tower top.
30. equipment according to claim 29, is characterized in that, described controller is configured to maintain described tower top and distillates the pH that expects stream in preset range.
31. equipment according to claim 29, is characterized in that, the pH that described controller is configured to described tower top to distillate material stream is from being greater than 7.0 pH that are reduced to lower than 7.0.
32. equipment according to claim 29, is characterized in that, described controller is configured to described tower top to distillate and expect that the pH of stream is reduced to 6.5 pH from being greater than 8.0.
33. equipment according to claim 29, is characterized in that, described controller is configured to described tower top to distillate and expect that the pH of stream is reduced to approximately 6.4 pH from being greater than 7.0.
34. equipment according to claim 25, is characterized in that, described acid tube line is configured to distillate material stream to described tower top and adds acid.
35. equipment according to claim 24, is characterized in that, it also comprises: transfer line, it is configured at least a portion that distillates material stream at the bottom of the tower of described acetonitrile fractionator to be sent to quencher.
36. equipment according to claim 35, is characterized in that, distillate material stream and comprise at least some acid of adding described reflux stream at the bottom of described tower.
37. equipment according to claim 36, is characterized in that, described quencher is configured to receive and comprises the gaseous stream of acrylonitrile and ammonia, and described gaseous stream contact with quench liquid, and described quench liquid comprises at the bottom of the tower of described acetonitrile fractionator and distillates and expect to flow.
CN201410256722.3A 2014-06-11 2014-06-11 Pollution reduction in acetonitrile removing step in acrylonitrile recovery Pending CN104107559A (en)

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CN201410256722.3A CN104107559A (en) 2014-06-11 2014-06-11 Pollution reduction in acetonitrile removing step in acrylonitrile recovery
CN201811122752.XA CN109499085A (en) 2014-06-11 2014-06-11 Pollution in the acetonitrile removing step of acrylonitrile recycling mitigates
JP2016572412A JP6761758B2 (en) 2014-06-11 2015-06-09 Reduced fouling in the acetonitrile removal step of acrylonitrile recovery
TR2016/17300T TR201617300T1 (en) 2014-06-11 2015-06-09 Reduction of fouling in acetonitrile removal stages of acrylonitrile recovery.
PCT/US2015/034826 WO2015191528A1 (en) 2014-06-11 2015-06-09 Fouling reduction in the acetonitrile removal steps of acrylonitrile recovery
EA201692339A EA034228B1 (en) 2014-06-11 2015-06-09 Fouling reduction in the acetonitrile removal steps of acrylonitrile recovery
TW104118782A TWI715532B (en) 2014-06-11 2015-06-10 Fouling reduction in the acetonitrile removal steps of acrylonitrile recovery
SA516380473A SA516380473B1 (en) 2014-06-11 2016-12-11 Fouling Reduction in The Acetonitrile Removal Steps of Acrylonitrile Recovery

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