CN108484442A - A kind of process for purification of adiponitrile - Google Patents
A kind of process for purification of adiponitrile Download PDFInfo
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- CN108484442A CN108484442A CN201810558872.8A CN201810558872A CN108484442A CN 108484442 A CN108484442 A CN 108484442A CN 201810558872 A CN201810558872 A CN 201810558872A CN 108484442 A CN108484442 A CN 108484442A
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- adiponitrile
- tower
- removing column
- weight
- light component
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/22—Preparation of carboxylic acid nitriles by reaction of ammonia with carboxylic acids with replacement of carboxyl groups by cyano groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of process for purification of adiponitrile, including the mixture containing adiponitrile is preheating to the 23rd layer, 25 layers or the 27th layer tower tray progress separating-purifying that lightness-removing column is sent into after 170 220 DEG C, and adiponitrile is collected in bottom of tower, and light component is discharged in tower top；Further control carries out separating-purifying to the adiponitrile temperature that bottom of tower is collected at 180 230 DEG C into the hypomere tower tray of weight-removing column, by adiponitrile of the discharge at the top of weight-removing column after refined, condensed device is condensed to being cooled to 30 50 DEG C in adiponitrile cooler again, is finally entered in storage tank.The present invention can reduce investment and the operating cost of equipment, reduce operation difficulty, improve the stability of production, extend the cycle of operation of equipment；The adiponitrile quality in refined raw postpartum has a degree of promotion simultaneously, can better meet the demand of downstream section production and promote the quality of final products.
Description
Technical field
The invention belongs to chemical fields, are related to a kind of process for purification of adiponitrile.
Background technology
Adiponitrile (ADN) alias Isosorbide-5-Nitrae-dicyanobutane, molecular formula are NC (CH3)4CN is a kind of colourless oil liquid,
Slightly smell, property are stablized.Mainly for the production of the intermediate diamines of Fypro, rubber accelerator and antirust agent.Oneself
Dintrile can generate hexamethylene diamine with hydrogen addition, and hexamethylene diamine, which is reacted with adipic acid under stringent material proportion, generates nylon66 fiber
Salt.Important intermediate of the adiponitrile as synthetic nylon 66 is main and most worthy the work that adiponitrile developed
Industry purposes.Research finds that hexamethylene diamine can synthesize 1, and hexamethylene-diisocyanate (HDI), this is the development of adiponitrile downstream product chain
Another important use；With rapid technological growth, adiponitrile is also gradual in the purposes of light industry, electronics and other organic synthesis fields
It is developed.
Include not only primary product adiponitrile in the product of industrially prepared ADN, also includes many by-products, how preferably
It is target that everybody studies always that purification ADN and method of purification, which are preferably applied in continuous industrialized production,.
Invention content
In view of this, the purpose of the present invention is to provide a kind of process for purification of adiponitrile.
In order to achieve the above objectives, the present invention provides the following technical solutions：
1. a kind of process for purification of adiponitrile, includes the following steps：
A. use adipic acid and ammonia that thick mixture of nitriles is made in thick nitrile reactor, after washing, filtering, decantation, drying,
It obtains containing the mixture based on adiponitrile；Containing based on δ-cyanopentanoic acid amine and imino group cyano pentamethylene in the mixture
Impurity, remaining all impurity content be less than 1%；It is sent into after this mixture for containing adiponitrile is preheating to 170-220 DEG C de-
Light the 23rd layer, 25 layers or the 27th layer tower tray of tower carries out separating-purifying, and adiponitrile is collected in bottom of tower, and light component is discharged in tower top；
B. the adiponitrile temperature control that bottom of tower is collected carries out separation into the hypomere tower tray of weight-removing column at 180-230 DEG C and carries
Pure, by adiponitrile of the discharge at the top of weight-removing column after refined, then condensed device is condensed to being cooled to 30-50 in adiponitrile cooler
DEG C, it finally enters in storage tank.
Further, the process for purification further includes the crystallization filtering of light component Central Asia cyanamide cyclopentane, tower top discharge
Light component steam dissolves heat preservation at 70-90 DEG C, by being pumped into the light component crystallizing tank for carrying blender, respectively with 33 DEG C
Recirculated water, 7 DEG C of chilled water and liquefied ammonia are passed through the inside and outside coil pipe in crystallizing tank and are cooled down, make be with imino group cyano pentamethylene
Main light component crystallization is precipitated, and residual filtrate is sent to filtrate tank.
Further, the temperature of lightness-removing column materials at bottom of tower carries out heat cycles with pump through reboiler, controls at 200-240 DEG C
Interior, tower bottom pressure is controlled in 5-20KPaA.
Further, adiponitrile content is 96-98% in the mixture, including δ-cyanopentanoic acid amine accounts for 1.0-2.0%, Asia
Cyanamide cyclopentane accounts for 0.2-1.0%, remaining δ-cyanopentanoic acid, 2- amyls -1- amino -5,6- trimethylenes pyrimidine and 2- amino
(3,4-5,6)-bis- front threes annulated pyridine is less than 1.0%.
Further, the lightness-removing column is decompression operation, and tower top operating pressure is 1-15KpaA, and the control of tower top operation temperature exists
145-175℃；Control can be kept completely separate out cyclopentanone in this operating condition, while make the content of ICCP in the heavy constituent of bottom of tower
Control is within 0.1%.
Further, hypomere tower tray described in step b is the 5th layer, the 7th layer and/or the 9th layer tower tray of weight-removing column.
Further, weight-removing column described in step b is decompression operation, and the control of tower top operating pressure is in 1-15KpaA, tower top behaviour
Make temperature control at 145-175 DEG C, control can ensure that the content of adiponitrile in tower top light component exists in this operating condition
99.5% or more.
Further, after being condensed material with pump by the light component being discharged at the top of weight-removing column, a part is through flowing back into weight-removing column
The 20th layer of tower tray, reflux ratio control between 1.6 to 2.7, another part is sent to adiponitrile storage tank, passes through this condensing reflux
The content of 2- amyls -1- amino -5,6- trimethylene pyrimidines in product can be reduced by 60% or more by method.
Further, the heavy constituent of weight-removing column bottom discharge carries out heat cycles with pump through reboiler, and temperature is controlled in 190-220
℃。
Further, the control of weight-removing column tower bottom pressure is in 2-20KpaA.
The beneficial effects of the present invention are：Compared with the purification process of traditional adiponitrile, the present invention can reduce equipment
Investment and operating cost reduce operation difficulty, improve the stability of production, extend the cycle of operation of equipment.Refined production simultaneously
Adiponitrile quality afterwards has a degree of promotion, can better meet the demand of downstream section production and promote final products
Quality.
Description of the drawings
In order to keep the purpose of the present invention, technical solution and advantageous effect clearer, the present invention provides following attached drawing and carries out
Explanation：
Fig. 1 is the adiponitrile refining system schematic diagram of the present invention；Wherein：1 lightness-removing column feed preheater, the charging of 2 lightness-removing columns
Tank, 3 lightness-removing columns, 4 lightness-removing column top return tanks, 5 lightness-removing column top condensers, 6 constant level tanks, 7 condenser lime set tanks, 8 light components
Surge tank, 9 light component crystallizers, 10 weight-removing columns, 11 weight-removing column top condensers, 12 vacuum separators, 13 adiponitrile coolers
Specific implementation mode
Below in conjunction with attached drawing, the preferred embodiment of the present invention is described in detail.It is not specified in embodiment specific
The experimental method of condition, usually according to conventional conditions or according to the manufacturer's recommendations.
A kind of adiponitrile refining system as shown in Figure 1, including it is lightness-removing column feed preheater 1, lightness-removing column head tank 2, de- light
Tower 3, lightness-removing column top return tank 4, lightness-removing column top condenser 5, constant level tank 6, condenser lime set tank 7, light component surge tank 8,
Light component crystallizer 9, weight-removing column 10, weight-removing column top condenser 11, vacuum separator 12, adiponitrile cooler 13；
Lightness-removing column feed preheater 1 is equipped with the entrance of adiponitrile combination mixture, and outlet is connected to de- by pipeline
The bottom of light tower head tank 2, lightness-removing column head tank 2 is equipped with the stage casing that pipeline is connected to lightness-removing column 3, and the tower top of lightness-removing column 3 passes through
Pipeline connects constant level tank 6 through lightness-removing column top condenser 5, and lightness-removing column top condenser 5 passes through condenser lime set tank 7, trap
It is connected with vacuum plant；One liquid outlet of constant level tank 6 is returned by lightness-removing column top return tank 4 is connected to lightness-removing column 3, another
Liquid outlet is connected to light component surge tank 8 by pipeline, and light component surge tank 8 is connected to light component crystallizer 9；
A part of adiponitrile that light component is sloughed in the bottom of lightness-removing column 3 is connected to the stage casing of weight-removing column 10 by pipeline, takes off
The tower top of weight tower 10 connects weight-removing column top condenser 11 by pipeline, and weight-removing column top condenser 11 is by vacuum separator 12 and very
Empty device connection, the discharge port of weight-removing column top 11 1 adiponitriles of condenser are connected to the epimere of weight-removing column 10 by back of pipeline, separately
The discharge port of one adiponitrile is connected to adiponitrile cooler 13 by pipeline；
Another part adiponitrile that light component is sloughed in the bottom of the lightness-removing column 3 is returned by reboiler 14 and is connected to lightness-removing column 3,
A part of heavy constituent in bottom of the weight-removing column 10 is returned by reboiler 15 is connected to weight-removing column, is heated through reboiler 15 with pump
Cycle, bottom another part heavy constituent of weight-removing column 10 connect back to the liter vapour plate of reaction workshop section multilayer knockout tower by pipeline.This
In embodiment, flow control valve is equipped between lightness-removing column head tank 2 and lightness-removing column 3.Lightness-removing column 3 and weight-removing column 10 respectively with boil again
It is equipped with flow control valve on the pipeline that device 14 and 15 connects.It is equipped with timer between the bottom and liter vapour plate of weight-removing column 10,
In 16 for pump.
A kind of refined method of 1 adiponitrile of embodiment
(1) light component is taken off
It is reacted in thick nitrile reactor with adipic acid and ammonia, thick nitrile product is made.Material is by washing, filtering, decantation, do
After dry equal operation, the thick mixture of nitriles based on adiponitrile is obtained.The thick mixture of nitriles being stored in adiponitrile storage tank contains oneself
Dintrile about 97.5% containing δ-cyanopentanoic acid amine is about 1.4%, imido- cyano pentamethylene about 0.4% and other δ-cyanogen
The various components such as base valeric acid, 2- amyl -1- amino -5,6- trimethylenes pyrimidine, 2- amino (3,4-5,6)-bis- front threes annulated pyridine are about
Account for 0.7%.The material is heated to 170-220 DEG C with pump through 1 lightness-removing column feed preheater, is sent in lightness-removing column head tank 2, then
The 23rd layer, 25 layers or the 27th layer tower tray for entering lightness-removing column by gravity, depending in the purity and tower top light component of bottom of tower adiponitrile oneself
The content of dintrile is adjusted, and minimum load is into 23 layers, and maximum load is into 27 layers.Dehydration adiponitrile flow into lightness-removing column is used
The steam flow of Flux Valve Control, feed preheater is adjusted by the drop temperature of dehydration adiponitrile.Preferably, feeding preheating
Temperature of charge after device 1 heats is controlled at 185-200 DEG C, to meet in the case where respective substance is formed into the Warm status of tower.
Lightness-removing column is decompression operation, is equipped with 44 layers of sieve plate, is controlled by the pressure-regulating valve with alarm for high voltage.Tower top operates
Pressure is 1-15KpaA, and tower top operation temperature is controlled at 145-175 DEG C.The distillate gone out from lightness-removing column top row, on lightness-removing column top
Condenser 5 condenses, and condensed temperature control is at 80-100 DEG C.Condensate liquid is collected in constant level tank 6.Overhead condenser is logical
Cross condenser lime set tank 7, trap is connected with vacuum plant.Preferably, tower top temperature control is at 150-165 DEG C, it is ensured that
The imino group cyano pentamethylene of 75% or more removing.
The temperature of materials at bottom of tower carries out heat cycles with pump through reboiler, controls within the scope of 200-240 DEG C.Into boiling again
The steam flow Flux Valve Control of device, to meet the required temperature of lightness-removing column.Tower bottom pressure is according to load and Ta Nei liquid
Position control is in 5-20KPaA.The adiponitrile for removing light component is sent to through flow control valve in weight-removing column in bottom of tower with pump.It is preferred that
, column bottom temperature controls within the scope of 215-230 DEG C, and to ensure that adiponitrile content is more than 98%, remaining light component total amount is less than
0.2%.
The 44th layer of tower tray that the condensate liquid in constant level tank flows back into lightness-removing column through a pump part is collected, flow is by perseverance
Determine the Liquid level of level tank, another part is sent with flow control to light component buffer reservoir.The finned tube of interior and
Chuck is passed through cooling water, may carry the volatile products into vacuum plant secretly with condensation.Two trap rotation behaviour in operation
Make, one cleaning of an operating.
(2) heavy constituent is taken off
This operation carries out in weight-removing column 10, mainly removes the recombination in adiponitrile based on δ-cyanopentanoic acid amine
Point, including a small amount of δ-cyanopentanoic acid, 2- amyl -1- amino -5,6- trimethylene pyrimidines and 2- amino (3,4-5,6)-bis- front threes
Annulated pyridine.Weight-removing column is equipped with 20 layers of sieve plate, is decompression operation.The adiponitrile for sloughing light component enters the 5th layer of weight-removing column, the 7th
Layer and the 9th layer of tower tray, feeding temperature are controlled at 180-230 DEG C.Preferably, it with the drop temperature of lightness-removing column, controls in 185-200
DEG C, to meet in the case where respective substance is formed into the Warm status of tower.
In 1-15KpaA, tower top operation temperature is controlled at 130-180 DEG C for the tower top operating pressure control of weight-removing column.Weight-removing column
The product adiponitrile of top discharge, by weight-removing column top condenser 11, at 60-80 DEG C, condenser is logical for condensed temperature control
Vacuum separator is crossed to connect with vacuum plant.A part is flowed back into the 20th layer of tower by the product adiponitrile condensed out with pump
Tower tray, regurgitant volume is by condenser Liquid level.Rest part is cooled with circulating water in adiponitrile cooler to 30-50 DEG C, is sent
Into product storage tank.Preferably, the control of tower top operation temperature can remove in component completely at this temperature at 145-175 DEG C
δ-cyanopentanoic acid amine.Preferably, at 145-175 DEG C of tower top temperature control tower top pressure in 1-12KpaA, it is ensured that tower
The content of adiponitrile in light component is pushed up 99.5% or more, while ensureing 2- amino in light component (3,4-5,6)-bis- trimethylene pyrroles
Pyridine content is within 0.13%.Preferably, it by the light component pump circulation being discharged at the top of weight-removing column, after material is condensed, will return
To weight-removing column regurgitant volume and overhead extraction amount Ratio control between 1.6 to 2.7, can will by the method for this condensing reflux
The content of 2- amyls -1- amino -5,6- trimethylene pyrimidines controls within 0.15% in product.
The heavy constituent at weight-removing column bottom carries out heat cycles with pump through reboiler.The drop temperature control of weight-removing column bottom heavy constituent
System is controlled at 190-220 DEG C by the quantity of steam that reboiler is passed through.Tower bottom pressure is according to load and the control of Ta Nei level conditions in 2-
20KPaA.The heavy constituent of bottom of tower is ceaselessly recycled in bottom of tower, and it is more to go back to thick nitrile reaction workshop section for intermittent discharge under the control of a timer
On the liter vapour plate of layer separation tower, by heavy constituent discharge system after detaching and evaporating recycling.
Embodiment 2
Presently preferred embodiment includes not only above-mentioned steps, further includes the crystallization filtering of ICCP, utilizes
The method for crystallizing filtering detaches the by-products such as the ICCP in light component, is intermittently operated.It collects in 8 light component surge tanks
Light component containing adiponitrile, ICCP and other volatile products is dissolved with steam and is kept the temperature, and is controlled at 70-90 DEG C.Then by pumping
It is sent in the light component crystallizing tank 9 with blender, is passed through in tank with 33 DEG C of recirculated water, 7 DEG C of chilled water and liquefied ammonia respectively
Inside and outside coil pipe cooled down, so that the light component based on ICCP is crystallized, after each section of cooling temperature is exchanged heat by respective media
Temperature controls.Speed of agitator need to be adjusted according to the crystallization situation in tank simultaneously in 150-250rpm, controls lump shaped crystalline object in tank.
Obtained after light component crystallisation by cooling suspension mixed solution temperature control at 0-20 DEG C, through tank bottom be pumped into filter
Filtering in device, filtrate, which is collected, to be sent after filtrate tanks, buffering heating to light component storage tank.The light components such as the ICCP in filter are brilliant
Body is kept crystal loose, is then discharged in the storage tank with blender and is collected with after being air-dried with pneumatic vibrator.
According to smart adiponitrile produced by the invention, product specification, which can reach and be not limited to Q/HFHG 007-2017 products, to be referred to
Target provides, and the rational design of technique and the reasonable selection of equipment also reduce operation and maintenance cost.
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (10)
1. a kind of process for purification of adiponitrile, which is characterized in that include the following steps：
A. it uses adipic acid and ammonia that thick mixture of nitriles is made in thick nitrile reactor, after washing, filtering, decantation, drying, obtains
Containing the mixture based on adiponitrile；Containing miscellaneous based on δ-cyanopentanoic acid amine and imino group cyano pentamethylene in the mixture
Matter, remaining all impurity content are less than 1%；It is sent into lightness-removing column after this mixture for containing adiponitrile is preheating to 170-220 DEG C
23rd layer, 25 layers or the 27th layer tower tray carries out separating-purifying, and adiponitrile is collected in bottom of tower, and light component is discharged in tower top；
B. the adiponitrile temperature that bottom of tower is collected controls the hypomere tower tray progress separating-purifying for entering weight-removing column at 180-230 DEG C, by
Adiponitrile after discharge is refined at the top of weight-removing column, then condensed device are condensed to being cooled to 30-50 DEG C in adiponitrile cooler, finally
Into in storage tank.
2. process for purification according to claim 1, which is characterized in that the process for purification further includes imino group in light component
The crystallization of cyano pentamethylene is filtered, and tower top is discharged light component steam and dissolves heat preservation at 70-90 DEG C, and blender is carried by being pumped into
Light component crystallizing tank in, respectively with 33 DEG C of recirculated water, 7 DEG C of chilled water and liquefied ammonia be passed through the inside and outside coil pipe in crystallizing tank into
Row cooling makes the light component based on imino group cyano pentamethylene crystallize and is precipitated, and residual filtrate is sent to filtrate tank.
3. process for purification according to claim 1, which is characterized in that the temperature of lightness-removing column materials at bottom of tower is pumped through reboiler
Heat cycles are carried out, are controlled in 200-240 DEG C, tower bottom pressure is controlled in 5-20KPaA.
4. according to claim 1-3 any one of them process for purification, which is characterized in that adiponitrile content is in the mixture
96-98%, including δ-cyanopentanoic acid amine accounts for 1.0-2.0%, imino group cyano pentamethylene accounts for 0.2-1.0%, remaining δ-cyano penta
Acid, 2- amyls -1- amino -5,6- trimethylenes pyrimidine and 2- amino (3,4-5,6)-bis- front threes annulated pyridine are less than 1.0%.
5. process for purification according to claim 4, which is characterized in that the lightness-removing column is decompression operation, tower top operation pressure
Power is 1-15KpaA, and tower top operation temperature is controlled at 145-175 DEG C.
6. process for purification according to claim 4, which is characterized in that hypomere tower tray described in step b is the 5 of weight-removing column
Layer, the 7th layer and/or the 9th layer of tower tray.
7. process for purification according to claim 4, which is characterized in that weight-removing column described in step b is decompression operation, tower top
Operating pressure control is controlled in 1-15KpaA, tower top operation temperature at 145-175 DEG C.
8. process for purification according to claim 4, which is characterized in that pumped object by the light component being discharged at the top of weight-removing column
After material condensation, a part of the 20th layer of tower tray through flowing back into weight-removing column, another part is sent to adiponitrile storage tank, and reflux ratio control exists
Between 1.6 to 2.7.
9. process for purification according to claim 4, which is characterized in that the heavy constituent of weight-removing column bottom discharge is pumped through reboiler
Heat cycles are carried out, temperature is controlled at 190-220 DEG C.
10. process for purification according to claim 4, which is characterized in that weight-removing column tower bottom pressure is controlled in 2-20KpaA.
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| CN201810558872.8A CN108484442A (en) | 2018-06-01 | 2018-06-01 | A kind of process for purification of adiponitrile |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111574400A (en) * | 2020-06-10 | 2020-08-25 | 江苏扬农化工集团有限公司 | Separation method of ammoniated and dehydrated product of caprolactam and synthesis method of hexamethylene diamine |
| CN112430196A (en) * | 2020-09-29 | 2021-03-02 | 瑞典国际化工技术有限公司 | Method and device for refining 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 |
| CN115023415A (en) * | 2020-01-31 | 2022-09-06 | 英威达纺织（英国）有限公司 | Reduction of impurity formation during product purification |
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| CN115023415A (en) * | 2020-01-31 | 2022-09-06 | 英威达纺织（英国）有限公司 | Reduction of impurity formation during product purification |
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| CN112430196A (en) * | 2020-09-29 | 2021-03-02 | 瑞典国际化工技术有限公司 | Method and device for refining 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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