CN102659625A - Industrial production method of acrylonitrile - Google Patents
Industrial production method of acrylonitrile Download PDFInfo
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- CN102659625A CN102659625A CN2012101184732A CN201210118473A CN102659625A CN 102659625 A CN102659625 A CN 102659625A CN 2012101184732 A CN2012101184732 A CN 2012101184732A CN 201210118473 A CN201210118473 A CN 201210118473A CN 102659625 A CN102659625 A CN 102659625A
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Abstract
The invention provides an industrial production method of acrylonitrile, which comprises that the air, propylene and ammonia are subjected to ammoxidation inside a reactor and generate a reaction gas containing the acrylonitrile; the reaction gas enters a first tower and shock cooling, neutralization and cooling are achieved; the reaction gas which is subjected to shock cooling, neutralization and cooling enters a second tower and the water absorbs organic materials contained in the reaction gas; the water absorbing liquid enters a third tower, the acrylonitrile, hydrocyanic acid and water vapor steamed out by the third tower are subjected to condensation, and then separation of an aqueous phase and an organic phase is achieved in a quantizer of the third tower; the water phase inside the quantizer of the third tower are delivered to the third tower; the water phase introduced from a last piece of tower plates of a tower kettle of the third tower is subjected to heat exchange and then serves as absorbing water of the second tower; a gas phase containing acetonitrile is extracted from the side lines of the third tower and sent into a fourth tower and a rough acetonitrile product is obtained; and the organic phase in the quantizer of the third tower enters a fifth tower and a sixth tower sequentially and hydrocyanic acid and a acrylonitrile product are respectively obtained. According to the method, the reliability of a device is improved and the energy utilization is high.
Description
Technical field
The present invention relates to a kind of industrialized preparing process of vinyl cyanide.
Background technology
Vinyl cyanide is mainly used in productions such as acrylic fibers, paracril, adiponitrile, acrylic amide, ABS resin, medicine, also can be used for the production of hexanolactam, polyhydric alcohol polymer, and it has wide application prospect in fields such as synthon, viton, plastics.
For acrylonitrile process; The exploitation of its production technique, improvement, to improve what will pay close attention to especially be environment protection and occupational health; Regulation according to " classification of occupational contact poison hazard rating "; Mostly the toxicity of the related substance that acrylonitrile process relates to is extremely or highly harm, occurs problem of environmental pollution probably as flow process is unreasonable, and cause personal injury.Therefore, the principle of design of process method is to improve the safety of device as far as possible, reduces even stops effluxing of process stream.
For traditional process for production of acrylonitrile, its operating process is longer, and the waste water and gas of generation is more, and the comprehensive utilization aspect of device energy is still waiting further to improve and is perfect.Long operating process needs more investment ability to accomplish on the one hand, has also increased the leakage point in the device simultaneously, is disadvantageous for the security and the stability of system; The waste water and gas intractability of acrylonitrile installation is big, special treatment unit need be set handle, and the discharging that reduces waste water and gas helps to reduce plant investment, can improve competitiveness of product; The comprehensive utilization of energy is a systems engineering, and traditional technology relates to seldom in this respect, and each grade thermal source does not make full use of in the device, has caused the waste of energy, has also improved the working cost of device.
Summary of the invention
The problem that the present invention will solve provides a kind of industrialized preparing process of vinyl cyanide; Through optimization to conventional process flow; Can effectively reduce effluxing of device refuse, improve the continuity and the stability of device operation, improve the yield of product; Also saved the consumption of steam simultaneously, finally can produce qualified vinyl cyanide product through the comprehensive utilization of energy.
For solving the problems of the technologies described above; The technical scheme that the present invention adopts is: a kind of industrialized preparing process of vinyl cyanide; Comprise the steps: that air, propylene and ammonia oxidative ammonolysis take place generates the reactant gases that contains vinyl cyanide, prussic acid and acetonitrile in reactor drum; This reactant gases gets in a tower and accomplishes quenching, neutralization and cooling;, quenching, neutralization, refrigerative reactant gases absorb contained organic materials in getting into No. two towers with water; This water absorption liquid gets in No. three towers, and vinyl cyanide, prussic acid and the water vapour that No. three column overhead steam is through realizing separating of water and organic phase after the condensation in No. three tower quantizers, and the water in No. three tower quantizers is sent back in No. three towers; The water of drawing from No. three last piece column plates of Tata still circulates after heat exchange and does No. two towers and absorb water; The gas phase that contains acetonitrile is sent into tower No. four from the extraction of No. three tower side lines, obtains the crude acetonitrile product; No. three the interior organic phase of tower quantizer gets into No. five towers and No. six towers successively, obtains prussic acid and vinyl cyanide product respectively.
Specifically, method of the present invention comprises the steps:
Reaction raw materials propylene liquid and liquefied ammonia are mixed in the reactor drum behind vaporizer and suphtr.Another raw air of reaction gets into air after filtering, also gets into after compression and participates in reaction in the reactor drum.
In reactor drum, propylene, ammonia and air carry out oxidizing reaction and generate vinyl cyanide under catalyst action, also generate prussic acid, acetonitrile, carbon monoxide, carbonic acid gas, propenal, vinylformic acid and water etc. simultaneously.Reactant gases flows out in the thing and also comprises the unreacted propylene of part, ammonia, oxygen and nitrogen etc.Reaction generates gas and gets into the cyclonic separator in the reactor drum, and the catalyzer that reactant gases is carried secretly returns bed through cyclone dip-leg.Reactant gases is delivered to tower No. one after getting into the cooling of reactant gases water cooler.
Preferably, a described tower is 3 segment structures, i.e. hypomere chilling, stage casing neutralization and epimere cooling; Reactant gases from reactor drum is in tower of hypomere tower still entering, and the hypomere recycling waste water is sprayed the reactant gases quenching to about 70-90 ℃ through nozzle by a tower hypomere recycle pump; Reactant gases rises to midsection No. one through riser after the hypomere quenching, in the reactant gases unreacted ammonia be added in the sulfuric acid of a tower epimere and generate the sulphur ammonium; Process gas after overpickling gets into a tower epimere; Gas at first gets off the liquid phase separation of carrying secretly in the gas phase through scum dredger; This liquid phase is collected on the valve tray; Send in No. two towers through flow by gravity, gaseous phase materials gets into one section water cooler, also delivers to after gas temperature further is cooled to 30-50 ℃ in No. two towers.
Preferably, the stage casing of a said tower and hypomere are respectively equipped with 1 stripping tower (i.e. first stripping tower and second stripping tower).Midsection still liquid and hypomere still liquid except that a part as the spray liquid circulation, also send into first stripping tower and second stripping tower respectively, in stripping tower, a spot of vinyl cyanide material of carrying secretly in the liquid phase is come out to return tower No. one by stripping.
The ammonium sulfate solution of a midsection can send sulphur ammonium retrieving arrangement to produce ammonium sulfate products through stage casing still liquid pump, contains granules of catalyst in the hypomere still liquid, can deliver to the catalyst sedimentation groove.
The reactant gases that comes out from tower top gets into No. two tower bottoms, water counter-current absorption in tower, recover acrylonitrile and other organic reaction product.The tower still obtains contains vinyl cyanide, acetonitrile, prussic acid and other aqueous organic (Fu Shui), and this solution is delivered to tower No. three.In No. two towers, the most of gas of carbon monoxide, carbonic acid gas, nitrogen and unreacted oxygen and hydro carbons is delivered to the tower exhaust treatment system No. two through cat head.No. two tops of tower of poor-water entering from No. six tower reboilers spray absorption.
No. two tower bottoms is delivered to tower No. three through the still liquid pump.In No. three towers, water adopts the method for extracting rectifying that vinyl cyanide, prussic acid are separated with acetonitrile as solvent.The vinyl cyanide of No. three column overhead, prussic acid and water vapor are divided into organic phase and water through No. three tower condensing surfaces in No. three tower quantizers.Organic phase (being mainly crude acetonitrile) is delivered to tower No. five, and water is sent tower back to No. three by No. three tower water pumps.No. three tower bottomss are pumped to multiple-effect evaporation with No. three tower bottomss and handle.
Less organic poor-water (aqueous solvent) is contained in the bottom of No. three towers, and this water temp is 100-130 ℃.Preferably, the water (being the poor-water the preceding text) of drawing from No. three last piece column plates of Tata still, through series system successively as the thermal source of No. five towers and No. six tower reboilers.
The poor-water of No. three tower bottoms need be returned No. two towers and continue as solvent reactant gases to be absorbed, but its temperature is higher, for satisfying the cooling of assimilation effect needs; The present invention fully utilizes the poor-water heat of No. three tower bottoms; This water at first gets into the tower reboiler No. five, and series connection gets into No. six tower reboilers again after heat exchange, is that two towers provide heat; Recirculated water and steam have been saved in this measure, have good economic benefits.
The gas phase that contains acetonitrile, water and little hydrogen cyanic acid gets into No. four tower by the extraction of No. three tower side lines.In No. four towers, acetonitrile, water and prussic acid can be delivered to the acetonitrile refining device and produce the acetonitrile product from the cat head extraction.No. four the Tata still is mainly water, and this water pump is sent back in No. three towers.
Organic phase from No. three towers gets into No. five towers.No. five tower is a negative-pressure operation, and cat head obtains hydrogen cyanide product.Vinyl cyanide after the tower still obtains dewatering is delivered to tower No. six.No. six tower is also operated under the negative pressure.Because vinyl cyanide and water form azeotrope, so this column overhead obtains is vinyl cyanide and water, so the vinyl cyanide product from the extraction of No. six tower side lines, send the product storage tank after cooling off.The overhead product of No. six towers is back to tower No. three.The tower still is vinyl cyanide and high boiling material, also returns tower No. three through No. six tower bottoms pumps.
The present invention rationally is provided with the working pressure of No. five towers and No. six towers on the basis of negative-pressure operation, make the solvent poor-water of No. three towers can be through placed in-line mode successively as the thermal source of No. five towers and No. six tower reboilers.Preferably, No. five towers are negative-pressure operation, and tower top pressure is 60-90KPa (A), and tower still pressure is 80-110KPa (A), and No. six tower is also operated under the negative pressure, and tower top pressure is 20-60KPa (A), and tower still pressure is 50-90KPa (A).
Compare with traditional technology and related invention, the present invention has following advantage:
1, the present invention is designed to three sections structure with a tower, in a tower, has realized chilling, neutralization and the cooling of process gas, has strengthened the functions of the equipments of a tower; Compare with traditional technology; Relevant device is integrated, and the liquid under the scum dredger gets into No. two towers, the investment of having saved pump through flow by gravity; Simultaneously also reduce leakage point, improved the security and the safety of system.
2, the present invention respectively is provided with a stripping tower at tower hypomere and stage casing, a small amount of material stripping that contains in two sections the still liquid is come out materials such as a small amount of vinyl cyanide of carrying secretly in the recycle-water, acetonitrile, prussic acid.This technology has improved product yield; To produce vinyl cyanide product per ton; Through two sections recyclable vinyl cyanide of stripping, acetonitrile and the about 10.4kg of prussic acid, wherein the about 8kg of vinyl cyanide can improve product, sub product yield 1%; Simultaneously also reduce the content of vinyl cyanide material in the waste water, played the effect of protection environment.
3, because vinyl cyanide and prussic acid all have very strong toxicity, so vinyl cyanide generally all is negative-pressure operation with the hydrogen cyanide product tower, can effectively prevent the leakage of material, the security and the stability of raising device.The present invention rationally is provided with the working pressure of two towers on the basis of negative-pressure operation, make the solvent poor-water of No. three towers can be through placed in-line mode successively as the thermal source of No. five towers and No. six tower reboilers, the consumption of having saved recirculated water and steam; And No. five towers and No. six towers are by steam thermal source to be provided in the traditional technology, produce vinyl cyanide product needed per ton and consume 10.4t steam, also need consume 49.2m simultaneously
3Recirculated water (in 10 ℃ of temperature difference) is used to cool off the solvent poor-water.The method of the invention total energy approach degree is high, and the pressure and the temperature of poor-water are more gentle simultaneously, has prolonged the work-ing life of reboiler greatly, has reduced the operational risk of reboiler, the security that has greatly improved system.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Among the figure:
1, reactor drum 2, tower 3, No. two towers
4, No. three towers 5, No. four towers 6, No. five towers
7, No. six towers 8, first stripping tower 9, second stripping tower
Embodiment
Below in conjunction with specific embodiment the present invention is described further, but does not limit protection scope of the present invention.
Embodiment 1
Reaction raw materials propylene liquid and liquefied ammonia are mixed in the reactor drum 1 behind vaporizer and suphtr.Another raw air of reaction gets into air after filtering, also gets into after compression and participates in reaction in the reactor drum 1.
In reactor drum 1, propylene, ammonia and air carry out oxidizing reaction and generate vinyl cyanide under catalyst action, also generate prussic acid, acetonitrile, carbon monoxide, carbonic acid gas, propenal, vinylformic acid and water etc. simultaneously.Reactant gases flows out in the thing and also comprises the unreacted propylene of part, ammonia, oxygen and nitrogen etc.Reaction generates gas and gets into the cyclonic separator in the reactor drum 1, and the catalyzer that reactant gases is carried secretly returns bed through cyclone dip-leg.Reactant gases is delivered to tower 2 No. one after getting into the cooling of reactant gases water cooler.
No. one tower 2 is divided into three parts, i.e. hypomere chilling, stage casing neutralization and epimere cooling.In the reactant gases that comes from reactor drum 1 gets into tower 2 from hypomere tower still, the hypomere recycling waste water by tower 2 hypomere recycle pump through the nozzle spray with the reactant gases quenching to about 70 ℃.Reactant gases rises to tower 2 stage casings No. one through riser after the hypomere quenching, in the reactant gases unreacted ammonia be added in the sulfuric acid of tower 2 epimeres and generate the sulphur ammonium.Process gas after overpickling gets into tower 2 epimeres; Gas at first gets off the liquid phase separation of carrying secretly in the gas phase through scum dredger; This liquid phase is collected on the valve tray; Send into through flow by gravity in No. two towers 3 of distillation system, gaseous phase materials gets into one section water cooler, and gas temperature further is cooled in No. two towers 3 also delivering to distillation system after 30 ℃.Tower 2 stage casing still liquid and hypomere still liquid except that a part as the spray liquid circulation, also send into first stripping tower 8 and second stripping tower 9 respectively, in stripping tower, a spot of vinyl cyanide material of carrying secretly in the liquid phase is come out to return tower 2 No. one by stripping.
The ammonium sulfate solution in tower 2 stage casings can send sulphur ammonium retrieving arrangement to produce ammonium sulfate products through stage casing still liquid pump, contains granules of catalyst in the hypomere still liquid, can deliver to the catalyst sedimentation groove.
The reactant gases that comes out from tower 2 top gets into No. two tower 3 bottoms, water counter-current absorption in tower, recover acrylonitrile and other organic reaction product.The tower still obtains contains vinyl cyanide, acetonitrile, prussic acid and other aqueous organic (Fu Shui), and this solution is delivered to tower 4 No. three.In No. two towers 3, the most of gas of carbon monoxide, carbonic acid gas, nitrogen and unreacted oxygen and hydro carbons is delivered to tower 3 exhaust treatment systems No. two through cat head.No. two tower 3 tops of poor-water entering from No. six tower reboilers spray absorption.
No. two tower 3 still liquid are delivered to tower 4 No. three through the still liquid pump.In No. three towers 4, water adopts the method for extracting rectifying that vinyl cyanide, prussic acid are separated with acetonitrile as solvent.Vinyl cyanide, prussic acid and the water vapor on No. three tower 4 tops are divided into organic phase and water through No. three tower 4 condensing surfaces in No. three tower quantizers.Organic phase (being mainly crude acetonitrile) is delivered to tower 6 No. five, and water is sent tower 4 back to No. three by No. three tower 4 water pumps.No. three tower 4 still liquid are delivered to multiple-effect evaporation with No. three tower 4 still liquid pumps and are handled.Less organism is contained in the bottom of No. three towers 4; Poor-water (aqueous solvent) is drawn from No. three last piece column plates of tower 4 tower stills and is got into a surge tank, and this water temp is 100 ℃, at first gets into tower 6 reboilers No. five; Series connection gets into No. six tower reboilers again after heat exchange, is that two towers provide heat.
The gas phase that contains acetonitrile, water and little hydrogen cyanic acid gets into No. four tower 5 by No. three tower 4 side line extraction.In No. four towers 5, acetonitrile, water and prussic acid can be delivered to the acetonitrile refining device and produce the acetonitrile product from the cat head extraction.No. four tower 5 tower stills are mainly water, and this water pump is sent back in No. three towers 4.
Organic phase from No. three towers 4 gets into No. five towers 6.No. five tower 6 is a negative-pressure operation, and tower top pressure is 60KPa (A), and tower still pressure is 80KPa (A), and cat head obtains hydrogen cyanide product.Vinyl cyanide after the tower still obtains dewatering is delivered to tower 7 No. six.
No. six tower 7 is also operated under the negative pressure, and tower top pressure is 20KPa (A), and tower still pressure is 50KPa (A).What this column overhead obtained is vinyl cyanide and water, and the vinyl cyanide product send the product storage tank from No. six tower 7 side line extraction after cooling.The overhead product of No. six towers 7 is back to tower 4 No. three.The tower still is vinyl cyanide and high boiling material, also returns tower 4 No. three through No. six tower 7 still liquid pumps.
Embodiment 2
Reaction raw materials propylene liquid and liquefied ammonia are mixed in the reactor drum 1 behind vaporizer and suphtr.Another raw air of reaction gets into air after filtering, also gets into after compression and participates in reaction in the reactor drum 1.
In reactor drum 1, propylene, ammonia and air carry out oxidizing reaction and generate vinyl cyanide under catalyst action, also generate prussic acid, acetonitrile, carbon monoxide, carbonic acid gas, propenal, vinylformic acid and water etc. simultaneously.Reactant gases flows out in the thing and also comprises the unreacted propylene of part, ammonia, oxygen and nitrogen etc.Reaction generates gas and gets into the cyclonic separator in the reactor drum 1, and the catalyzer that reactant gases is carried secretly returns bed through cyclone dip-leg.Reactant gases is delivered to tower 2 No. one after getting into the cooling of reactant gases water cooler.
No. one tower 2 is divided into three parts, i.e. hypomere chilling, stage casing neutralization and epimere cooling.In the reactant gases that comes from reactor drum 1 gets into tower 2 from hypomere tower still, the hypomere recycling waste water by tower 2 hypomere recycle pump through the nozzle spray with the reactant gases quenching to about 83 ℃.Reactant gases rises to tower 2 stage casings No. one through riser after the hypomere quenching, in the reactant gases unreacted ammonia be added in the sulfuric acid of tower 2 epimeres and generate the sulphur ammonium.Process gas after overpickling gets into tower 2 epimeres; Gas at first gets off the liquid phase separation of carrying secretly in the gas phase through scum dredger; This liquid phase is collected on the valve tray; Send into through flow by gravity in No. two towers 3 of distillation system, gaseous phase materials gets into one section water cooler, and gas temperature further is cooled in No. two towers 3 also delivering to distillation system after 40 ℃.Tower 2 stage casing still liquid and hypomere still liquid except that a part as the spray liquid circulation, also send into first stripping tower 8 and second stripping tower 9 respectively, in stripping tower, a spot of vinyl cyanide material of carrying secretly in the liquid phase is come out to return tower 2 No. one by stripping.
The ammonium sulfate solution in tower 2 stage casings can send sulphur ammonium retrieving arrangement to produce ammonium sulfate products through stage casing still liquid pump, contains granules of catalyst in the hypomere still liquid, can deliver to the catalyst sedimentation groove.
The reactant gases that comes out from tower 2 top gets into No. two tower 3 bottoms, water counter-current absorption in tower, recover acrylonitrile and other organic reaction product.The tower still obtains contains vinyl cyanide, acetonitrile, prussic acid and other aqueous organic (Fu Shui), and this solution is delivered to tower 4 No. three.In No. two towers 3, the most of gas of carbon monoxide, carbonic acid gas, nitrogen and unreacted oxygen and hydro carbons is delivered to tower 3 exhaust treatment systems No. two through cat head.No. two tower 3 tops of poor-water entering from No. six tower reboilers spray absorption.
No. two tower 3 still liquid are delivered to tower 4 No. three through the still liquid pump.In No. three towers 4, water adopts the method for extracting rectifying that vinyl cyanide, prussic acid are separated with acetonitrile as solvent.The vinyl cyanide of No. three tower 4 cats head, prussic acid and water vapor are divided into organic phase and water through No. three tower 4 condensing surfaces in No. three tower quantizers.Organic phase (being mainly crude acetonitrile) is delivered to tower 6 No. five, and water is sent tower 4 back to No. three by No. three tower 4 water pumps.No. three tower 4 tower bottomss are pumped to multiple-effect evaporation with No. three tower 4 tower bottomss and handle.Less organism is contained in the bottom of No. three towers 4; Poor-water (aqueous solvent) is drawn from No. three last piece column plates of tower 4 tower stills and is got into a surge tank, and this water temp is 115 ℃, at first gets into the tower reboiler No. five; Series connection gets into No. six tower reboilers again after heat exchange, is that two towers provide heat.
The gas phase that contains acetonitrile, water and little hydrogen cyanic acid gets into No. four tower 5 by No. three tower 4 side line extraction.In No. four towers 5, acetonitrile, water and prussic acid can be delivered to the acetonitrile refining device and produce the acetonitrile product from the cat head extraction.No. four tower 5 tower stills are mainly water, and this water pump is sent back in No. three towers 4.
Organic phase from No. three towers 4 gets into No. five towers 6.No. five tower 6 is a negative-pressure operation, and tower top pressure is 75KPa (A), and tower still pressure is 95KPa (A), and cat head obtains hydrogen cyanide product.Vinyl cyanide after the tower still obtains dewatering is delivered to tower 7 No. six.
No. six tower 7 is also operated under the negative pressure, and tower top pressure is 40KPa (A), and tower still pressure is 70KPa (A).What this column overhead obtained is vinyl cyanide and water, and the vinyl cyanide product send the product storage tank from No. six tower 7 side line extraction after cooling.The overhead product of No. six towers 7 is back to tower 4 No. three.The tower still is vinyl cyanide and high boiling material, also returns tower 4 No. three through No. six tower 7 still liquid pumps.
Embodiment 3
Reaction raw materials propylene liquid and liquefied ammonia are mixed in the reactor drum 1 behind vaporizer and suphtr.Another raw air of reaction gets into air after filtering, also gets into after compression and participates in reaction in the reactor drum 1.
In reactor drum 1, propylene, ammonia and air carry out oxidizing reaction and generate vinyl cyanide under catalyst action, also generate prussic acid, acetonitrile, carbon monoxide, carbonic acid gas, propenal, vinylformic acid and water etc. simultaneously.Reactant gases flows out in the thing and also comprises the unreacted propylene of part, ammonia, oxygen and nitrogen etc.Reaction generates gas and gets into the cyclonic separator in the reactor drum 1, and the catalyzer that reactant gases is carried secretly returns bed through cyclone dip-leg.Reactant gases is delivered to tower 2 No. one after getting into the cooling of reactant gases water cooler.
No. one tower 2 is divided into three parts, i.e. hypomere chilling, stage casing neutralization and epimere cooling.In the reactant gases that comes from reactor drum 1 gets into tower 2 from hypomere tower still, the hypomere recycling waste water by tower 2 hypomere recycle pump through the nozzle spray with the reactant gases quenching to about 90 ℃.Reactant gases rises to tower 2 stage casings No. one through riser after the hypomere quenching, in the reactant gases unreacted ammonia be added in the sulfuric acid of tower 2 epimeres and generate the sulphur ammonium.Process gas after overpickling gets into tower 2 epimeres; Gas at first gets off the liquid phase separation of carrying secretly in the gas phase through scum dredger; This liquid phase is collected on the valve tray; Send into through flow by gravity in No. two towers 3 of distillation system, gaseous phase materials gets into one section water cooler, and gas temperature further is cooled in No. two towers 3 also delivering to distillation system after 50 ℃.Tower 2 stage casing still liquid and hypomere still liquid except that a part as the spray liquid circulation, also send into first stripping tower 8 and second stripping tower 9 respectively, in stripping tower, a spot of vinyl cyanide material of carrying secretly in the liquid phase is come out to return tower 2 No. one by stripping.
The ammonium sulfate solution in tower 2 stage casings can send sulphur ammonium retrieving arrangement to produce ammonium sulfate products through stage casing still liquid pump, contains granules of catalyst in the hypomere still liquid, can deliver to the catalyst sedimentation groove.
The reactant gases that comes out from tower 2 top gets into No. two tower 3 bottoms, water counter-current absorption in tower, recover acrylonitrile and other organic reaction product.The tower still obtains contains vinyl cyanide, acetonitrile, prussic acid and other aqueous organic (Fu Shui), and this solution is delivered to tower 4 No. three.In No. two towers 3, the most of gas of carbon monoxide, carbonic acid gas, nitrogen and unreacted oxygen and hydro carbons is delivered to tower 3 exhaust treatment systems No. two through cat head.No. two tower 3 tops of poor-water entering from No. six tower reboilers spray absorption.
No. two tower 3 still liquid are delivered to tower 4 No. three through the still liquid pump.In No. three towers 4, water adopts the method for extracting rectifying that vinyl cyanide, prussic acid are separated with acetonitrile as solvent.The vinyl cyanide of No. three tower 4 cats head, prussic acid and water vapor are divided into organic phase and water through No. three tower 4 condensing surfaces in No. three tower quantizers.Organic phase (being mainly crude acetonitrile) is delivered to tower 6 No. five, and water is sent tower 4 back to No. three by No. three tower 4 water pumps.No. three tower 4 tower bottomss are pumped to multiple-effect evaporation with No. three tower 4 tower bottomss and handle.Less organism is contained in the bottom of No. three towers 4; Poor-water (aqueous solvent) is drawn from No. three last piece column plates of tower 4 tower stills and is got into a surge tank, and this water temp is 130 ℃, at first gets into the tower reboiler No. five; Series connection gets into No. six tower reboilers again after heat exchange, is that two towers provide heat.
The gas phase that contains acetonitrile, water and little hydrogen cyanic acid gets into No. four tower 5 by No. three tower 4 side line extraction.In No. four towers 5, acetonitrile, water and prussic acid can be delivered to the acetonitrile refining device and produce the acetonitrile product from the cat head extraction.No. four tower 5 tower stills are mainly water, and this water pump is sent back in No. three towers 4.
Organic phase from No. three towers 4 gets into No. five towers 6.No. five tower 6 is a negative-pressure operation, and tower top pressure is 90KPa (A), and tower still pressure is 110KPa (A), and cat head obtains hydrogen cyanide product.Vinyl cyanide after the tower still obtains dewatering is delivered to tower 7 No. six.
No. six tower 7 is also operated under the negative pressure, and tower top pressure is 60KPa (A), and tower still pressure is 90KPa (A).What this column overhead obtained is vinyl cyanide and water, and the vinyl cyanide product send the product storage tank from No. six tower 7 side line extraction after cooling.The overhead product of No. six towers 7 is back to tower 4 No. three.The tower still is vinyl cyanide and high boiling material, also returns tower 4 No. three through No. six tower 7 still liquid pumps.
More than preferred embodiment of the present invention is specified, but said content is merely preferred embodiment of the present invention, can not be considered to be used to limit practical range of the present invention.All equalizations of doing according to application range of the present invention change and improve etc., all should still belong within the patent covering scope of the present invention.
Claims (5)
1. the industrialized preparing process of a vinyl cyanide; It is characterized in that: comprise the steps: that air, propylene and ammonia oxidative ammonolysis take place generates the reactant gases that contains vinyl cyanide, prussic acid and acetonitrile in reactor drum; This reactant gases gets in a tower and accomplishes quenching, neutralization and cooling;, quenching, neutralization, refrigerative reactant gases absorb contained organic materials in getting into No. two towers with water; This water absorption liquid gets in No. three towers, and vinyl cyanide, prussic acid and the water vapour that No. three column overhead steam is through realizing separating of water and organic phase after the condensation in No. three tower quantizers, and the water in No. three tower quantizers is sent back in No. three towers; The water of drawing from No. three last piece column plates of Tata still circulates after heat exchange and does No. two towers and absorb water; The gas phase that contains acetonitrile is sent into tower No. four from the extraction of No. three tower side lines, obtains the crude acetonitrile product; No. three the interior organic phase of tower quantizer gets into No. five towers and No. six towers successively, obtains prussic acid and vinyl cyanide product respectively.
2. the industrialized preparing process of vinyl cyanide according to claim 1, it is characterized in that: a described tower is 3 segment structures, i.e. hypomere chilling, stage casing neutralization and epimere cooling; Reactant gases from reactor drum is in tower of hypomere tower still entering, and the hypomere recycling waste water is sprayed the reactant gases quenching to about 70-90 ℃ through nozzle by a tower hypomere recycle pump; Reactant gases rises to midsection No. one through riser after the hypomere quenching, in the reactant gases unreacted ammonia be added in the sulfuric acid of a tower epimere and generate the sulphur ammonium; Process gas after overpickling gets into a tower epimere; Gas at first gets off the liquid phase separation of carrying secretly in the gas phase through scum dredger; This liquid phase is collected on the valve tray; Send in No. two towers through flow by gravity, gaseous phase materials gets into one section water cooler, also delivers to after gas temperature further is cooled to 30-50 ℃ in No. two towers.
3. the industrialized preparing process of vinyl cyanide according to claim 1 and 2, it is characterized in that: the stage casing of a said tower and hypomere are respectively equipped with 1 stripping tower.
4. according to the industrialized preparing process of each described vinyl cyanide of claim 1-3, it is characterized in that: the water of drawing from No. three last piece column plates of Tata still, through series system successively as the thermal source of No. five towers and No. six tower reboilers.
5. the industrialized preparing process of vinyl cyanide according to claim 4, it is characterized in that: the tower top pressure of No. five towers is 60-90KPa (A), tower still pressure is 80-110KPa (A); No. six towers also are negative-pressure operation, and tower top pressure is 20-60KPa (A), and tower still pressure is 50-90KPa (A).
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| CN104672106A (en) * | 2015-03-06 | 2015-06-03 | 英尼奥斯欧洲股份公司 | Improved acrylonitrile manufacture process |
| CN104693068A (en) * | 2015-03-06 | 2015-06-10 | 英尼奥斯欧洲股份公司 | Improved acrylonitrile production |
| CN104693069A (en) * | 2015-03-06 | 2015-06-10 | 英尼奥斯欧洲股份公司 | Improved acrylonitrile production |
| CN104941380A (en) * | 2014-03-31 | 2015-09-30 | 英尼奥斯欧洲股份公司 | Improved smog eliminator operation for quenching effluent |
| CN105597360A (en) * | 2014-09-29 | 2016-05-25 | 英尼奥斯欧洲股份公司 | Evaporation system for process stream |
| CN105985262A (en) * | 2015-03-06 | 2016-10-05 | 英尼奥斯欧洲股份公司 | Improved acrylonitrile preparation |
| CN106474900A (en) * | 2015-08-26 | 2017-03-08 | 中国石油化工股份有限公司 | Improve recovery of acrylonitrile the chilling tower apparatus of reduces cost and quick cooling method |
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| CN104693068A (en) * | 2015-03-06 | 2015-06-10 | 英尼奥斯欧洲股份公司 | Improved acrylonitrile production |
| CN104693069A (en) * | 2015-03-06 | 2015-06-10 | 英尼奥斯欧洲股份公司 | Improved acrylonitrile production |
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| CN112441948A (en) * | 2019-09-05 | 2021-03-05 | 中石油吉林化工工程有限公司 | Comprehensive utilization method and system for energy of water recovered by dehydrocyanation tower |
| CN112439302A (en) * | 2019-09-05 | 2021-03-05 | 中石油吉林化工工程有限公司 | Tail gas treatment method in acrylonitrile production system |
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