CN103896805B - Method and equipment for production of adiponitrile from adipic acid - Google Patents
Method and equipment for production of adiponitrile from adipic acid Download PDFInfo
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- CN103896805B CN103896805B CN201210577924.9A CN201210577924A CN103896805B CN 103896805 B CN103896805 B CN 103896805B CN 201210577924 A CN201210577924 A CN 201210577924A CN 103896805 B CN103896805 B CN 103896805B
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- cyanation
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- adiponitrile
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- 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 17
- 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
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 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 30
- 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
- 230000000630 rising effect Effects 0.000 claims description 11
- 239000013067 intermediate product Substances 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
- 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 that hexanodioic acid produces adiponitrile and the equipment used.
Background technology:
It is unreasonable that existing hexanodioic acid produces catalyzer addition point in the method for adiponitrile, phosphoric acid catalyst adds before hexanodioic acid enters hexanodioic acid basin, in hexanodioic acid storage process, there is sedimentation in catalyzer, cause catalyst content in the hexanodioic acid entering reactor unstable, time height time low, be zero even sometimes.Make dehydration reaction unstable, namely 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 centrally pipe outer wall upwards flows, 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 comparatively large, and in reactor center part tubulation, material film forming is bad, namely non-complete reaction is gone out outside pipe, and cause reaction not thorough, hexanodioic acid degraded is more serious, partial material, due to overheated and carbonization coking, shortens the life cycle of reactor.Cause upper tubesheet coking serious.
That carrys out the heavy constituent interval of autospasy tailing column enters the nethermost one deck tower tray of knockout tower (namely rising gas plate), and the part then as thinner enters reactor.The heavy constituent carrying out autospasy tailing column by adiponitrile, ammonium cyanovalerate, cyanovaleramide, hexanediamide, adipimide and not easily volatility product form, and heavy constituent content in this material is more much bigger than the heavy constituent content risen on gas plate.Because entering of this part material causes the material composition risen on gas plate unstable; The level fluctuation risen on gas plate is frequent, causes the overhead product produced quantity fluctuation by rising gas plate Liquid level frequent.Because produced quantity fluctuation frequently causes the operating parameter of each layer column plate unstable, because operating parameter instability causes the unstable product quality of extraction.Due to the existence of intermediate product ammonium cyanovalerate in heavy constituent, cyanovaleramide, hexanediamide, adipimide and not easily volatility product, the heavy constituent content of each layer column plate is above caused to increase, equally, the heavy constituent content in product production increases, and causes vicious cycle.Very easily cause coking at reactor after not easily volatility product in heavy constituent enters reactor, shorten 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 that hexanodioic acid produces adiponitrile and the equipment used.The adiponitrile good product quality gone 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 used 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: during initial start-up, and 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, to set up at the bottom of cyanation device → knockout tower → motoritis circulation line → cyanation device between circulation; When in cyanation device, temperature reaches 100 DEG C, gaseous ammonia after being compressed by ammonia compressor, in the pipe core that ammonia pipeline enters into cyanation device, gaseous ammonia enters into backward upper flowing bottom cyanation device from the top of pipe core, it becomes several tiny bubble or air-flows behind several holes of umbrella even gas distribution device, adjustment gaseous ammonia flow, and increase to rated value 3300m gradually
3/ h.
Along with the rising of cyanation actuator temperature, rise gas plate liquid level in knockout tower and formed, the material that knockout tower rises on gas plate turns back to cyanation device as thinner.When the temperature out that cyanation device top leads to knockout tower is 250 DEG C, 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, illustrate that the adiponitrile in cyanation device is almost all vaporized, now in cyanation device, add melting hexanodioic acid, the melting hexanodioic acid come by hexanodioic acid basin enters into bottom cyanation device, diluted by the thinner rising gas plate from knockout tower, the inlet amount of melting hexanodioic acid is brought up to rated value 2400kg/h gradually.Meanwhile, in cyanation device, phosphoric acid is added by diluent line; Now, to stop at the bottom of cyanation device → knockout tower → motoritis circulation line → cyanation device between circulation.
Catalyzer phosphoric acid volume pump quantitatively joins in line mixer that thinner pipeline is installed, with mixing diluents.Add-on (weight ratio) is hexanodioic acid: phosphoric acid=1000: 1.8.
After hexanodioic acid and gaseous ammonia carry out 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, enter bottom knockout tower through the outlet of cyanation device reacting rear material and pipeline and be separated, gas phase rises to each layer column plate and continues to be separated, then from the light fraction outlet energy extraction adiponitrile product on knockout tower top, rise gas plate extraction thinner, thinner enters in line mixer through thinner pipeline, with the catalyzer phosphoric acid entered in line mixer mixes 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; Liquid phase falls at the bottom of tower, and deliver to scraper-type vaporizer and reclaim adiponitrile and intermediate product, waste material then enters outside three wastes system.The heavy constituent carrying out autospasy tailing column by adiponitrile, intermediate product (ammonium cyanovalerate, cyanovaleramide, hexanediamide, adipimide) and not easily volatility product form, interval enters bottom knockout tower, deliver to scraper-type vaporizer with the liquid phase reaction resultant fallen at the bottom of tower, reclaim adiponitrile and intermediate product.
The equipment used 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, pipe core is had in housing, pipe core top is gas material import, bottom is gas material outlet, material outlet after housing central section responds, hexanodioic acid import and thinner import are arranged at the bottom of housing, upper tubesheet and lower tubesheet is had in the housing of reacting rear material outlet below, on, tubulation is connected with between lower tubesheet, pipe core is from upper, pass through in lower tubesheet, pipe core above upper tubesheet there is expansion joint, pipe core above expansion joint there is pod, the even gas distribution device of umbrella is set up in the bottom of pipe core, the central authorities of even gas distribution device are provided with the opening passed through for pipe core, even gas distribution device surrounding is fixed on housing, even gas distribution device has 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, reacting rear material outlet in the middle part of cyanation device has pipeline to be connected with the material inlet that the tower body risen in knockout tower below gas plate is arranged, knockout tower comprises tower body, heavy constituent material 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, gas plate is risen in tower body, rise in the tower body above gas plate and have column plate, rising the reaction product entrance that the tower body below gas plate is arranged has pipeline to be connected with de-tailing column, heavy constituent material outlet bottom knockout tower has pipeline to be connected with scraper-type evaporator inlet, heavy constituent material outlet bottom knockout tower and the pipeline between scraper-type evaporator inlet are also connected with motoritis circulating line, the other end of motoritis circulating line is connected with the bottom of cyanation device, 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, outlet bottom line mixer has pipeline to be connected with the thinner import bottom cyanation device, 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, and material is advanced while add catalyzer, so catalyst content is stablized in the material exported, reaction is normal, and by product is few.
Owing to having set up even gas distribution device in cyanation device, it can be divided into some strands of threads or bubble by from pipe core gas material out, add 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 risen below gas plate, the material that operation is come below enters at the bottom of tower from material inlet, so the liquid level risen on gas plate and material form 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 gone 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.
Accompanying drawing illustrates:
Fig. 1 is the structural representation of the equipment used in the present invention;
Fig. 2 is the structural representation of the knockout tower amplified in equipment used in the present invention;
Fig. 3 is the structural representation of the cyanation device amplified in equipment used in the present invention;
Fig. 4 is the structural representation of the even gas distribution device in the cyanation device amplified.
Embodiment:
The material used 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: during initial start-up, and 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, set up at 5 ends of cyanation device 3 → knockout tower → motoritis circulation line 11 → cyanation device 3 between circulation; When in cyanation device, temperature reaches 100 DEG C, gaseous ammonia after being compressed by ammonia compressor 1, in the pipe core that ammonia pipeline 10 enters into cyanation device 3, gaseous ammonia enters into backward upper flowing bottom cyanation device from the top of pipe core, it becomes several tiny bubble or air-flows behind several holes of umbrella even gas distribution device, adjustment gaseous ammonia flow, and increase to rated value 3300m gradually
3/ h;
Along with the rising of cyanation actuator temperature, rise gas plate liquid level in knockout tower 5 and formed, the material that knockout tower rises on gas plate turns back to cyanation device as thinner; When the temperature out that cyanation device top leads to knockout tower is 250 DEG C, 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, illustrate that the adiponitrile in cyanation device is almost all vaporized, now in cyanation device, add melting hexanodioic acid, enter into bottom cyanation device by the melting hexanodioic acid of hexanodioic acid basin 2, diluted by the thinner rising gas plate from knockout tower, the inlet amount of melting hexanodioic acid is brought up to rated value 2400kg/h gradually; Meanwhile, in cyanation device, phosphoric acid is added by diluent line 14; Now, to stop at the bottom of cyanation device → knockout tower → motoritis circulation line → cyanation device between circulation;
Catalyzer phosphoric acid volume pump 7 in phosphoric acid storage tank 8 quantitatively joins in line mixer 4 that thinner pipeline is installed, with mixing diluents; The weight ratio of hexanodioic acid and phosphoric acid add-on is 1000: 1.8;
After hexanodioic acid and gaseous ammonia carry out 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, enter bottom knockout tower through the outlet of cyanation device reacting rear material and pipeline and be separated, gas phase rises to each layer column plate and continues to be separated, then from the light fraction outlet energy extraction adiponitrile product on knockout tower top, rise gas plate extraction thinner, thinner enters in line mixer 4 through thinner pipeline 14, with the catalyzer phosphoric acid entered in line mixer mixes 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; Liquid phase falls at the bottom of tower, delivers to scraper-type vaporizer 9 and reclaims adiponitrile and intermediate product, and waste material then enters outside three wastes system; The heavy constituent carrying out autospasy tailing column 6 by adiponitrile, intermediate product (ammonium cyanovalerate, cyanovaleramide, hexanediamide, adipimide) and not easily volatility product form, interval enters bottom knockout tower, deliver to scraper-type vaporizer with the liquid phase reaction resultant fallen at the bottom of tower, reclaim adiponitrile and intermediate product.
See figures.1.and.2, the equipment used 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 top, hexanodioic acid basin 2 has pipeline to be connected with the hexanodioic acid import of cyanation device 3 housing bottom, reacting rear material outlet in the middle part of cyanation device has pipeline to be connected with the material inlet 5-2 that the tower body risen in knockout tower 5 below gas plate is arranged, knockout tower 5 comprises tower body 5-5, heavy constituent material 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, gas plate 5-3 is risen in tower body, rise in the tower body above gas plate and have column plate 5-4, rising the reaction product entrance 5-9 that the tower body below gas plate is arranged has pipeline to be connected with de-tailing column 6, heavy constituent material outlet 5-1 bottom knockout tower has pipeline to be connected with scraper-type vaporizer 9 entrance, heavy constituent material outlet bottom knockout tower and the pipeline between scraper-type evaporator inlet are also connected with motoritis circulating line 11, the other end of motoritis circulating line is connected with the bottom of cyanation device, 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, outlet bottom line mixer has pipeline to be connected with the thinner import bottom cyanation device, 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, pipe core 3-2 is had in housing, pipe core top is gas material import, bottom is gas material outlet, material outlet 3-3 after housing central section responds, hexanodioic acid import 3-4 and thinner import 3-11 are arranged at the bottom of housing, upper tubesheet 3-5 and lower tubesheet 3-6 is had in the housing of reacting rear material outlet below, on, tubulation 3-7 is connected with between lower tubesheet, pipe core is from upper, pass through in lower tubesheet, pipe core above upper tubesheet there is expansion joint 3-8, pipe core above expansion joint there is pod 3-9, the even gas distribution device 3-10 of umbrella is set up in the bottom of pipe core, the central authorities of even gas distribution device are provided with the opening passed through for pipe core, even gas distribution device surrounding is fixed on housing, even gas distribution device has several holes 3-12, the total sectional area in several holes is greater than the sectional area of pipe core.
Claims (3)
1. produce a method for adiponitrile with hexanodioic acid, it is characterized in that: the material used and the weight ratio of material are: melting hexanodioic acid: ammonia: phosphoric acid: thinner=1: 1.5: 0.003: 2.2;
Concrete production method is: during initial start-up, and 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, set up cyanation device (3) → knockout tower (5) end → motoritis circulation line (11) → cyanation device (3) between circulation; When 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 backward upper flowing bottom cyanation device from the top of pipe core, it becomes several tiny bubble or air-flows behind several holes of umbrella even gas distribution device, adjustment gaseous ammonia flow, and increase to rated value 3300m gradually
3/ h;
Along with the rising of cyanation actuator temperature, rise gas plate liquid level in knockout tower (5) and formed, the material that knockout tower rises on gas plate turns back to cyanation device as thinner; When the temperature out that cyanation device top leads to knockout tower is 250 DEG C, 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, illustrate that the adiponitrile in cyanation device is almost all vaporized, now in cyanation device, add melting hexanodioic acid, the melting hexanodioic acid come by hexanodioic acid basin (2) enters into bottom cyanation device, diluted by the thinner rising gas plate from knockout tower, the inlet amount of melting hexanodioic acid is brought up to rated value 2400kg/h gradually; Meanwhile, in cyanation device, phosphoric acid is added by diluent line (14); Now, to stop at the bottom of cyanation device → knockout tower → motoritis circulation line → cyanation device between circulation;
Catalyzer phosphoric acid volume pump (7) in phosphoric acid storage tank (8) quantitatively joins in line mixer (4) that thinner pipeline is installed, with mixing diluents; The weight ratio of hexanodioic acid and phosphoric acid add-on is 1000: 1.8;
After hexanodioic acid and gaseous ammonia carry out 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, enter bottom knockout tower through the outlet of cyanation device reacting rear material and pipeline and be separated, gas phase rises to each layer column plate and continues to be separated, then from the light fraction outlet energy extraction adiponitrile product on knockout tower top, rise gas plate extraction thinner, thinner enters in line mixer (4) through thinner pipeline (14), mix with the catalyzer phosphoric acid entered 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; Liquid phase falls at the bottom of tower, and deliver to scraper-type vaporizer (9) and reclaim adiponitrile and intermediate product, waste material then enters outside three wastes system; The heavy constituent carrying out autospasy tailing column (6) by adiponitrile, intermediate product and not easily volatility product form, interval enters bottom knockout tower, delivers to scraper-type vaporizer with the liquid phase reaction resultant fallen at the bottom of tower, reclaims adiponitrile and intermediate product.
2. with the equipment that hexanodioic acid production 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, reacting rear material outlet in the middle part of cyanation device has pipeline to be connected with the material inlet (5-2) that the tower body risen in knockout tower (5) below gas plate is arranged, knockout tower (5) comprises tower body (5-5), heavy constituent material 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, gas plate (5-3) is risen in tower body, rise in the tower body above gas plate and have column plate (5-4), rising the reaction product entrance (5-9) that the tower body below gas plate is arranged has pipeline to be connected with de-tailing column (6), heavy constituent material outlet (5-1) bottom knockout tower has pipeline to be connected with scraper-type vaporizer (9) entrance, heavy constituent material outlet bottom knockout tower and the pipeline between scraper-type evaporator inlet are also connected with motoritis circulating line (11), the other end of motoritis circulating line is connected with the bottom of cyanation device, 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, outlet bottom line mixer has pipeline to be connected with the thinner import bottom cyanation device, 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 that hexanodioic acid production adiponitrile according to claim 2 uses, it is characterized in that: described cyanation device (3) comprises housing (3-1), pipe core (3-2) is had in housing, pipe core top is gas material import, bottom is gas material outlet, material outlet (3-3) after housing central section responds, hexanodioic acid import (3-4) and thinner import (3-11) are arranged at the bottom of housing, upper tubesheet (3-5) and lower tubesheet (3-6) is had in the housing of reacting rear material outlet below, on, tubulation (3-7) is connected with between lower tubesheet, pipe core is from upper, pass through in lower tubesheet, pipe core above upper tubesheet there is expansion joint (3-8), pipe core above expansion joint there is pod (3-9), the even gas distribution device (3-10) of umbrella is set up in the bottom of pipe core, the central authorities of even gas distribution device are provided with the opening passed through for pipe core, even gas distribution device surrounding is fixed on housing, even gas distribution device has several holes (3-12), the total sectional area in several holes is greater than the sectional area of pipe core.
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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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|---|---|---|---|
| CN201210577924.9A CN103896805B (en) | 2012-12-27 | 2012-12-27 | Method and equipment for production of adiponitrile from adipic acid |
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| CN103896805B true CN103896805B (en) | 2015-04-15 |
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|---|---|---|---|---|
| CN106146345B (en) * | 2015-04-17 | 2018-05-04 | 中国石油天然气股份有限公司 | Method for producing adiponitrile by adipic acid liquid phase method |
| 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 |
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| 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 |
| 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 |
| 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 |
| 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 |
| CN111056972B (en) * | 2019-12-16 | 2021-06-08 | 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 |
| CN115814713A (en) * | 2021-09-17 | 2023-03-21 | 中国石油化工股份有限公司 | System and method for preparing adiponitrile from adipic acid |
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