Summary of the invention
For the problem existing in correlation technique, the object of the present invention is to provide a kind of vinyl cyanide system for separating and purifying, at least to realize the refining yield that improves acrylonitrile process.
For achieving the above object, the invention provides a kind of vinyl cyanide system for separating and purifying, comprising: quench tower, is connected by the first connection pipeline section with its tower top sidewall at the bottom of the tower of quench tower; Knockout tower, the material inlet of knockout tower is communicated with pipeline section and is communicated with pipeline section connection by second with first, and the gaseous phase materials outlet on its top is communicated with quench tower; And sulphuric acid soln transfer lime, transfer lime is communicated with quench tower.
According to the present invention, sulphuric acid soln transfer lime is connected with the first connection pipeline section, be communicated with quench tower to be communicated with pipeline section by first, wherein, along the first connection pipeline section from the direction to its tower top sidewall at the bottom of quench tower tower, transfer lime and first is communicated with the first link position of being connected of pipeline section, is positioned at the downstream of the second link position that the second connection pipeline section and the first connection pipeline section be connected.
According to the present invention, also comprise reboiler and steam manifold, wherein, reboiler is connected with knockout tower, and steam manifold has the first branch road and the second branch road, and the first branch road is connected to reboiler, the second branch road is connected to knockout tower, wherein, by being arranged on the shifter in steam manifold, the steam of controlling in steam manifold enters the first branch road or the second branch road.
According to the present invention, between knockout tower and steam manifold, be connected with tandem setting device, tandem setting device comprises temperature monitor, flow monitor and variable valve, wherein, temperature monitor is monitored the tower top temperature of knockout tower, and regulates the aperture of variable valve according to monitor value control flow monitor.
According to the present invention, at the bottom of the tower of quench tower and between the second connection pipeline section, be connected with level monitoring device, wherein, level monitoring device, according to the liquid level of reaction mass in quench tower, is controlled the flow that is flowed into the intermediate reaction product of the second connection pipeline section by the first connection pipeline section.
According to the present invention, sulphuric acid soln transfer lime and first is communicated with and between pipeline section, is provided with pH value monitoring device, wherein, pH value monitoring device is communicated with the link position of pipeline section with first, between the first link position and the second link position, wherein, pH value monitoring device, according to the pH value of intermediate reaction product in the first connection pipeline section, is controlled the operational throughput of sulphuric acid soln transfer lime to the first connection pipeline section conveying sulphuric acid soln.
According to the present invention, knockout tower bottom is connected with material recycle pipe, is provided with fluid level control device, wherein between knockout tower bottom and material recycle pipe, fluid level control device, according to the liquid level of reaction mass in knockout tower, is controlled the flow that flows into material to be recycled in material recovery tube.
According to the present invention, the tower top of quench tower is provided with the outlet of finished product product, and quench tower inside is provided with the first spray equipment, and wherein, the first spray equipment is communicated with the first port that is communicated with pipeline section of the tower top sidewall that is communicated to quench tower.
According to the present invention, quench tower sidewall is also provided with reaction gas entrance, and quench tower inside is also provided with the second spray equipment, and wherein, reaction gas entrance is communicated with the second spray equipment.
According to the present invention, first at the bottom of the tower of quench tower and between the second link position is communicated with and in pipeline section, is in series with recycle pump.
Useful technique effect of the present invention is:
In vinyl cyanide system for separating and purifying of the present invention, sulphuric acid soln transfer lime can be carried sulphuric acid soln in quench tower, to react with the reaction gas of sending into quench tower.Wherein, in reaction gas, at least comprise propylene steam nitrile and ammonia, also can include gaseous hydrogen cyanic acid, gaseous state acetonitrile etc.In quench tower, sulphuric acid soln reacts that with this reaction gas this reaction gas is purified.Particularly, in quench tower, sulphuric acid soln and ammonia gas react generate ammoniumsulphate soln, so that the ammonia in reaction gas is removed.Propylene steam nitrile in reaction gas is towards the tower top motion of quench tower.At the bottom of the ammoniumsulphate soln generating after reaction flow to the tower of quench tower, wherein, in the process of ammoniumsulphate soln at the bottom of flowing to tower, can be mingled with the liquid propylene nitrile of condensation in quench tower, and at the bottom of unreacted sulphuric acid soln also flow to the tower of quench tower, thus, the intermediate reaction product being positioned at the bottom of quench tower tower at least comprises ammoniumsulphate soln, sulphuric acid soln, liquid propylene nitrile.By accessing knockout tower at the bottom of the tower of quench tower and between tower top sidewall, the intermediate reaction product of quench tower is carried out to secondary and separate again and required product is sent back in quench tower again.Particularly, in knockout tower, quench tower is isolated and sent back to vinyl cyanide in intermediate reaction product, and then the propylene steam nitrile of gained and form finished product product through the propylene steam nitrile of knockout tower secondary separation gained and discharged by quench tower of purifying for the first time in quench tower.In this way, on the one hand, can effectively remove the ammonia in reaction gas, on the other hand, reduce the loss of vinyl cyanide in above-mentioned removal process.Make thus the refining yield of vinyl cyanide improve, and promote the purity of propylene steam nitrile.
Embodiment
Specifically describe embodiments of the invention referring to accompanying drawing.With reference to Fig. 1, show an embodiment of vinyl cyanide system for separating and purifying of the present invention, the sulphuric acid soln transfer lime 3 that it comprises quench tower 1, knockout tower 2 and is communicated in quench tower 1.Wherein, at the bottom of the tower of quench tower 1, be connected by the first connection pipeline section 8 with the tower top sidewall of quench tower 1, the material inlet of knockout tower 2 is communicated with pipeline section 8 and is communicated with by the second connection pipeline section 9 with first, the gaseous phase materials outlet on knockout tower 2 tops is communicated with by third connecting pipeline section 22 with quench tower 1.
In the time that said system is worked, sulphuric acid soln transfer lime 3 can be carried sulphuric acid soln in quench tower 1, to react with the reaction gas of sending into quench tower 1.Wherein, in reaction gas, at least comprise propylene steam nitrile and ammonia, also can include gaseous hydrogen cyanic acid, gaseous state acetonitrile etc.In quench tower 1, sulphuric acid soln reacts that with this reaction gas this reaction gas is purified.Particularly, in quench tower 1, sulphuric acid soln and ammonia gas react generate ammoniumsulphate soln, so that the ammonia in reaction gas is removed.Propylene steam nitrile in reaction gas is towards the tower top motion of quench tower 1.At the bottom of the ammoniumsulphate soln generating after reaction flow to the tower of quench tower 1, wherein, in the process of ammoniumsulphate soln at the bottom of flowing to tower, can be mingled with the liquid propylene nitrile of condensation in quench tower 1, and at the bottom of unreacted sulphuric acid soln also flow to the tower of quench tower 1, thus, the intermediate reaction product being positioned at the bottom of quench tower 1 tower at least comprises ammoniumsulphate soln, sulphuric acid soln, liquid propylene nitrile.By accessing knockout tower 2 at the bottom of the tower at quench tower 1 and between tower top sidewall, the intermediate reaction product of quench tower 1 is carried out to secondary and separate again and required product is sent back in quench tower again.Particularly, in knockout tower 2, quench tower is isolated and sent back to vinyl cyanide in intermediate reaction product, and then the propylene steam nitrile of gained and form finished product product through the propylene steam nitrile of knockout tower secondary separation gained and discharged by quench tower 1 of purifying for the first time in quench tower 1.In this way, on the one hand, can effectively remove the ammonia in reaction gas, on the other hand, reduce the loss of vinyl cyanide in above-mentioned removal process.Make thus the refining yield of vinyl cyanide improve, and promote the purity of propylene steam nitrile.
Continue with reference to Fig. 1, sulphuric acid soln transfer lime 3 is connected with the first connection pipeline section 8, to be communicated with quench tower 1 by the first connection pipeline section 8, wherein, along the first connection pipeline section 8 from the direction to its tower top sidewall at the bottom of quench tower 1 tower, sulphuric acid soln transfer lime 3 and first is communicated with the first link position 10 of being connected of pipeline section 8, is positioned at the downstream of the second link position 11 that the second connection pipeline section 9 is connected with the first connection pipeline section 8.In other words, along the first connection pipeline section 8 from the direction to its tower top sidewall at the bottom of quench tower 1 tower, set gradually above-mentioned the second link position 11 and the first link position 10.Make thus, after the intermediate reaction product of quench tower 1 is flowed out by the tower bottom outlet of quench tower 1, first through the second link position 11, the intermediate reaction product of a part enters in knockout tower 2 via the second connection pipeline section 9.The intermediate reaction product of another part flows through the second link position 11 to be continued to flow along the first connection pipeline section 8.In the time that the intermediate reaction product of above-mentioned another part flows to the first link position 10, sulphuric acid soln flows into the first connection pipeline section 8 through sulphuric acid soln transfer lime 3, and the common quench tower 1 that flows into after mixing with the intermediate reaction product of this another part.
With further reference to Fig. 1, in the present embodiment, vinyl cyanide system for separating and purifying also comprises reboiler 4 and steam manifold 5.Wherein, reboiler 4 is connected with knockout tower 2, and steam manifold 5 has the first branch road 12 and the second branch road 13, the first branch roads 12 and is connected to reboiler 4, the second branch roads 13 and is connected to knockout tower 2.Shifter 14 is set in steam manifold 5, and the steam that this shifter 14 is controlled in steam manifold 5 enters the first branch road 12 or the second branch road 13.Alternatively, above-mentioned shifter 14 is T-valve.Particularly, reboiler 4 has first channel and the second passage of heat exchange mutually.Wherein, at the bottom of the tower of the entrance of first channel and knockout tower 2, be communicated with, the outlet of first channel is communicated with the sidewall of knockout tower 2, and the entrance of second passage is communicated with the first branch road 12 of steam manifold 5, and the outlet of second passage is communicated with phlegma recovery line 25.
In the time of the vinyl cyanide system for separating and purifying of application the present embodiment, make the steam in steam manifold 5 enter the first branch road 12 if select, the material being positioned at the bottom of the tower of knockout tower 2 imports first channel, steam imports second passage through the first branch road 12, steam is for the material in first channel provides heat, leads back knockout tower 2 after making liquid in first channel heated.Wherein, in the material at the bottom of the tower of knockout tower 2, at least there is ammoniumsulphate soln, liquid propylene nitrile.Ammoniumsulphate soln and liquid propylene nitrile are heated in reboiler, the liquid propylene nitrile gasification of part forms gas-phase propene nitrile, this part gas-phase propene nitrile is led and is back in knockout tower by knockout tower sidewall together with the liquid propylene nitrile not gasifying, ammoniumsulphate soln, separate to realize secondary, secondary more isolated gas-phase propene nitrile is led back in quench tower 1 through third connecting pipeline section 22 by the tower top of knockout tower 2 again.
In the time of the vinyl cyanide system for separating and purifying of application the present embodiment, make the steam in steam manifold 5 enter the second branch road 13 if select, steam is directly imported in knockout tower 2 so that the reaction mass in knockout tower is heated, make Partial Liquid Phase vinyl cyanide wherein be gasificated into gas-phase propene nitrile, separate again to realize secondary.
To sum up, make the steam in steam manifold 5 enter the first branch road 12 or the second branch road 13 no matter select, steam has all played the effect that thermal source is provided for the reaction mass in knockout tower 2, to make the gasification of liquid propylene nitrile form gas-phase propene nitrile, and enter quench tower 1 via the third connecting pipeline section 22 being communicated with knockout tower 2 tower tops.And vapour stream is condensed into water of condensation by phlegma recovery line 25 after crossing second passage heat release.
In addition, in the present embodiment, between knockout tower 2 and steam manifold 5, be connected with tandem setting device, tandem setting device comprises temperature monitor 15, flow monitor 16 and variable valve 17.Wherein, temperature monitor 15 is monitored the tower top temperature of knockout tower 2, and regulates the aperture of variable valve 17 according to monitor value control flow monitor 16.Preferably, tower top service temperature is positioned at the scope of 105 DEG C~115 DEG C.In the present embodiment, tower top service temperature is 100 DEG C.Temperature monitor 15 detects the tower top temperature of knockout tower 2, and when tower top temperature is during higher than 100 DEG C, temperature monitor 15 sends signal to flow detector 16.Flow detector 16 resets initial value after receiving signal, and then reduces aperture to variable valve 17 signals, variable valve 17 and then reduce steam add-on.The final tower top temperature that reduces.When tower top temperature is during lower than 100 DEG C, make variable valve 17 increase aperture and then increase steam add-on.In the time that tower top temperature equals 100 DEG C, temperature monitor 15 does not carry out any operation.
In addition, in the present embodiment, at the bottom of the tower of quench tower 1 and between the second connection pipeline section 9, be connected with level monitoring device, wherein, level monitoring device, according to the liquid level of reaction mass in quench tower 1, is controlled the flow that is flowed into the intermediate reaction product of the second connection pipeline section 9 by the first connection pipeline section 8.Particularly, the liquid level detector 23 that detects quench tower liquid level is set at quench tower 1, and on the second connection pipeline section 9, valve 24 is set, in the time that liquid level detector 23 detects quench tower liquid level higher than preset value, send signal to increase the aperture of valve 24 to valve 24, and then increase the ammoniumsulphate soln flow that enters knockout tower 2.In the time that liquid level detector 23 detects quench tower liquid level lower than preset value, send signal to reduce the aperture of valve 24 to valve 24, and then reduce to enter the ammoniumsulphate soln flow of knockout tower 2.In the time that liquid level detector 23 detects that quench tower liquid level equals preset value, do not carry out any operation.Alternatively, liquid level detector 23, except having above-mentioned functions, also can have the function of instruction liquid level and warning.Preferably, first at the bottom of the tower of quench tower 1 and between the second link position 11 is communicated with and in pipeline section 8, is in series with recycle pump 7.Wherein, aborning, above-mentioned preset value definite depends primarily on two aspects: 1, the produced quantity of recycle pump 7 ensures that the amount of liquid in quench tower tower reactor has a certain amount of surge time, then sets predetermined level value (being above-mentioned preset value) according to the diameter of this amount of liquid and quench tower.2, remove outside Article 1 chief reason, in an embodiment of the present invention, more than the liquid level of the reaction gas entrance 20 of guarantee quench tower in quench tower.
With further reference to Fig. 1, in the present embodiment, sulphuric acid soln transfer lime 3 and first is communicated with and between pipeline section 8, is provided with pH value monitoring device, wherein, pH value monitoring device is communicated with the link position of pipeline section 8 with first, between the first link position 10 and the second link position 11, wherein, pH value monitoring device, according to the pH value of intermediate reaction product in the first connection pipeline section 8, is controlled the operational throughput that sulphuric acid soln transfer lime 3 is carried sulphuric acid soln to the first connection pipeline section 8.Particularly, when the pH of intermediate reaction product value is during lower than set(ting)value, reduce the operational throughput of sulphuric acid soln.When the pH of intermediate reaction product value is during higher than set(ting)value, increase the operational throughput of sulphuric acid soln.In the time that the pH of intermediate reaction product value equals set(ting)value, do not do any operation.Wherein, preferably, above-mentioned set(ting)value is positioned at the scope of 4.8-6.0.
Continue with reference to Fig. 1, in the present embodiment, knockout tower 2 bottoms are connected with material recycle pipe 6, and in knockout tower 2, reaction mass can be discharged by material recycle pipe 6.Between knockout tower 2 bottoms and material recycle pipe 6, be provided with fluid level control device, wherein, fluid level control device, according to the liquid level of reaction mass in knockout tower 2, is controlled the flow that flows into material to be recycled in material recovery tube 6.The concrete level monitoring device being same as for regulating quench tower 1 that arranges, does not repeat them here.
By using above-mentioned tandem setting device, level monitoring device for quench tower, pH value monitoring device and one or more for separating of the fluid level control device of tower, can ensure the steady running of this vinyl cyanide system for separating and purifying, and ensure that each installs in good running status, further to improve the refining yield of vinyl cyanide, and further promote the purity of propylene steam nitrile.Certainly, the setting of above-mentioned each device is not limited to this, as long as can realize the control of liquid level, the temperature of knockout tower 2 and the flow of sulphuric acid soln of liquid level to knockout tower 2, quench tower 1.
Alternatively, be provided with finished product product outlet 18 at the tower top of quench tower 1, aforementioned finished product product is discharged by finished product product outlet 18, quench tower 1 inside is provided with the first spray equipment 19, the first spray equipment 19 is communicated with the first port that is communicated with pipeline section 8 of the tower top sidewall that is communicated to quench tower 1, ammoniumsulphate soln and sulphuric acid soln enter the first spray equipment 19 through the first connection pipeline section 8, and spray in quench tower 1 through the first spray equipment 19.By this structure, can increase sulphuric acid soln and contact area ammonia, and the liquid propylene nitrile that is conducive to carry secretly in ammoniumsulphate soln departs from ammoniumsulphate soln gasification, and then gas-phase propene nitrile after gasification can be discharged by finished product product outlet 18.
In addition, be also provided with reaction gas entrance 20 at quench tower 1 sidewall, quench tower 1 inside is also provided with the second spray equipment 21, and wherein, reaction gas entrance 20 is communicated with the second spray equipment 21.Thus, the ammonia in can augmenting response gas and the contact area of sulphuric acid soln, can react with sulphuric acid soln more ammonia and generate ammoniumsulphate soln, to reduce the ammonia in finished product product.
In addition, in knockout tower 2, tower tray is set, to strengthen separating effect.Be more preferably, 10 tower trays are set.
Table 1 is the material balance table of the process of the refining vinyl cyanide of application said system.With reference to following table, A, B, C, D, E are five material balance points shown in Fig. 1.Wherein, A point is positioned on the pipeline being connected with reaction gas entrance 20, with component and its physical features of detection reaction gas.B point is positioned at on finished product product outlet 18 pipelines that are connected, to detect component and its physical features of finished product product.C point is positioned on the second connection pipeline section 9, to detect component and its physical features of intermediate reaction product.D point is positioned on third connecting pipeline section 22, and with secondary component and its physical features of isolated gas-phase propene nitrile again, this secondary more isolated gas-phase propene nitrile can be mingled with other gases.E point is positioned on material recycle pipe 6, to detect component and its physical features of the reaction mass of being discharged by separator 2.Said components and physical features are listed particularly in table 1.
Table 1
Thing stream number |
? |
A |
B |
C |
D |
E |
Liquid phase fraction |
? |
0.000 |
0.000 |
0.847 |
0.000 |
0.828 |
Temperature |
℃ |
255.0 |
82.9 |
84.1 |
109.5 |
111.0 |
Pressure |
MPA |
0.1540 |
0.1460 |
0.4600 |
0.1440 |
0.1520 |
Mass rate |
KG/HR |
135380.97 |
147005.06 |
11986.11 |
1361.35 |
10624.76 |
Liquid phase actual flow |
M
3/HR
|
? |
? |
10.51 |
? |
9.24 |
Liquid phase actual density |
KG/M
3 |
? |
? |
965.93 |
? |
952.03 |
Gas phase actual flow |
M
3/HR
|
141300.22 |
113943.84 |
? |
1588.36 |
? |
Gas phase actual density |
KG/M
3 |
0.96 |
1.29 |
? |
0.86 |
? |
Constituent mass flow |
KG/HR |
? |
? |
? |
? |
? |
Vinyl cyanide |
KG/HR |
16917.68 |
16607.30 |
66.89 |
66.88 |
0.00 |
Acetonitrile |
KG/HR |
613.51 |
568.89 |
8.02 |
7.94 |
0.08 |
Prussic acid |
KG/HR |
1938.67 |
1762.26 |
8.18 |
8.17 |
0.00 |
Water |
KG/HR |
24014.16 |
36723.34 |
9394.79 |
1253.28 |
8141.51 |
Sulphur ammonium |
KG/HR |
0.00 |
0.00 |
1832.59 |
0.00 |
1832.59 |
Vinylformic acid |
KG/HR |
344.63 |
252.35 |
55.64 |
11.47 |
44.17 |
Propenal |
KG/HR |
178.74 |
134.06 |
0.81 |
0.81 |
0.00 |
Other components |
KG/HR |
91373.58 |
90956.86 |
619..19 |
12.79 |
606.4 |
These are only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.