CN103936595A - Refining method of crude hexamethylenediamine - Google Patents
Refining method of crude hexamethylenediamine Download PDFInfo
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Abstract
The invention provides a refining method of crude hexamethylenediamine. The refining method is characterized in that eight rectifying columns are utilized for separating a crude hexamethylenediamine mixture containing ETOH, H2O, NaOH, HMI, DCH, AMCPA, gamma-AP, Propylamine, ACN, N-ETHMD and BHT, and thus the purity of hexamethylenediamine can reach more than 99.99%.
Description
Technical field
The invention belongs to Chemicals purification technique field, relate in particular to a kind of process for purification of thick hexanediamine.
Background technology
Hexanediamine is a kind of important chemical intermediate, as the monomer of polymeric amide or as the intermediate of synthesizing isocyanate compound, has excellent thermostability, processibility, mechanicalness and chemical-resistant for the manufacture of polymkeric substance.
As everyone knows, under the existence of the catalyzer such as nickel, cobalt, rhodium or ruthenium, continuous hydrogenation of adiponitrile becomes the intermediate hexanediamine (HMD) of nylon 66.But in continuous hydrogenation process, can produce a series of by product as HMI (vulkacit H), DCH (diamines basic ring hexane), AMCPA (amine methylcyclopentane), γ-AP (α-amino isopropyl alcohol), Propylamine (propylamine), ACN (aminoacetonitriles), N-ETHMD (n-ethylcyclohexane diamines, is abbreviated as N-ET), BHT (two-hexanaphthene triamine) etc.Wherein HMI, DCH, AMCPA etc. are more difficult separates with HMD, also has reaction solvent ETOH and NaOH solution in additionally mixed thing.The existence of above-mentioned substance can affect the quality of the finished product nylon 66, as quality of colour.
Therefore, the content of above-mentioned impurity in HMD must drop to the remaining level of ppm level.
Summary of the invention
The problem to be solved in the present invention is for the impurity existing in HMD, and a kind of process for purification of thick hexanediamine is provided.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A process for purification for thick hexanediamine, for the refining thick hexanediamine that comprises following component, ETOH, H
2o, NaOH, HMI, DCH, AMCPA, γ-AP, Propylamine, ACN, N-ETHMD, BHT and HMD.
Further, the method is for separating of containing ETOH:5～25% (mass content, lower same); H
2o:5～15%; NaOH:0.2～0.5%; HMI:0.1～0.5%; DCH:0.1～1%; AMCPA:0.1～0.3%; γ-AP:0.1～0.3%; Propylamine:0.1～0.3%; ACN:0.1～1%; N-ETHMD:0.1～0.3%; BHT:0.1～0.3%; The thick hexanediamine of HMD:50～85%.
This process for purification adopts the method for 8 tower continuous rectifications, isolates light, heavy constituent and impurity wherein, makes product purity reach 99.99%; Wherein, ETOH and part H
2o is from 1
#tower top is separated, remainder H
2o is from 2
#tower top is separated, and NaOH and BHT are from 3
#at the bottom of tower, separate, HMI, DCH, AMCPA, γ-AP, Propylamine is from 4
#with 6
#tower top is separated, and ACN and N-ETHMD are from 5
#at the bottom of tower, separate, the finished product HMD is from 5
#overhead extraction, 7
#with 8
#tower reclaims remaining HMD.
Specifically comprise the steps:
(1) thick hexanediamine is delivered to 1
#in tower, ETOH and part H
2o separates from its tower top, and at the bottom of tower, liquid sends into 2
#tower;
(2) H of remainder
2o is from 2
#column overhead separates, and at the bottom of tower, liquid sends into 3
#tower;
(3) heavy constituent NaOH and BHT are from being rich in 3 of tar
#at the bottom of tower tower, in liquid, separate, send into 8
#tower, the component of enrichment HMD is from 3
#column overhead separates and sends into 6
#tower;
(4) light constituent HMI, DCH is from 6
#column overhead separates and with 8
#tower materials at bottom of tower transmitting system together, further the component of enrichment HMD is from 6
#at the bottom of tower tower, separate and send into 4
#tower;
(5) light constituent HMI, DCH, AMCPA, γ-AP, Propylamine further separates with HMD, from 4
#column overhead separates and sends into 6
#tower, further the component of enrichment HMD is from 4
#at the bottom of tower tower, separate and send into 5
#tower;
(6) content reaches 99.99% HMD from 5
#the extraction of column overhead side line, 5
#column overhead light constituent sends into 4
#tower, heavy constituent ACN at the bottom of tower, N-ETHMD sends into 7
#tower;
(7) 7
#column overhead reclaims after HMD, is delivered to 4
#in tower, process, at the bottom of tower, component transports to 8 again
#tower;
(8) 8
#overhead product returns to 1
#tower is processed and is reclaimed HMD, does not discharge end liquid at the bottom of tower.
Preferably, 1
#tower is packing tower, and form of bio-carrier is BX filler, and theoretical plate number is 5～30, tower top pressure 770～900mmHgA, and 65～100 DEG C of tower top temperatures, reflux ratio is 0.2～10.
Preferably, 2
#tower is sieve plate tray column, and the percentage of open area of sieve plate is 6%-20%, and theoretical plate number is 5～35,20～80 DEG C of tower top temperatures, and tower top pressure 50～120mmHgA, reflux ratio is 0.5～20.
Preferably, 3
#tower is sieve plate tray column, and the percentage of open area of sieve plate is 6%-20%, and theoretical plate number is 1～5,100～160 DEG C of tower top temperatures, and tower top pressure 60～130mmHgA, reflux ratio is 0.1～10.
Preferably, 4
#tower is sieve plate tray column, and the percentage of open area of sieve plate is 6%-20%, and theoretical plate number is 10～50,60～120 DEG C of tower top temperatures, and tower top pressure 10～50mmHgA, reflux ratio is 5～30.
Preferably, 5
#tower is sieve plate tray column, and the percentage of open area of sieve plate is 6%-20%, and theoretical plate number is 5～40,80～120 DEG C of tower top temperatures, and tower top pressure 10～50mmHgA, reflux ratio is 10～50.
Preferably, 6
#tower is packing tower, and form of bio-carrier is BX filler, and theoretical plate number is 6～35,70～120 DEG C of tower top temperatures, and tower top pressure 10～50mmHgA, reflux ratio is 10～300.
Preferably, 7
#tower is sieve plate tray column, and the percentage of open area of sieve plate is 6%-20%, and theoretical plate number is 5～60,80～130 DEG C of tower top temperatures, and tower top pressure 10～40mmHgA, reflux ratio is 0.2～10.
Preferably, 8
#tower is sieve plate tray column, and the percentage of open area of sieve plate is 6%-20%, and theoretical plate number is 5～50,90～130 DEG C of tower top temperatures, and tower top pressure 10～70mmHgA, reflux ratio is 1～50.
Preferably, 2～8
#tower adopts the mode of rectification under vacuum, and the operating temperature of 8 towers is 45～210 DEG C.
Preferably, 1
#the opening for feed of tower is 10th～25 blocks of theoretical trays; 2
#the opening for feed of tower is 15th～30 blocks of theoretical trays; 3
#the opening for feed of tower is 1st～4 blocks of theoretical trays; 4
#the opening for feed of tower is 10th～30 blocks of theoretical trays; 5
#the opening for feed of tower is 15th～30 blocks of theoretical trays; 6
#the opening for feed of tower is 15th～30 blocks of theoretical trays; 7
#the opening for feed of tower is 15th～50 blocks of theoretical trays; 8
#the opening for feed of tower is 15th～40 blocks of theoretical trays.
The advantage that the present invention has with positively effect is: thick hexanediamine is completed and separated by 8 rectifying tower, makes the purity of product HMD reach 99.99%.
Brief description of the drawings
Fig. 1 is process flow diagram.
T1 in figure, T2, T3, T4, T5, T6, T7, T8 is correspondence 1 respectively
#, 2
#, 3
#, 4
#,
5
#, 6
#, 7
#, 8
#tower.
Embodiment
For a better understanding of the present invention, below in conjunction with specific embodiments and the drawings, the present invention is conducted further description.
In following three embodiment, 1
#with 6
#tower is the packing tower that is filled with BX filler; 2
#, 3
#, 4
#, 5
#, 7
#, 8
#tower is sieve-tray tower, and sieve aperture rate is respectively 6%, 15%, 8%, 12%, 15% and 20%, and in rectifying, for fear of HMD crystallization and degraded, 2
#～8
#tower adopts the mode of underpressure distillation to carry out, and 1
#tower adopts atmospheric distillation mode to carry out, and must ensure that operating between 45～210 DEG C of whole rectifying carry out.
Embodiment 1:
Be ETOH:20～25% (mass content, lower same) by feed composition; H
2o:5～10%; NaOH:0.2～0.5%; HMI:0.1～0.5%; DCH:0.1～0.5%; AMCPA:0.1～0.3%; γ-AP:0.1～0.3%; Propylamine:0.1～0.3%; ACN:0.4～0.8%; N-ETHMD:0.1～0.3%; BHT:0.1～0.3%; The material of HMD:70～75% carries out rectifying separation.
1
#tower is from charging between the 10th theoretical stage, control tower pressure on top surface 900mmHgA, 65 DEG C of tower top temperatures, reflux ratio is 0.2, in overhead extraction material containing ETOH:90%, H
2o:10%, contains HMD:84.5%, H in extraction material at the bottom of tower
2o:14.5%, all the other account for 1%, and the ETOH of extraction goes recycle in continuous hydrogenation reactor.The bottomsstream is by being pumped into 2
#the 17th theoretical stage of tower; 2
#20 DEG C of column overhead temperature, under tower top pressure 120mmHgA, reflux ratio is 0.5, contains H in overhead extraction material
2o:99%, HMI:0.7%, HMD:0.15%, all the other account for 0.15%, and overhead fraction is delivered to waste water pretreatment system after extracting out and is processed, and contains HMD:96%, DCH:1.5%, BHT:1.5%, all the other high boiling material: 1% at the bottom of tower in extraction material.The bottomsstream is by being pumped into 3
#the 2nd theoretical stage of tower;
3
#100 DEG C of tower top temperatures, tower top pressure 130mmHgA, reflux ratio is 0.1, contains DCH:0.4%, HMD:98.9% in overhead extraction material, all the other account for 0.7%, at the bottom of tower, in extraction material, contain HMD:91.8%, N-ET:1.5%, BHT:5.7%, all the other high boiling material: 1%, overhead product is by being pumped into 6
#the 25th theoretical stage of tower, at the bottom of tower, discharging tar heavy oil goes out after residue through separating centrifuge sub-argument, enters 8
#the 30th theoretical stage of tower;
6
#column overhead temperature 70 C, tower top pressure 50mmHgA, reflux ratio is 10, in overhead extraction material containing DCH:13.5%, HMD:73.2%, N-ET:13.3% with 8
#materials at bottom of tower is transmitting system together; At the bottom of tower, in extraction material, contain DCH:0.5%, HMD:98.8%, N-ET:0.7%, the bottomsstream sends into 4 through charging surge tank
#the 18th theoretical stage of tower;
4
#column overhead temperature 60 C, tower top pressure 50mmHgA, reflux ratio is 5, contains DCH:1% in overhead extraction material, HMD:98.8%, all the other: 0.2%, at the bottom of tower, in extraction material, contain HMD:99%, N-ET:0.7%, all the other account for 0.3%, and the bottomsstream is by being pumped into 5
#the 17th theoretical stage of tower, overhead product enters 6
#tower;
5
#80 DEG C of column overhead temperature, tower top pressure 50mmHgA, reflux ratio is 10, in overhead extraction material, contain HMD:99.6%, all the other: 0.4%, at the bottom of tower, in extraction material, contain HMD:98.5%, N-ET:0.8%, BHT:0.5%, all the other account for 0.2%, and the HMD of product 99.6% enters products pot by the extraction of tower top side line.Overhead product is by being pumped into 4
#tower, the bottomsstream enters 7
#the 40th theoretical stage of tower;
7
#80 DEG C of column overhead temperature, tower top pressure 40mmHgA, reflux ratio is 0.2, contains DCH:0.3% in overhead extraction material, HMD:99.0%, N-ET:0.5%, all the other: 0.2%, at the bottom of tower, in extraction material, contain HMD:68%, N-ET:11%, BHT:17%, other high boiling material 4%.Overhead product is by being pumped into 4
#tower, the bottomsstream enters 8
#tower;
8
#90 DEG C of column overhead temperature, tower top pressure 70mmHgA, reflux ratio is 1, in overhead extraction material, containing HMD:98.8%, N-ET:1.2%, returns to 1
#tower is processed and is reclaimed hexanediamine; At the bottom of tower, in extraction material, contain HMD:15%, N-ET:25.6%, BHT:46.3%, NaOH:6.2%, other high boiling material 6.9%, do not discharge end liquid.
Embodiment 2:
Be ETOH:20～25% (mass content, lower same) by feed composition; H
2o:5～10%; NaOH:0.2～0.5%; HMI:0.1～0.5%; DCH:0.1～0.5%; AMCPA:0.1～0.3%; γ-AP:0.1～0.3%; Propylamine:0.1～0.3%; ACN:0.4～0.8%; N-ETHMD:0.1～0.3%; BHT:0.1～0.3%; The material of HMD:70～75% carries out rectifying separation.
1
#tower is from charging between the 10th theoretical stage, control tower pressure on top surface, 650mmHgA, 100 DEG C of tower top temperatures, reflux ratio is 5, in overhead extraction material containing ETOH:88%, H
2o:12%, contains HMD:85.5%, H in extraction material at the bottom of tower
2o:14%, all the other account for 0.5%.The bottomsstream is by being pumped into 2
#the 17th theoretical stage of tower;
2
#80 DEG C of column overhead temperature, tower top pressure 50mmHgA, reflux ratio is 10, contains H2O:99.5% in overhead extraction material, HMI:0.3%, HMD:0.1%, all the other account for 0.1%, contain HMD:97.9% at the bottom of tower in extraction material, DCH:0.3%, BHT:0.9%, all the other high boiling material: 0.9%.The bottomsstream is by being pumped into 3
#the 3rd theoretical stage of tower;
3
#160 DEG C of tower top temperatures, tower top pressure 60mmHgA, reflux ratio is 5, contains DCH:0.3% in overhead extraction material, HMD:99.1%, all the other account for 0.6%, contain HMD:90.4% at the bottom of tower in extraction material, N-ET:0.9%, BHT:5.9%, all the other high boiling material: 2.8%.Overhead product is by being pumped into 6
#the 30th theoretical stage of tower, the bottomsstream enters 8
#the 15th theoretical stage of tower;
6
#120 DEG C of column overhead temperature, tower top pressure 10mmHgA, reflux ratio is 150, in overhead extraction material containing DCH:14.3%, HMD:72.3%, N-ET:13.4% with 8
#materials at bottom of tower is transmitting system together; , at the bottom of tower, in extraction material, contain DCH:0.2%, HMD:99.3%, N-ET:0.5%, the bottomsstream is by being pumped into 4
#the 26th theoretical stage of tower;
4
#120 DEG C of column overhead temperature, tower top pressure 10mmHgA, reflux ratio is 20, in overhead extraction material, containing DCH:1.6%, HMD:98.4%, contains HMD:99.5% in extraction material at the bottom of tower, N-ET:0.4%, all the other account for 0.1%, and the bottomsstream is by being pumped into 5
#the 15th theoretical stage of tower, overhead product enters 6
#tower;
5
#120 DEG C of column overhead temperature, tower top pressure 10mmHgA, reflux ratio is 30, in overhead extraction material, contain HMD:99.8%, all the other: 0.2%, at the bottom of tower, in extraction material, contain HMD:97.5%, N-ET:2.2%, BHT:0.2%, all the other account for 0.1%, and the HMD of product 99.8% enters products pot by the extraction of tower top side line.Overhead product is by being pumped into 4
#tower, the bottomsstream enters 7
#the 50th theoretical stage of tower;
7
#130 DEG C of column overhead temperature, tower top pressure 10mmHgA, reflux ratio is 5, contains DCH:0.1% in overhead extraction material, HMD:99.1%, N-ET:0.5%, all the other: 0.3%, at the bottom of tower, in extraction material, contain HMD:67.2%, N-ET:10.9%, BHT:16.2%, other high boiling material 5.7%.Overhead product is by being pumped into 4
#tower, the bottomsstream enters 8
#tower;
8
#130 DEG C of column overhead temperature, tower top pressure 10mmHgA, reflux ratio is 25, contains HMD:98.8% in overhead extraction material, N-ET:1.2%, contains HMD:7.1%, N-ET:24.9% in extraction material at the bottom of tower, BHT:47.2%, NaOH:7.2%, other high boiling material 13.6%.
Embodiment 3:
Be ETOH:20～25% (mass content, lower same) by feed composition; H
2o:5～10%; NaOH:0.2～0.5%; HMI:0.1～0.5%; DCH:0.1～0.5%; AMCPA:0.1～0.3%; γ-AP:0.1～0.3%; Propylamine:0.1～0.3%; ACN:0.4～0.8%; N-ETHMD:0.1～0.3%; BHT:0.1～0.3%; The material of HMD:70～75% carries out rectifying separation.
1
#tower is from charging between the 10th theoretical stage, control tower pressure on top surface, 760mmHgA, 85 DEG C of tower top temperatures, reflux ratio is 10, in overhead extraction material containing ETOH:90%, H
2o:10%, contains HMD:85%, H in extraction material at the bottom of tower
2o:14%, all the other account for 1%.The bottomsstream is by being pumped into 2
#the 17th theoretical stage of tower;
2
#column overhead temperature 60 C, tower top pressure 70mmHgA, reflux ratio is 20, contains H2O:99.8% in overhead extraction material, HMI:0.1%, HMD:0.1%1, contains HMD:98.8% in extraction material at the bottom of tower, DCH:0.2%, BHT:0.9%, all the other high boiling material: 0.1%.The bottomsstream is by being pumped into 3
#the 3rd theoretical stage of tower;
3
#120 DEG C of tower top temperatures, tower top pressure 100mmHgA, reflux ratio is 10, contains DCH:0.6% in overhead extraction material, HMD:99%, all the other account for 0.4%, contain HMD:91.5% at the bottom of tower in extraction material, N-ET:1.2%, BHT:6.2%, all the other high boiling material: 1.1%.Overhead product is by being pumped into 6
#the 30th theoretical stage of tower, the bottomsstream enters 8
#the 15th theoretical stage of tower;
6
#90 DEG C of column overhead temperature, tower top pressure 20mmHgA, reflux ratio is 300, in overhead extraction material containing DCH:16.6%, HMD:71.1%, N-ET:12.3% with 8
#materials at bottom of tower is transmitting system together; At the bottom of tower, in extraction material, contain DCH:0.1%, HMD:99.5%, N-ET:0.4%, the bottomsstream is by being pumped into 4
#the 10th theoretical stage of tower;
4
#90 DEG C of column overhead temperature, tower top pressure 30mmHgA, reflux ratio is 30, in overhead extraction material, containing DCH:1.8%, HMD:98.2%, contains HMD:99.6% in extraction material at the bottom of tower, N-ET:0.4%, the bottomsstream is by being pumped into 5
#the 20th theoretical stage of tower, overhead product enters 6
#tower;
5
#100 DEG C of column overhead temperature, tower top pressure 20mmHgA, reflux ratio is 50, in overhead extraction material, contain HMD:99.99%, all the other: 0.01%, at the bottom of tower, in extraction material, contain HMD:96.4%, N-ET:3.2%, BHT:0.3%, all the other account for 0.1%, and the HMD of product 99.99% enters products pot by the extraction of tower top side line.Overhead product is by being pumped into 4
#tower, the bottomsstream enters 7
#the 40th theoretical stage of tower;
7
#100 DEG C of column overhead temperature, tower top pressure 30mmHgA, reflux ratio is 10, contains DCH:0.5% in overhead extraction material, HMD:98.8%, N-ET:0.4%, all the other: 0.3%, at the bottom of tower, in extraction material, contain HMD:68%, N-ET:11%, BHT:17%, other high boiling material 4%.Overhead product is by being pumped into 4
#tower, the bottomsstream enters 8
#tower;
8
#100 DEG C of column overhead temperature, tower top pressure 50mmHgA, reflux ratio is 50, contains HMD:97.6% in overhead extraction material, N-ET:2.4%, contains HMD:5.1%, N-ET:28.2% in extraction material at the bottom of tower, BHT:48.9%, NaOH:7.5%, other high boiling material 10.3%.
Above embodiments of the invention are had been described in detail, but described content is only preferred embodiment of the present invention, can not be considered to for limiting practical range of the present invention.All equalization variation and improvement etc. of doing according to the scope of the invention, within all should still belonging to this patent covering scope.
Claims (10)
1. a process for purification for thick hexanediamine, is characterized in that: the component containing in thick hexanediamine comprises ETOH, H
2o, NaOH, HMI, DCH, AMCPA, γ-AP, Propylamine, ACN, N-ETHMD, BHT and HMD, adopt the method for 8 tower continuous rectifications, isolates light, heavy constituent and impurity wherein; Specifically comprise the steps:
(1) thick hexanediamine is delivered to 1
#in tower, ETOH and part H
2o separates from its tower top, and at the bottom of tower, liquid sends into 2
#tower;
(2) H of remainder
2o is from 2
#column overhead separates, and at the bottom of tower, liquid sends into 3
#tower;
(3) heavy constituent NaOH and BHT are from being rich in 3 of tar
#at the bottom of tower tower, in liquid, separate, send into 8
#tower, the component of enrichment HMD is from 3
#column overhead separates and sends into 6
#tower;
(4) light constituent HMI, DCH is from 6
#column overhead separates and with 8
#discharging transmitting system together at the bottom of tower tower, further the component of enrichment HMD is from 6
#at the bottom of tower tower, separate and send into 4
#tower;
(5) light constituent HMI, DCH, AMCPA, γ-AP, Propylamine further separates with HMD, from 4
#column overhead separates and sends into 6
#tower, further the component of enrichment HMD is from 4
#at the bottom of tower tower, separate and send into 5
#tower;
(6) content reaches 99.99% HMD from 5
#the extraction of column overhead side line, 5
#column overhead light constituent sends into 4
#tower, heavy constituent ACN at the bottom of tower, N-ETHMD sends into 7
#tower;
(7) 7
#column overhead reclaims after HMD, is delivered to 4
#in tower, process, at the bottom of tower, component transports to 8 again
#tower;
(8) 8
#overhead product returns to 1
#tower is processed and is reclaimed HMD, does not discharge end liquid at the bottom of tower.
2. the process for purification of thick hexanediamine according to claim 1, is characterized in that: 1
#tower is packing tower, and form of bio-carrier is BX filler, and theoretical plate number is 5～30, tower top pressure 770～900mmHgA, and 65～100 DEG C of tower top temperatures, reflux ratio is 0.2～10.
3. the process for purification of thick hexanediamine according to claim 1, is characterized in that: 2
#tower is sieve plate tray column, and the percentage of open area of sieve plate is 6%-20%, and theoretical plate number is 5～35,20～80 DEG C of tower top temperatures, and tower top pressure 50～120mmHgA, reflux ratio is 0.5～20.
4. the process for purification of thick hexanediamine according to claim 1, is characterized in that: 3
#tower is sieve plate tray column, and the percentage of open area of sieve plate is 6%-20%, and theoretical plate number is 1～5,100～160 DEG C of tower top temperatures, and tower top pressure 60～130mmHgA, reflux ratio is 0.1～10.
5. the process for purification of thick hexanediamine according to claim 1, is characterized in that: 4
#tower is sieve plate tray column, and the percentage of open area of sieve plate is 6%-20%, and theoretical plate number is 10～50,60～120 DEG C of tower top temperatures, and tower top pressure 10～50mmHgA, reflux ratio is 5～30.
6. the process for purification of thick hexanediamine according to claim 1, is characterized in that: 5
#tower is sieve plate tray column, and the percentage of open area of sieve plate is 6%-20%, and theoretical plate number is 5～40,80～120 DEG C of tower top temperatures, and tower top pressure 10～50mmHgA, reflux ratio is 10～50.
7. according to the process for purification of the arbitrary described thick hexanediamine of claim 1-6, it is characterized in that: 6
#tower is packing tower, and form of bio-carrier is BX filler, and theoretical plate number is 6～35,70～120 DEG C of tower top temperatures, and tower top pressure 10～50mmHgA, reflux ratio is 10～300.
8. the process for purification of thick hexanediamine according to claim 7, is characterized in that: 7
#tower is sieve plate tray column, and the percentage of open area of sieve plate is 6%-20%, and theoretical plate number is 5～60,80～130 DEG C of tower top temperatures, and tower top pressure 10～40mmHgA, reflux ratio is 0.2～10.
9. the process for purification of thick hexanediamine according to claim 8, is characterized in that: 8
#tower is sieve plate tray column, and the percentage of open area of sieve plate is 6%-20%, and theoretical plate number is 5～50,90～130 DEG C of tower top temperatures, and tower top pressure 10～70mmHgA, reflux ratio is 1～50.
10. the process for purification of thick hexanediamine according to claim 1, is characterized in that: 2～8
#tower adopts the mode of rectification under vacuum, and the operating temperature of 8 towers is 45～210 DEG C.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004080932A2 (en) * | 2003-03-07 | 2004-09-23 | Invista Technologies S.À.R.L. | Distillative method for separating hexamethylenediamine from a mixture comprising hexamethylenediamine, -aminocapronitrile and tetrahydroazepine |
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