CN205241574U - Acidification system in refined technology of acetonitrile - Google Patents
Acidification system in refined technology of acetonitrile Download PDFInfo
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- CN205241574U CN205241574U CN201520652410.4U CN201520652410U CN205241574U CN 205241574 U CN205241574 U CN 205241574U CN 201520652410 U CN201520652410 U CN 201520652410U CN 205241574 U CN205241574 U CN 205241574U
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- acid
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Abstract
The utility model relates to an acidification system in refined technology of acetonitrile, include: first knockout tower, it is arranged in the light component of the thick acetonitrile of desorption raw materials by the configuration and obtains containing the acetonitrile material, the fractional distilling tube, it is used for the condensation to follow by the configuration the partial gaseous phase commodity circulation of distilling off in the top of first knockout tower to commodity circulation backward flow to first knockout tower with the partial condensation, the acidification pipeline, it is configured as to adding sourly in the first knockout tower, PH detecting element, it is configured as on -line measuring the pH value of the cauldron liquid of first knockout tower, sour flow control unit, it is configured as the mass flow who adjusts the acid in the acidification pipeline, its characterized in that, sour flow control unit basis the mass flow of the acid in the automatically regulated acidification pipeline is come to the pH value that pH detecting element detected. The utility model discloses an acidification system in refined technology of acetonitrile has the first separation tata cauldron pH value of effective control, effectively reduces the interior hydrogen cyanide polymeric characteristics of tower.
Description
Technical field
The utility model relates to the acid system that adds in a kind of acetonitrile refining process.
Background technology
In the production process of ammoxidating propylene to prepare acrylonitrile, simultaneously coproduct hydrogen cyanic acid and acetonitrile, wherein aldehyde, Tong, oxazole,The impurity such as propionitrile and a small amount of hydrogen cyanide are extracted to acetonitrile solution in acrylonitrile extraction desorption process, through acetonitrile desorb orStripping is in crude acetonitrile. In the prior art, conventionally adopt the combination by decyanation tower, chemical treatment, decompression, pressurization azeotropic distillationTechnique, reclaims continuously to acetonitrile.
EP055920 discloses a kind of technique of continuous recovery acetonitrile. This process using rectifying removes the light groups such as hydrogen cyanideThe method divide, chemical treatment further removing hydrogen cyanide, rectification under vacuum and compression rectification combined dehydration, has improved the refining of acetonitrileThe rate of recovery, can obtain the acetonitrile product of higher degree. In addition, CN1328994A also disclose a kind of from contain acetonitrile, water, HCN,In oxazole and heavy organic crude acetonitrile, reclaim continuously the high-purity acetonitrile refining method of high-purity acetonitrile. The method is returned continuously to traditionReceive the technique of acetonitrile and improve, increase a liquid phase by the rectifying section top at the first knockout tower and extract mouth out, make accumulationOxazole is discharged system smoothly.
Above-mentioned technique has all adopted at the first knockout tower and has removed the light components such as hydrogen cyanide, stripping section side line gas phase is extracted out moistureDeng the technique of the acetonitrile of impurity, this extraction acetonitrile material obtains acetonitrile finished product after chemical treatment, decompression and pressurizing and dehydrating. SoAnd the hydrogen cyanide impurity containing in the charging due to the first knockout tower easy polymerization in subtractive process causes knockout tower insideStop up, and then affect the normal operation continuously of long period of running gear.
Utility model content
In order to solve the aforementioned problems in the prior, the utility model provides the acid adding in a kind of acetonitrile refining processSystem. This adds acid system and has effective control the first knockout tower tower reactor pH value, effectively reduces the feature of hydrogen cyanide polymerization in tower.
The utility model provides the acid system that adds in a kind of acetonitrile refining process, comprising:
The first knockout tower, it is arranged to and removes the light component in raw material crude acetonitrile and obtain containing acetonitrile material;
Fractional distilling tube, it is connected to the gaseous stream outlet at the top of described the first knockout tower through the first pipeline, andBe arranged to condensation and export the part gaseous stream distillating from described gaseous stream, and the logistics of partial condensation is managed through the 3rdLine is back to described the first knockout tower;
Acid adding pipeline, it is configured to add acid in described the first knockout tower;
PH detecting unit, it is arranged at for the tower reactor still liquid of described the first knockout tower being discharged to described the first knockout towerOn the 4th pipeline, and be configured to detect online the pH value of described still liquid;
Acid flow regulating unit, it is connected to described acid adding pipeline, and is configured to regulate in described acid adding pipelineThe mass flow of described acid,
It is characterized in that, the pH value that described sour flow regulating unit detects according to described pH detecting unit, adjusts automaticallySave the mass flow of the described acid in described acid adding pipeline.
Preferably, add in acid system described, described sour flow regulating unit comprises flow controller and control valve,
Wherein, the pH value that described flow controller detects according to described pH detecting unit regulates beating of described control valveOpen degree, to regulate the mass flow of the described acid in described acid adding pipeline.
Preferably, add in acid system described, described sour flow regulating unit is measuring pump,
Wherein, the pH value that described measuring pump detects according to described pH detecting unit regulates the institute in described acid adding pipelineState sour mass flow.
Preferably, add in acid system described, be positioned at described the first knockout tower to the position of described the first knockout tower acid addingThe position of material inlet on.
Preferably, add in acid system described, the distance of the tower top of described the first knockout tower of described material inlet distance is40%～70% of the height of described the first knockout tower, and for extracting out described in the described distance of the products export containing acetonitrile materialThe distance of the tower top of the first knockout tower be described the first knockout tower height 55%～95%.
Preferably, add in acid system described, described acid by described acid adding pipeline via described fractional distilling tube, with describedThe logistics of partial condensation is back to described the first knockout tower.
Preferably, add in acid system the acetonitrile that described raw material crude acetonitrile comprises 20～60wt%, 1～4wt%'s describedHCN, the acrylonitrile of 0.1～0.3wt% and the water of 34～79wt%.
Preferably, add in acid system described, described acid is acetic acid.
Preferably, add in acid system described, the concentration of described acetic acid is about 50wt%.
Effect of the present utility model
The utility model passes through in the first knockout tower top interpolation acid, also by the first knockout tower tower reactor pH value and acid adding amountTandem control, effectively controlled the pH value of this tower reactor, effectively ensured that this tower operates under the condition of slant acidity, effectivelyReduce the polymerization of hydrogen cyanide in tower. Adopt the utility model, realized the long-period stable operation of device.
Brief description of the drawings
Fig. 1 is the schematic diagram that adds acid system of the first embodiment of the present utility model.
Fig. 2 is the schematic diagram that adds acid system of the second embodiment of the present utility model.
List of reference signs
1 first knockout tower
2 fractional distilling tubes
3pH detector
4 control valves
5 flow controllers
25 measuring pumps.
Detailed description of the invention
Below with reference to accompanying drawing, the acid system that adds in acetonitrile refining process of the present utility model is described in detail, but this realityBe not limited to following detailed description of the invention with novel.
As shown in Figure 1, the acid system that adds in acetonitrile refining process of the present utility model comprises: the first knockout tower 1, part are coldCondenser 2, pH detector 3, control valve 4 and flow controller 5.
The first knockout tower 1 can be divided into top, middle part and bottom. Top is provided with the gaseous stream outlet that is positioned at top15, and be positioned at gaseous stream and export the phegma entrance 16 of 15 belows. Middle part comprises material inlet 17 Hes that are positioned at side lineBe positioned at the acetonitrile products export 18 of material inlet 17 belows, and this acetonitrile products export 18 is positioned described the first knockout tower1 55～95% position highly from top to bottom, takes out the gas phase acetonitrile after purifying by pipeline 7 from this acetonitrile products export 18Go out. Bottom comprises still liquid outlet 19, by pipeline 11 by part water (account for the raw material water yield 50～80%), the acid of adding and heavyComponent is discharged.
Fractional distilling tube 2 is provided with gas access 21, lime set outlet 23 and fixed gas outlet 22. The first knockout tower 1 topThe gas access 21 of gaseous stream outlet 15 and condenser 2 between be connected with the first pipeline 8, this first pipeline 8 is configured useIn being exported to 15 effluent airs, the first knockout tower 1 top gaseous stream is delivered to fractional distilling tube 2. Comprise hydrogen cyanide, propyleneJing is with the light component of oxazole etc. is sent to burning by fixed gas outlet 22 through pipeline 9 as fixed gas. The phegma of the first knockout tower 1Between the lime set outlet 23 of entrance 16 and fractional distilling tube 2, be connected with the 3rd pipeline 10, the three pipelines 10 be arranged to byLime set in fractional distilling tube 2 is transmitted back to the first knockout tower 1.
Between the still liquid outlet 19 at the tower reactor place of the first knockout tower 1 and still liquid pump (not shown), be connected with the 4th pipeline 11,The 4th pipeline is arranged to discharges the first knockout tower 1 by the tower reactor still liquid of the first knockout tower 1. On the 4th pipeline 11, establishBe equipped with pH and detect mouth 20, connecting line 24 is connected to pH and detects between mouth 20 and pH detector 3.
Between pH detector 3 and flow controller 5, be connected with first signal and transmit loop 14; For detector 3 is detectedTo signal be sent to flow controller 5.
Flow controller 5 is connected to control valve 4. The import of control valve 4 is connected with the pipeline 12 for delivery of raw material acid. AdjustThe outlet of joint valve 4 is connected with the second pipeline 13, and this second pipeline 13 adds acid the gaseous stream one of the tower top of the first knockout tower 1In entering part condenser 2.
The second pipeline 13 is added acid to not concrete restriction of particular location of the first knockout tower 1, as long as it is positioned at raw materialThe top of import 17. For example, can make the second pipeline 13 be communicated with the 3rd pipeline 10 fluids, thereby make acid solution pass through the 3rdPipeline 10 enters the first knockout tower 1; Or, also can in the first knockout tower charging aperture top any part, add. But preferablyGround, makes the second pipeline 13 be communicated with the first pipeline 8 fluids, and acid adding adds in the first pipeline 8, with the tower top of the first knockout tower 1Gaseous stream is entering part condenser 2 together, enters the first knockout tower 1 through fractional distilling tube 2 and by the 3rd pipeline 10.
According to the acid system that adds in acetonitrile refining process of the present utility model as shown in Figure 1, by feed line 6 by formerMaterial crude acetonitrile is delivered in the first knockout tower 1 by the material inlet 17 at the middle part that is positioned the first knockout tower 1. Raw material crude acetonitrile canTo comprise the acetonitrile of Partial purification, can be from any applicable source, for example, from acrylonitrile installation acetonitrile desorb tower top.By weight percentage, raw material crude acetonitrile can comprise 20～60% acetonitriles, 1～4%HCN, 0.1～0.3% acrylonitrile, 34～79% water.
In the first knockout tower 1, carry out after initial gross separation, gaseous stream is discharged from the gaseous stream outlet 15 that is positioned at tower top,Be delivered to fractional distilling tube 2 through the first pipeline 8. Meanwhile, raw material acid is delivered to acid adding control valve 4 by pipeline 12, through control valve 4After adjust flux, enter the first pipeline 8 by the second pipeline 13, converge with the gaseous stream that comes from knockout tower tower top, enter togetherEnter fractional distilling tube 2. The acid of adding can be sulfuric acid, phosphoric acid or acetic acid etc., is preferably acetic acid. The concentration of acetic acid is preferably20～50wt%, most preferably is 50wt%.
Gaseous stream in fractional distilling tube 2 after partial condensation, together with added acid through the 3rd pipeline 10 by phegmaEntrance 16 is back to the first knockout tower 1 inside. Acetonitrile product after separation is drawn out of through pipeline 7 by acetonitrile products export 18. AndThe still liquid that comprises added acid, part water and heavy constituent exports 19 through the 4th pipeline 11 quilts from the still liquid of knockout tower tower reactorOutside discharge knockout tower.
Detect mouth 20 through connecting line 24 from pH the part still liquid the 4th pipeline 11 is delivered to pH detector 3, to examineSurvey the pH value of still liquid. PH detector 3 transmits loop 14 by detected result through first signal and is delivered to flow controller 5. StreamAmount controller 5 controls to adjust the aperture size of valve 4 according to received still liquid pH value, thereby controls by the second pipeline 13Add the sour mass flow in fractional distilling tube 2. In the time that the pH of still liquid is too low, flow controller 5 sends finger to control valve 4Order, reduces the aperture of control valve 4, thereby reduces the mass flow of the acid solution in the second pipeline 13, to improve still liquid pH value. PhaseInstead, in the time that the pH of still liquid is too high, flow controller 5 sends instruction to control valve 4, the aperture of control valve 4 is increased, thereby subtract largeThe mass flow of the acid solution in the second pipeline 13, to reduce still liquid pH value.
The pH value of still liquid is preferably 1～7, and more preferably 3～5, also more preferably 3.5～4.5.
Above with reference to accompanying drawing in acetonitrile refining process of the present utility model add acid system and acid-adding method has carried out in detailThin description. But the utility model is not limited to this, not departing from the scope of essence of the present utility model, art technology peopleMember can add acid system and acid-adding method improves to of the present utility model.
For example, as shown in Figure 2, can adopt measuring pump 25 to replace the combination of flow controller 5 and control valve 4. EquallyCan realize above-mentioned effect of the present utility model.
For example, can not adopt the automation control of the online detection of PH and acid adding amount, adopt offline inspection and the acid adding of PHThe manual control of amount, can realize above-mentioned effect of the present utility model too.
In addition, as shown in the dotted line in Fig. 1 and 2, pH detects mouth 20 and can not open on the 4th pipeline 11, but directly opensIn the tower reactor of the first knockout tower 1, and be connected to pH detector 3 via connecting line 24.
Embodiment
To be further elaborated the utility model by specific embodiment below.
[embodiment 1]
Adopt the first knockout tower shown in Fig. 1, by containing acetonitrile 45%, HCN2%, acrylonitrile 0.1%, that all the other are water is formerMaterial crude acetonitrile adds from the material inlet 17 of the first knockout tower 1, and feeding temperature is 40 DEG C, and tower top pressure is 0.12MPa, and tower top goes outMaterial temperature degree is 55 DEG C, and tower reactor temperature is 115 DEG C. Acetonitrile product at height 85% place (from top to bottom) of the first knockout tower 1 goes outThe acetonitrile concentration that extract out at mouth 18 places is 75 % by weight, and extracting temperature out is 94 DEG C. Can guarantee that the first separation tower bottoms pH value keeps4～4.5, acetonitrile refining device even running 1 year.
[embodiment 2]
Adopt the acid system that adds shown in Fig. 2, by containing acetonitrile 50%, HCN2.5%, acrylonitrile 0.12%, that all the other are water is formerMaterial crude acetonitrile adds from the feed(raw material)inlet 17 of the first knockout tower 1, and feeding temperature is 40 DEG C, and tower top pressure is 0.12MPa, and tower top goes outMaterial temperature degree is 53 DEG C, and tower reactor temperature is 115 DEG C. Acetonitrile product at height 85% place (from top to bottom) of the first knockout tower 1 goes outThe acetonitrile concentration that extract out at mouth 18 places is 78 % by weight, and extracting temperature out is 96 DEG C. Can guarantee that the first separation tower bottoms pH value keeps3.5～4, acetonitrile refining device even running 1 year 6 months.
[comparative example 1]
This practicality is never set newly containing acetonitrile 50%, HCN2.5%, acrylonitrile 0.12%, raw material crude acetonitrile that all the other are waterThe middle part of first knockout tower that adds acid system of type adds, and feeding temperature is 40 DEG C, and tower top pressure is 0.12MPa, tower top dischargingTemperature is 53 DEG C, and tower reactor temperature is 115 DEG C. At the acetonitrile products export at height 85% place (from top to bottom) of the first knockout tower 1The acetonitrile concentration that extract out at 18 places is 78 % by weight, and extracting temperature out is 96 DEG C. The operation of acetonitrile refining device 3 months is because of first pointFrom the serious and parking maintenance of tower polymerization.
According to adding acid system and preventing the method for hydrogen cyanide polymerization in acetonitrile refining process of the present utility model, byThe first knockout tower top is added acid, is also passed through the tandem control of the first knockout tower tower reactor pH value and acid adding amount, has effectively controlledThe pH value of this tower reactor, has effectively ensured that this tower operates under the condition of slant acidity, has effectively reduced the polymerization of hydrogen cyanide in tower.Adopt the utility model, realized the long-period stable operation of device.
Claims (11)
1. in acetonitrile refining process, add an acid system, comprising:
The first knockout tower, it is arranged to and removes the light component in raw material crude acetonitrile and obtain containing acetonitrile material;
Fractional distilling tube, it is connected to the gaseous stream outlet at the top of described the first knockout tower through the first pipeline, and is joinedPut and export the part gaseous stream distillating for condensation from described gaseous stream, and the logistics of partial condensation is returned through the 3rd pipelineFlow to described the first knockout tower;
Acid adding pipeline, it is configured to add acid in described the first knockout tower;
PH detecting unit, it is arranged at for the tower reactor still liquid of described the first knockout tower is discharged to the 4th of described the first knockout towerOn pipeline, and be configured to detect online the pH value of described still liquid;
Acid flow regulating unit, it is connected to described acid adding pipeline, and be configured to regulate in described acid adding pipeline described inThe mass flow of acid,
It is characterized in that, the pH value that described sour flow regulating unit detects according to described pH detecting unit, regulates institute automaticallyState the mass flow of the described acid in acid adding pipeline.
2. the acid system that adds according to claim 1, is characterized in that, described sour flow regulating unit comprises flow controllerAnd control valve,
Wherein, the pH value that described flow controller detects according to described pH detecting unit regulates the journey of opening of described control valveDegree, to regulate the mass flow of the described acid in described acid adding pipeline.
3. the acid system that adds according to claim 1, is characterized in that, described sour flow regulating unit is measuring pump,
Wherein, the pH value that described measuring pump detects according to described pH detecting unit regulates the described acid in described acid adding pipelineMass flow.
4. the acid system that adds according to claim 1, is characterized in that, described acid adding pipeline is to described the first knockout tower acid addingPosition be positioned on the position of material inlet of described the first knockout tower.
5. the acid system that adds according to claim 4, is characterized in that, described the first knockout tower of described material inlet distanceThe distance of tower top be described the first knockout tower height 40%～70%, and for extracting the described product containing acetonitrile material outThe distance of the tower top of described the first knockout tower of outlet distance be described the first knockout tower height 55%～95%.
6. the acid system that adds according to claim 4, is characterized in that, described acid by described acid adding pipeline via described partCondenser, is back to described the first knockout tower with the logistics of described partial condensation.
7. the acid system that adds according to claim 1, is characterized in that, the second that described raw material crude acetonitrile comprises 20～60wt%Nitrile, the HCN of 1～4wt%, the acrylonitrile of 0.1～0.3wt% and the water of 34～79wt%.
8. the acid system that adds according to claim 1, is characterized in that, described acid is sulfuric acid, phosphoric acid or acetic acid.
9. the acid system that adds according to claim 8, is characterized in that, described acid is acetic acid.
10. the acid system that adds according to claim 9, is characterized in that, the concentration of described acetic acid is 20～50wt%.
11. acid systems that add according to claim 10, is characterized in that, the concentration of described acetic acid is 50wt%.
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| CN201520652410.4U CN205241574U (en) | 2015-08-26 | 2015-08-26 | Acidification system in refined technology of acetonitrile |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112444139A (en) * | 2019-09-05 | 2021-03-05 | 中石油吉林化工工程有限公司 | Tower top condensing system of dehydrocyanic acid tower |
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2015
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112444139A (en) * | 2019-09-05 | 2021-03-05 | 中石油吉林化工工程有限公司 | Tower top condensing system of dehydrocyanic acid tower |
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