CN103896805A - Method and equipment for production of adiponitrile from adipic acid - Google Patents
Method and equipment for production of adiponitrile from adipic acid Download PDFInfo
- Publication number
- CN103896805A CN103896805A CN201210577924.9A CN201210577924A CN103896805A CN 103896805 A CN103896805 A CN 103896805A CN 201210577924 A CN201210577924 A CN 201210577924A CN 103896805 A CN103896805 A CN 103896805A
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- Prior art keywords
- cyanation
- pipeline
- adiponitrile
- tower
- hexanodioic acid
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- BTGRAWJCKBQKAO-UHFFFAOYSA-N adiponitrile Chemical compound N#CCCCCC#N BTGRAWJCKBQKAO-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 11
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 title abstract 14
- 239000001361 adipic acid Substances 0.000 title abstract 7
- 235000011037 adipic acid Nutrition 0.000 title abstract 7
- 238000007333 cyanation reaction Methods 0.000 claims abstract description 93
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 82
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000000463 material Substances 0.000 claims abstract description 60
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 41
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 34
- 239000000047 product Substances 0.000 claims abstract description 17
- 238000003860 storage Methods 0.000 claims abstract description 17
- 239000003085 diluting agent Substances 0.000 claims abstract description 16
- 239000007791 liquid phase Substances 0.000 claims abstract description 11
- 239000012071 phase Substances 0.000 claims abstract description 8
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims description 56
- 239000000470 constituent Substances 0.000 claims description 33
- 238000009826 distribution Methods 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 230000008676 import Effects 0.000 claims description 15
- 238000002844 melting Methods 0.000 claims description 15
- 230000008018 melting Effects 0.000 claims description 15
- 238000000605 extraction Methods 0.000 claims description 14
- 239000006200 vaporizer Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 12
- 239000013067 intermediate product Substances 0.000 claims description 10
- 230000000630 rising effect Effects 0.000 claims description 10
- 238000006297 dehydration reaction Methods 0.000 claims description 7
- 239000002699 waste material Substances 0.000 claims description 6
- 230000007423 decrease Effects 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000010813 municipal solid waste Substances 0.000 claims description 3
- 238000009834 vaporization Methods 0.000 claims description 3
- 230000008016 vaporization Effects 0.000 claims description 3
- 230000006835 compression Effects 0.000 claims 1
- 238000007906 compression Methods 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract 3
- 229910019142 PO4 Inorganic materials 0.000 abstract 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 abstract 1
- 239000010452 phosphate Substances 0.000 abstract 1
- 238000004939 coking Methods 0.000 description 6
- JRZLXTBWVCJQFZ-UHFFFAOYSA-N 2-cyanopentanamide Chemical compound CCCC(C#N)C(N)=O JRZLXTBWVCJQFZ-UHFFFAOYSA-N 0.000 description 4
- GVNWZKBFMFUVNX-UHFFFAOYSA-N Adipamide Chemical compound NC(=O)CCCCC(N)=O GVNWZKBFMFUVNX-UHFFFAOYSA-N 0.000 description 4
- CDPFUVXUIHOXCW-UHFFFAOYSA-N CCCCC(OC#N)=O.N Chemical compound CCCCC(OC#N)=O.N CDPFUVXUIHOXCW-UHFFFAOYSA-N 0.000 description 4
- OSNDUYDDOHEKEE-UHFFFAOYSA-N azepane-2,7-dione Chemical compound O=C1CCCCC(=O)N1 OSNDUYDDOHEKEE-UHFFFAOYSA-N 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention relates to a method and equipment for production of adiponitrile from adipic acid, and mainly solves the problem of unstable product quality in the prior art for production of adiponitrile from adipic acid. The method employs materials of fusing adipic acid, ammonia, phosphate and a diluent. The production method is as below: mixing phosphoric acid with the diluent in a pipeline mixer; conducting neutralization of adipic acid and ammonia in a cyanation reactor; sending reaction products into the bottom of a separation tower for separation; recovering gas phase of light components from an outlet; sending the diluent recovered by a gas lifting plate into the pipeline mixer, mixing the diluent with phosphoric acid in the pipeline mixer, and sending the mixture into the cyanation reactor to dilute adipic acid; and sending a liquid phase to a scraper type evaporator. The employed equipment includes an adipic acid storage tank, an ammonia compressor, a cyanation reactor, a pipeline mixer, a separation tower, a tail gas removal tower, a phosphoric acid storage tank and a scraper type evaporator. The invention has the advantage of a good quality of the produced adiponitrile product.
Description
Technical field:
The present invention relates to a kind of method with hexanodioic acid production adiponitrile and the equipment using.
Background technology:
In existing method of producing adiponitrile with hexanodioic acid, catalyzer adds a little unreasonable, phosphoric acid catalyst adds before hexanodioic acid enters hexanodioic acid basin, in hexanodioic acid storage process, there is sedimentation in catalyzer, cause in the hexanodioic acid that enters reactor catalyst content unstable, low when time is high, be zero even sometimes.Make dehydration reaction unstable, partial material unreacted discharges system.
Gaseous ammonia enters reactor bottom by the pipe core of reactor, and due to the extruding of surrounding liquid, gas upwards flows along pipe core outer wall, and the contact area of gas phase and liquid phase is little, and mixing effect is undesirable.Because air-flow is more concentrated, velocity ratio is larger, and in reactor center part tubulation, material film forming is bad, complete reaction is not gone out outside pipe, causes reaction not thorough, and hexanodioic acid degraded is more serious, partial material, due to overheated and carbonization coking, has shortened the life cycle of reactor.Cause upper tubesheet coking serious.
The heavy constituent of carrying out autospasy tailing column intermittently enter the nethermost one deck tower tray of knockout tower (rising gas plate), then enter reactor as a part for thinner.The heavy constituent of carrying out autospasy tailing column is by adiponitrile, ammonium cyanovalerate, cyanovaleramide, hexanediamide, adipimide and be difficult for volatility product and form, and heavy constituent content in this material is more much bigger than rising heavy constituent content on gas plate.Because entering of this part material causes the material composition rising on gas plate unstable; Level fluctuation on liter gas plate is frequent, causes the overhead product produced quantity fluctuation by rising the control of gas plate liquid level frequent.Because produced quantity fluctuation frequently causes the operating parameter of each layer of column plate unstable, cause the unstable product quality of extraction because operating parameter is unstable.Due to intermediate product ammonium cyanovalerate, cyanovaleramide, hexanediamide, adipimide in heavy constituent be difficult for the existence of volatility product, cause the heavy constituent content of each layer of column plate above to increase, equally, the heavy constituent content in product production increases, and causes vicious cycle.Being difficult for after volatility product enters reactor in heavy constituent very easily causes coking at reactor, shortens reactor life cycle.
For above-mentioned reasons: make whole production process by product many, raw materials consumption is high; Reactor coking is serious, and the cycle of operation is short; Unstable product quality, heavy constituent content is higher; Production process is unstable, and operating parameter is wayward.
Summary of the invention:
Technical problem to be solved by this invention is to provide a kind of method with hexanodioic acid production adiponitrile and the equipment using.The adiponitrile good product quality going out with the method and device fabrication, by product is few, and raw materials consumption is low, and the coking of cyanation device is few, long service life.
Above-mentioned purpose is achieved in that
The material using with hexanodioic acid production adiponitrile and the weight ratio of material thereof are: melting hexanodioic acid: ammonia: phosphoric acid: thinner=1: 1.5: 0.003: 2.2;
Concrete production method is: when initial start-up, replace melting hexanodioic acid to join in cyanation device with adiponitrile, and add phosphoric acid, the weight ratio of adiponitrile and phosphoric acid is 1: 0.004; Heating cyanation device, heats up gradually, at the bottom of setting up cyanation device → knockout tower → and circulation between motoritis circulation line → cyanation device; In the time that in cyanation device, temperature reaches 100 DEG C, gaseous ammonia after being compressed by ammonia compressor, in ammonia pipeline enters into the pipe core of cyanation device, gaseous ammonia enters into cyanation device bottom from the top of pipe core backward mobile, it becomes several tiny bubble or air-flows behind several holes of umbrella even gas distribution device, adjust gaseous ammonia flow, and increase to gradually rated value 3300m
3/ h.
Along with the rising of cyanation actuator temperature, in knockout tower, rise gas plate liquid level and form, the material that knockout tower rises on gas plate turns back to cyanation device as thinner.In the time that cyanation device top is 250 DEG C towards the temperature out of knockout tower, regulate diluent mass flow to rated value 4800kg/h.Meanwhile, rise the liquid level of gas plate according to knockout tower, at tower top light constituent extraction mouth extraction adiponitrile.
At the bottom of knockout tower tower, liquid level starts to decline, when cyanation device internal pressure also declines, almost all vaporizations of adiponitrile in cyanation device are described, now in cyanation device, add melting hexanodioic acid, the melting hexanodioic acid being come by hexanodioic acid basin enters into cyanation device bottom, the thinner that is risen gas plate from knockout tower dilutes, and the inlet amount of melting hexanodioic acid is brought up to rated value 2400kg/h gradually.Meanwhile, in cyanation device, add phosphoric acid by diluent line; Now, stop cyanation device → knockout tower at the bottom of → circulation between motoritis circulation line → cyanation device.
Catalyzer phosphoric acid quantitatively joins with volume pump in the line mixer of installing on thinner pipeline, with mixing diluents.Add-on (weight ratio) is hexanodioic acid: phosphoric acid=1000: 1.8.
Hexanodioic acid and gaseous ammonia are carried out after neutralization reaction in cyanation device, continue to carry out dehydration reaction in the tubulation of cyanation device, temperature of reaction is 250--290 DEG C, dehydration reaction provides heat by DO steam, DO vapor temperature is initially 307 DEG C, the end of term in week is 340 DEG C, and reaction pressure is 0.04MPa; After reaction, reaction product is gas phase and liquid phase, entering knockout tower bottom through cyanation device reacting rear material outlet and pipeline separates, gas phase rises to each layer of column plate and continues to separate, then export energy extraction adiponitrile product from the light constituent on knockout tower top, rise gas plate extraction thinner, thinner enters in line mixer through thinner pipeline, mix with the catalyzer phosphoric acid entering in line mixer from catalyzer phosphoric acid storage tank, then enter into dilution hexanodioic acid in cyanation device.The weight ratio of hexanodioic acid and thinner is 1: 2.2; At the bottom of liquid phase falls into tower, deliver to scraper-type vaporizer and reclaim adiponitrile and intermediate product, waste material enters outside three wastes system.The heavy constituent of carrying out autospasy tailing column is by adiponitrile, intermediate product (ammonium cyanovalerate, cyanovaleramide, hexanediamide, adipimide) and be difficult for volatility product and form, intermittently enter knockout tower bottom, deliver to scraper-type vaporizer with the liquid phase reaction resultant falling at the bottom of tower, reclaim adiponitrile and intermediate product.
The equipment using comprises hexanodioic acid basin, ammonia compressor, cyanation device, line mixer, knockout tower, volume pump, de-tailing column, phosphoric acid storage tank and scraper-type vaporizer, wherein said cyanation device comprises housing, in housing, there is pipe core, pipe core top is gas material import, bottom is gas material outlet, material outlet after housing middle part responds, hexanodioic acid import and thinner import are arranged at the bottom of housing, in the housing of reacting rear material outlet below, there are upper tubesheet and lower tubesheet, on, between lower tubesheet, be connected with tubulation, pipe core is from upper, in lower tubesheet, pass through, on the pipe core of upper tubesheet top, there is expansion joint, on the pipe core of expansion joint top, there is pod, set up the even gas distribution device of umbrella in the bottom of pipe core, the central authorities of even gas distribution device are provided with the opening passing through for pipe core, even gas distribution device surrounding is fixed on housing, on even gas distribution device, have several holes, the total sectional area in several holes is greater than the sectional area of pipe core.
The outlet of ammonia compressor has ammonia pipeline to be connected with cyanation device inner central tube top, hexanodioic acid basin has pipeline to be connected with the hexanodioic acid import of cyanation device housing bottom, the material inlet arranging on the reacting rear material outlet at cyanation device middle part has pipeline and rises the tower body of gas plate below in knockout tower is connected, knockout tower comprises tower body, heavy constituent material relief outlet is arranged at the bottom of tower body, light constituent material outlet is arranged at the top of tower body, pneumatic outlet is arranged at the top of tower body, in tower body, rise gas plate, in the tower body of liter gas plate top, there is column plate, rising the reaction product entrance arranging on the tower body of gas plate below has pipeline to be connected with de-tailing column, the heavy constituent material relief outlet of knockout tower bottom has pipeline to be connected with scraper-type evaporator inlet, on pipeline between heavy constituent material relief outlet and the scraper-type evaporator inlet of knockout tower bottom, be also connected with motoritis circulating line, the other end of motoritis circulating line is connected with the bottom of cyanation device, on scraper-type vaporizer, there are reclaimed materials discharge tube and trash discharge pipeline, also comprise phosphoric acid storage tank, phosphoric acid storage tank outlet has pipeline to be connected with phosphoric acid volume pump entrance, the outlet of phosphoric acid volume pump has pipeline to be connected with line mixer entrance, the outlet of line mixer bottom has pipeline to be connected with the thinner import of cyanation device bottom, and line mixer top has thinner pipeline to be connected with the diluent inlet of knockout tower.
Advantage of the present invention is: owing to having set up line mixer, material is to add catalyzer while advancing, so catalyst content is stable in the material of output, reaction is normal, and by product is few.
Owing to having set up even gas distribution device in cyanation device, it can will be divided into some strands of threads or bubble from pipe core gas material out, increase the contact area of gas material and liquid material, mix, fast reaction speed, thoroughly, yield is high, can extend the work-ing life of cyanation device in reaction.
Because the material inlet of knockout tower is arranged on the tower body that rises gas plate below, in the material that operation is come below enters at the bottom of tower from material inlet, so rises liquid level on gas plate and material composition is relatively stable, overhead extraction thing (light constituent) flow is easy to control, quality is steady, and heavy constituent content is low.
So the adiponitrile good product quality going out with the method and device fabrication, by product is few, and raw materials consumption is low, and heavy constituent content is low, stable production process, and the coking of cyanation device is few, long service life.
Brief description of the drawings:
Fig. 1 is the structural representation of the equipment that uses in the present invention;
Fig. 2 is the structural representation of the knockout tower that amplifies in equipment used in the present invention;
Fig. 3 is the structural representation of the cyanation device that amplifies in equipment used in the present invention;
Fig. 4 is the structural representation of the even gas distribution device in the cyanation device amplifying.
Embodiment:
The material using with hexanodioic acid production adiponitrile and the weight ratio of material thereof are: melting hexanodioic acid: ammonia: phosphoric acid: thinner=1: 1.5: 0.003: 2.2;
Concrete production method is: when initial start-up, replace melting hexanodioic acid to join in cyanation device 3 with adiponitrile, and add phosphoric acid, the weight ratio of adiponitrile and phosphoric acid is 1: 0.004; Heating cyanation device, heats up gradually, sets up the circulation between 5 ends of cyanation device 3 → knockout tower → motoritis circulation line, 11 → cyanation device 3; In the time that in cyanation device, temperature reaches 100 DEG C, gaseous ammonia after being compressed by ammonia compressor 1, in ammonia pipeline 10 enters into the pipe core of cyanation device 3, gaseous ammonia enters into cyanation device bottom from the top of pipe core backward mobile, it becomes several tiny bubble or air-flows behind several holes of umbrella even gas distribution device, adjust gaseous ammonia flow, and increase to gradually rated value 3300m
3/ h;
Along with the rising of cyanation actuator temperature, the interior gas plate liquid level that rises of knockout tower 5 forms, and the material that knockout tower rises on gas plate turns back to cyanation device as thinner; In the time that cyanation device top is 250 DEG C towards the temperature out of knockout tower, regulate diluent mass flow to rated value 4800kg/h; Meanwhile, rise the liquid level of gas plate according to knockout tower, at tower top light constituent extraction mouth extraction adiponitrile;
At the bottom of knockout tower tower, liquid level starts to decline, when cyanation device internal pressure also declines, almost all vaporizations of adiponitrile in cyanation device are described, now in cyanation device, add melting hexanodioic acid, enter into cyanation device bottom by the melting hexanodioic acid of hexanodioic acid basin 2, the thinner that is risen gas plate from knockout tower dilutes, and the inlet amount of melting hexanodioic acid is brought up to rated value 2400kg/h gradually; Meanwhile, in cyanation device, add phosphoric acid by diluent line 14; Now, stop cyanation device → knockout tower at the bottom of → circulation between motoritis circulation line → cyanation device;
Catalyzer phosphoric acid in phosphoric acid storage tank 8 quantitatively joins with volume pump 7 in the line mixer 4 of installing on thinner pipeline, with mixing diluents; The weight ratio of hexanodioic acid and phosphoric acid add-on is 1000: 1.8;
Hexanodioic acid and gaseous ammonia are carried out after neutralization reaction in cyanation device, continue to carry out dehydration reaction in the tubulation of cyanation device, temperature of reaction is 250 DEG C or 270 DEG C or 290 DEG C, dehydration reaction provides heat by DO steam, DO vapor temperature is initially 307 DEG C, the end of term in week is 340 DEG C, and reaction pressure is 0.04MPa; After reaction, reaction product is gas phase and liquid phase, entering knockout tower bottom through cyanation device reacting rear material outlet and pipeline separates, gas phase rises to each layer of column plate and continues to separate, then export energy extraction adiponitrile product from the light constituent on knockout tower top, rise gas plate extraction thinner, thinner is in thinner pipeline 14 enters into line mixer 4, mix with the catalyzer phosphoric acid entering in line mixer from catalyzer phosphoric acid storage tank 8, then enter into dilution hexanodioic acid in cyanation device; The weight ratio of hexanodioic acid and thinner is 1: 2.2; At the bottom of liquid phase falls into tower, deliver to scraper-type vaporizer 9 and reclaim adiponitrile and intermediate product, waste material enters outside three wastes system; The heavy constituent of carrying out autospasy tailing column 6 is by adiponitrile, intermediate product (ammonium cyanovalerate, cyanovaleramide, hexanediamide, adipimide) and be difficult for volatility product and form, intermittently enter knockout tower bottom, deliver to scraper-type vaporizer with the liquid phase reaction resultant falling at the bottom of tower, reclaim adiponitrile and intermediate product.
See figures.1.and.2, the equipment using comprises hexanodioic acid basin 2, ammonia compressor 1, cyanation device 3, line mixer 4, knockout tower 5, volume pump 7, de-tailing column 6, phosphoric acid storage tank 8 and scraper-type vaporizer 9, the outlet of ammonia compressor 1 has ammonia pipeline 10 to be connected with cyanation device 3 inner central tube tops, hexanodioic acid basin 2 has pipeline to be connected with the hexanodioic acid import of cyanation device 3 housing bottoms, the reacting rear material outlet at cyanation device middle part has the interior material inlet 5-2 arranging on the tower body of gas plate below that rises of pipeline and knockout tower 5 to be connected, knockout tower 5 comprises tower body 5-5, heavy constituent material relief outlet 5-1 is arranged at the bottom of tower body, light constituent material outlet 5-7 is arranged at the top of tower body, pneumatic outlet 5-6 is arranged at the top of tower body, in tower body, rise gas plate 5-3, in the tower body of liter gas plate top, there is column plate 5-4, rising the reaction product entrance 5-9 arranging on the tower body of gas plate below has pipeline to be connected with de-tailing column 6, the heavy constituent material relief outlet 5-1 of knockout tower bottom has pipeline to be connected with scraper-type vaporizer 9 entrances, on pipeline between heavy constituent material relief outlet and the scraper-type evaporator inlet of knockout tower bottom, be also connected with motoritis circulating line 11, the other end of motoritis circulating line is connected with the bottom of cyanation device, on scraper-type vaporizer, there are reclaimed materials discharge tube 12 and trash discharge pipeline 13, also comprise phosphoric acid storage tank 8, phosphoric acid storage tank outlet has pipeline to be connected with volume pump 7 entrances, volume pump outlet has pipeline to be connected with line mixer 4 entrances, the outlet of line mixer bottom has pipeline to be connected with the thinner import of cyanation device bottom, and line mixer top has thinner pipeline 14 to be connected with the diluent inlet 5-8 of knockout tower.
With reference to Fig. 3 and Fig. 4, wherein said cyanation device 3 comprises housing 3-1, in housing, there is pipe core 3-2, pipe core top is gas material import, bottom is gas material outlet, material outlet 3-3 after housing middle part responds, hexanodioic acid import 3-4 and thinner import 3-11 are arranged at the bottom of housing, in the housing of reacting rear material outlet below, there are upper tubesheet 3-5 and lower tubesheet 3-6, on, between lower tubesheet, be connected with tubulation 3-7, pipe core is from upper, in lower tubesheet, pass through, on the pipe core of upper tubesheet top, there is expansion joint 3-8, on the pipe core of expansion joint top, there is pod 3-9, set up the even gas distribution device 3-10 of umbrella in the bottom of pipe core, the central authorities of even gas distribution device are provided with the opening passing through for pipe core, even gas distribution device surrounding is fixed on housing, on even gas distribution device, have several holes 3-12, the total sectional area in several holes is greater than the sectional area of pipe core.
Claims (3)
1. a method of producing adiponitrile with hexanodioic acid, is characterized in that: the material using and the weight ratio of material thereof are: melting hexanodioic acid: ammonia: phosphoric acid: thinner=1: 1.5: 0.003: 2.2;
Concrete production method is: when initial start-up, replace melting hexanodioic acid to join in cyanation device (3) with adiponitrile, and add phosphoric acid, the weight ratio of adiponitrile and phosphoric acid is 1: 0.004; Heating cyanation device, heats up gradually, sets up the circulation between cyanation device (3) → knockout tower (5) end → motoritis circulation line (11) → cyanation device (3); In the time that in cyanation device, temperature reaches 100 DEG C, by the gaseous ammonia after ammonia compressor (1) compression, enter in the pipe core of cyanation device (3) through ammonia pipeline (10), gaseous ammonia enters into cyanation device bottom from the top of pipe core backward mobile, it becomes several tiny bubble or air-flows behind several holes of umbrella even gas distribution device, adjust gaseous ammonia flow, and increase to gradually rated value 3300m
3/ h;
Along with the rising of cyanation actuator temperature, in knockout tower (5), rise gas plate liquid level and form, the material that knockout tower rises on gas plate turns back to cyanation device as thinner; In the time that cyanation device top is 250 DEG C towards the temperature out of knockout tower, regulate diluent mass flow to rated value 4800kg/h; Meanwhile, rise the liquid level of gas plate according to knockout tower, at tower top light constituent extraction mouth extraction adiponitrile;
At the bottom of knockout tower tower, liquid level starts to decline, when cyanation device internal pressure also declines, almost all vaporizations of adiponitrile in cyanation device are described, now in cyanation device, add melting hexanodioic acid, the melting hexanodioic acid being come by hexanodioic acid basin (2) enters into cyanation device bottom, the thinner that is risen gas plate from knockout tower dilutes, and the inlet amount of melting hexanodioic acid is brought up to rated value 2400kg/h gradually; Meanwhile, in cyanation device, add phosphoric acid by diluent line (14); Now, stop cyanation device → knockout tower at the bottom of → circulation between motoritis circulation line → cyanation device;
Catalyzer in phosphoric acid storage tank (8) for phosphoric acid volume pump (7) quantitatively join in the line mixer (4) of installing on thinner pipeline, with mixing diluents; The weight ratio of hexanodioic acid and phosphoric acid add-on is 1000: 1.8;
Hexanodioic acid and gaseous ammonia are carried out after neutralization reaction in cyanation device, continue to carry out dehydration reaction in the tubulation of cyanation device, temperature of reaction is 250 DEG C or 270 DEG C or 290 DEG C, dehydration reaction provides heat by DO steam, DO vapor temperature is initially 307 DEG C, the end of term in week is 340 DEG C, and reaction pressure is 0.04MPa; After reaction, reaction product is gas phase and liquid phase, entering knockout tower bottom through cyanation device reacting rear material outlet and pipeline separates, gas phase rises to each layer of column plate and continues to separate, then export energy extraction adiponitrile product from the light constituent on knockout tower top, rise gas plate extraction thinner, thinner is in thinner pipeline (14) enters into line mixer (4), mix with the catalyzer phosphoric acid entering in line mixer from catalyzer phosphoric acid storage tank (8), then enter into dilution hexanodioic acid in cyanation device; The weight ratio of hexanodioic acid and thinner is 1: 2.2; At the bottom of liquid phase falls into tower, deliver to scraper-type vaporizer (9) and reclaim adiponitrile and intermediate product, waste material enters outside three wastes system; The heavy constituent of carrying out autospasy tailing column (6) is by adiponitrile, intermediate product and be difficult for volatility product and form, and intermittently enters knockout tower bottom, delivers to scraper-type vaporizer with the liquid phase reaction resultant falling at the bottom of tower, reclaims adiponitrile and intermediate product.
2. produce with hexanodioic acid the equipment that adiponitrile uses, it is characterized in that: comprise hexanodioic acid basin (2), ammonia compressor (1), cyanation device (3), line mixer (4), knockout tower (5), volume pump (7), de-tailing column (6), phosphoric acid storage tank (8) and scraper-type vaporizer (9);
The outlet of ammonia compressor (1) has ammonia pipeline (10) to be connected with cyanation device (3) inner central tube top, hexanodioic acid basin (2) has pipeline to be connected with the hexanodioic acid import of cyanation device (3) housing bottom, the material inlet (5-2) arranging on the reacting rear material outlet at cyanation device middle part has pipeline and rises the tower body of gas plate below in knockout tower (5) is connected, knockout tower (5) comprises tower body (5-5), heavy constituent material relief outlet (5-1) is arranged at the bottom of tower body, light constituent material outlet (5-7) is arranged at the top of tower body, pneumatic outlet (5-6) is arranged at the top of tower body, in tower body, rise gas plate (5-3), in the tower body of liter gas plate top, there is column plate (5-4), rising the reaction product entrance (5-9) arranging on the tower body of gas plate below has pipeline to be connected with de-tailing column (6), the heavy constituent material relief outlet (5-1) of knockout tower bottom has pipeline to be connected with scraper-type vaporizer (9) entrance, on pipeline between heavy constituent material relief outlet and the scraper-type evaporator inlet of knockout tower bottom, be also connected with motoritis circulating line (11), the other end of motoritis circulating line is connected with the bottom of cyanation device, on scraper-type vaporizer, there are reclaimed materials discharge tube (12) and trash discharge pipeline (13), also comprise phosphoric acid storage tank (8), phosphoric acid storage tank outlet has pipeline to be connected with volume pump (7) entrance, volume pump outlet has pipeline to be connected with line mixer (4) entrance, the outlet of line mixer bottom has pipeline to be connected with the thinner import of cyanation device bottom, and line mixer top has thinner pipeline (14) to be connected with the diluent inlet (5-8) of knockout tower.
3. according to the equipment using with hexanodioic acid production adiponitrile claimed in claim 2, it is characterized in that: described cyanation device (3) comprises housing (3-1), in housing, there is pipe core (3-2), pipe core top is gas material import, bottom is gas material outlet, material outlet (3-3) after housing middle part responds, hexanodioic acid import (3-4) and thinner import (3-11) are arranged at the bottom of housing, in the housing of reacting rear material outlet below, there are upper tubesheet (3-5) and lower tubesheet (3-6), on, between lower tubesheet, be connected with tubulation (3-7), pipe core is from upper, in lower tubesheet, pass through, on the pipe core of upper tubesheet top, there is expansion joint (3-8), on the pipe core of expansion joint top, there is pod (3-9), set up the even gas distribution device (3-10) of umbrella in the bottom of pipe core, the central authorities of even gas distribution device are provided with the opening passing through for pipe core, even gas distribution device surrounding is fixed on housing, on even gas distribution device, have several holes (3-12), the total sectional area in several holes is greater than the sectional area of pipe core.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210577924.9A CN103896805B (en) | 2012-12-27 | 2012-12-27 | Method and equipment for production of adiponitrile from adipic acid |
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|---|---|---|---|
| CN201210577924.9A CN103896805B (en) | 2012-12-27 | 2012-12-27 | Method and equipment for production of adiponitrile from adipic acid |
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| CN103896805A true CN103896805A (en) | 2014-07-02 |
| CN103896805B CN103896805B (en) | 2015-04-15 |
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| CN201210577924.9A Active CN103896805B (en) | 2012-12-27 | 2012-12-27 | Method and equipment for production of adiponitrile from adipic acid |
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Cited By (11)
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| CN105797419A (en) * | 2016-05-11 | 2016-07-27 | 中国天辰工程有限公司 | Coking corrosion inhibitor for adiponitrile rectification device |
| CN106146345A (en) * | 2015-04-17 | 2016-11-23 | 中国石油天然气股份有限公司 | Adipic acid liquid phase method produces the method for adiponitrile |
| CN107325022A (en) * | 2017-08-09 | 2017-11-07 | 无锡殷达尼龙有限公司 | A kind of preparation method of Long carbon chain cyano group acid |
| CN108409606A (en) * | 2018-06-01 | 2018-08-17 | 重庆华峰化工有限公司 | A kind of production system of adiponitrile |
| CN108484442A (en) * | 2018-06-01 | 2018-09-04 | 重庆华峰化工有限公司 | A kind of process for purification of adiponitrile |
| CN108821997A (en) * | 2018-06-01 | 2018-11-16 | 重庆华峰化工有限公司 | A kind of preparation method of adiponitrile and products thereof |
| CN111056972A (en) * | 2019-12-16 | 2020-04-24 | 中国科学院大连化学物理研究所 | Application of alkyl quaternary phosphonium salt ionic liquid in synthesis of adiponitrile from adipic acid |
| CN111233703A (en) * | 2020-02-24 | 2020-06-05 | 山东金石新材料有限公司 | Primary diamine production equipment and method for producing primary diamine by adopting same |
| CN111250113A (en) * | 2018-11-30 | 2020-06-09 | 中国科学院大连化学物理研究所 | Application of super acidic catalyst in direct synthesis of adiponitrile from adipic acid |
| CN113264848A (en) * | 2020-01-29 | 2021-08-17 | 英威达纺织（英国）有限公司 | Production of adiponitrile |
| CN113429316A (en) * | 2021-06-30 | 2021-09-24 | 瑞典国际化工技术有限公司 | Method for refining adiponitrile |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106146345A (en) * | 2015-04-17 | 2016-11-23 | 中国石油天然气股份有限公司 | Adipic acid liquid phase method produces the method for adiponitrile |
| CN106146345B (en) * | 2015-04-17 | 2018-05-04 | 中国石油天然气股份有限公司 | The method that adipic acid liquid phase method produces adiponitrile |
| CN105797419A (en) * | 2016-05-11 | 2016-07-27 | 中国天辰工程有限公司 | Coking corrosion inhibitor for adiponitrile rectification device |
| CN105797419B (en) * | 2016-05-11 | 2018-01-26 | 中国天辰工程有限公司 | A kind of coking corrosion inhibiter for adiponitrile rectifier unit |
| CN107325022A (en) * | 2017-08-09 | 2017-11-07 | 无锡殷达尼龙有限公司 | A kind of preparation method of Long carbon chain cyano group acid |
| CN107325022B (en) * | 2017-08-09 | 2021-06-18 | 无锡殷达尼龙有限公司 | Preparation method of long-carbon-chain cyano acid |
| CN108409606B (en) * | 2018-06-01 | 2019-03-29 | 重庆华峰化工有限公司 | A kind of production system of adiponitrile |
| CN108821997A (en) * | 2018-06-01 | 2018-11-16 | 重庆华峰化工有限公司 | A kind of preparation method of adiponitrile and products thereof |
| CN108484442A (en) * | 2018-06-01 | 2018-09-04 | 重庆华峰化工有限公司 | A kind of process for purification of adiponitrile |
| CN108821997B (en) * | 2018-06-01 | 2021-03-16 | 重庆华峰聚酰胺有限公司 | Preparation method of adiponitrile and product thereof |
| CN108409606A (en) * | 2018-06-01 | 2018-08-17 | 重庆华峰化工有限公司 | A kind of production system of adiponitrile |
| CN111250113A (en) * | 2018-11-30 | 2020-06-09 | 中国科学院大连化学物理研究所 | Application of super acidic catalyst in direct synthesis of adiponitrile from adipic acid |
| CN111056972A (en) * | 2019-12-16 | 2020-04-24 | 中国科学院大连化学物理研究所 | Application of alkyl quaternary phosphonium salt ionic liquid in synthesis of adiponitrile from adipic acid |
| CN113264848A (en) * | 2020-01-29 | 2021-08-17 | 英威达纺织（英国）有限公司 | Production of adiponitrile |
| CN111233703A (en) * | 2020-02-24 | 2020-06-05 | 山东金石新材料有限公司 | Primary diamine production equipment and method for producing primary diamine by adopting same |
| CN113429316A (en) * | 2021-06-30 | 2021-09-24 | 瑞典国际化工技术有限公司 | Method for refining adiponitrile |
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| CN103896805B (en) | 2015-04-15 |
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