CN104672052A - Refining method of impure dichloropropane - Google Patents
Refining method of impure dichloropropane Download PDFInfo
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- CN104672052A CN104672052A CN201510004499.8A CN201510004499A CN104672052A CN 104672052 A CN104672052 A CN 104672052A CN 201510004499 A CN201510004499 A CN 201510004499A CN 104672052 A CN104672052 A CN 104672052A
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- propylene dichloride
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Abstract
The invention provides a refining method of impure dichloropropane. Light components, heavy components and epoxy chloropropane of impure dichloropropane are separated by adopting a method of four-tower continuous rectification, and 1,2-dichloropropane in impure dichloropropane accounts for 50-90% of total weight. By utilizing the refining method, impurities of impure dichloropropane are separated through four-tower rectification, the purity of separated product 1,2-dichloropropane reaches 99.9%, and the purity of by-product epoxy chloropropane reaches 99.8%.
Description
Technical field
The invention belongs to Chemicals technical field of purification, especially relate to a kind of process for purification of impure propylene dichloride.
Background technology
Propylene dichloride is a kind of important chemical intermediate, for preparing paint, ink, thinner etc., is a kind of excellent organic solvent.Also can be used as the raw material producing other organic chlorides multiple.
As everyone knows, propylene dichloride is the by product that epoxy chloropropane and chlorohydrination production propylene oxide are prepared in propylene high-temperature chlorination; Also propylene and chlorine liquid phase low temperature chlorination technique direct production propylene dichloride product in propylene dichloride can be adopted.Usually, containing plurality of impurities in propylene dichloride raw material, as propionic aldehyde, acetone, 2-methyl-2-pentenal serving, epoxy chloropropane, 3-alkene-1-ketone, trichloropropane (containing isomer), 1-chloro-2-propanol, 2-chloro-1-propanol, chloropropane ether, water etc.In organic chlorides production technique, the existence of above-mentioned impurity can affect the quality of organic chlorides.
Therefore, need to reduce the content of above-mentioned impurity in propylene dichloride as much as possible.
Summary of the invention
The problem to be solved in the present invention is to provide a kind of process for purification of impure propylene dichloride, and the mode especially by 4 tower rectifying is refined propylene dichloride.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of process for purification of impure propylene dichloride, the method of 4 tower continuous rectifications is adopted to isolate light constituent, heavy constituent and epoxy chloropropane in described impure propylene dichloride, in described impure propylene dichloride 1,2-propylene dichloride accounts for the 50-90% of gross weight, and the method for described 4 tower continuous rectifications specifically comprises the following steps:
S01, impure propylene dichloride is delivered to 1
#in tower, light constituents whole in charging and a small amount of 1,2-propylene dichloride are from 1
#tower top separates, and liquid at the bottom of tower sends into 2
#tower;
S02, from 2
#column overhead separates 1,2-propylene dichloride, and its purity reaches 99.9%, and 2
#liquid at the bottom of the tower of tower sends into 3
#tower;
S03, from 3
#column overhead separates 1,2-a small amount of propylene dichloride of residue, and its purity is greater than 95%, and 3
#liquid at the bottom of the tower of tower sends into 4
#tower;
S04, from 4
#column overhead separates epoxy chloropropane, and its purity reaches 99.8%, from 4
#discharge heavy constituent and a small amount of residual epoxide chloropropane at the bottom of tower, deliver to incinerator.
Further, the material outlet place of each tower top of described 4 towers is connected with condenser, return tank and reflux pump in turn, and described reflux pump connects refluxing opening and extraction mouth, and described refluxing opening is connected to the top of corresponding tower body.
Further, described light constituent accounts for 1.6 ~ 18% of impure propylene dichloride gross weight, and described light constituent comprises propionic aldehyde, acetone and water.
Further, described heavy constituent accounts for 7.4 ~ 31% of impure propylene dichloride gross weight, and described heavy constituent comprises 2-methyl-2-pentenal serving, 3-alkene-1-ketone, trichloropropane, 1-chloro-2-propanol, 2-chloro-1-propanol, chloropropane ether; Described epoxy chloropropane accounts for 1 ~ 20% of impure propylene dichloride gross weight.
Further, described impure propylene dichloride comprises the following component of percentage: this propionic aldehyde: 1 ~ 10%; Acetone: 0.5 ~ 5%; 1,2-propylene dichloride: 50 ~ 90%; 2-methyl-2-pentenal serving: 0.5 ~ 5%; Epoxy chloropropane: 1 ~ 20%; 3-is alkene-1-ketone: 0.1 ~ 2%; Trichloropropane: 0.5 ~ 5%; 1-chloro-2-propanol: 0.2 ~ 3%; 2-chloro-1-propanol: 0.1 ~ 2%; Chloropropane ether: 1 ~ 10%; Water: 0.1 ~ 3%; Described trichloropropane also comprises its isomer.
Further, described 4 towers all adopt the mode of pressure-fired rectifying, and described pressure-fired refers to that working pressure is lower than 10KPa, and the operating temperature of described 4 towers is 40 ~ 200 DEG C.
Further, described 1
#tower is float valve tray column, and the percentage of open area of column plate is 6 ~ 20%, and theoretical plate number is 20 ~ 50 pieces, tower top temperature 40 ~ 90 DEG C, tower top pressure 101 ~ 110kPa, and reflux ratio is 5 ~ 20.
Further, described 2
#tower is float valve tray column, and the percentage of open area of column plate is 6 ~ 20%, and theoretical plate number is 15 ~ 50 pieces, tower top temperature 70 ~ 120 DEG C, tower top pressure 101 ~ 110kPa, and reflux ratio is 2 ~ 10.
Further, described 3
#tower is packing tower, and form of bio-carrier is Raschig ring filler, and theoretical plate number is 30 ~ 60 pieces, tower top temperature 70 ~ 120 DEG C, tower top pressure 101 ~ 110kPa, and reflux ratio is 10 ~ 40.
Further, described 4
#tower is packing tower, and form of bio-carrier is Raschig ring filler, and theoretical plate number is 20 ~ 50 pieces, tower top temperature 100 ~ 140 DEG C, tower top pressure 101 ~ 110kPa, and reflux ratio is 1 ~ 15.
Further, 1
#the opening for feed of tower is at 15th ~ 25 pieces of theoretical tray places; 2
#the opening for feed of tower is at 15th ~ 25 pieces of theoretical tray places; 3
#the opening for feed of tower is at 15th ~ 25 pieces of theoretical tray places; 4
#the opening for feed of tower is at 20th ~ 30 pieces of theoretical tray places.
The advantage that the present invention has and positively effect are: impure propylene dichloride has come magazins' layout by 4 tower rectifying, and the purity of isolated product 1,2-propylene dichloride all reaches 99.9%, and the purity of its byproduct epoxy chloropropane reaches 99.8%.
Accompanying drawing explanation
Fig. 1 is the 4 tower rectifying device structural representations of the present embodiment
In figure: E1, E2, E3, E4 are condenser, V1, V2, V3, V4 are return tank, and P2, P4, P6, P8 are reflux pump, and P1, P3, P5, P7 are transferpump, and T1 is 1
#tower, T2 is 2
#tower, T3 is 3
#tower, T4 is 4
#tower, 1 is 1
#material inlet, 2,3,4,5,6 are respectively extraction mouth.
Embodiment
As shown in Figure 1, the invention provides a kind of process for purification of impure propylene dichloride, the method of 4 tower continuous rectifications is adopted to isolate light constituent, heavy constituent and epoxy chloropropane in described impure propylene dichloride, described impure propylene dichloride comprises following component by weight percentage: 1 of 50-90%, 2-propylene dichloride, the light constituent of 1.6 ~ 18%, the heavy constituent of 7.4 ~ 31% and 1 ~ 20% epoxy chloropropane, the method for described 4 tower continuous rectifications specifically comprises the following steps:
S01, impure propylene dichloride is delivered to 1
#in tower, light constituents whole in charging and a small amount of 1,2-propylene dichloride are from 1
#tower top separates, through 1
#after overhead condenser E1 condensation, via 1
#tower return tank V1 is from flowing to 1
#tower reflux pump P2, pumping hole discharging small portion is from side direction extraction, and all extraction mouth extraction thus of the light constituent now in charging, most of discharging is back to 1 from refluxing opening
#tower top, liquid at the bottom of tower sends into 2
#tower;
S02, from 2
#column overhead separates 1,2-propylene dichloride, through 2
#after overhead condenser E2 condensation, via 2
#tower return tank V2 is from flowing to 2
#tower reflux pump P4, pumping hole discharging small portion is from the extraction of side direction extraction mouth, and 1,2-propylene dichloride purity of now extraction reaches 99.9%, and most of discharging is back to 2 from refluxing opening
#tower top, 2
#liquid at the bottom of the tower of tower sends into 3
#tower;
S03, from 3
#column overhead separates 1,2-a small amount of propylene dichloride of residue, through 3
#after overhead condenser E3 condensation, via 3
#tower return tank V3 is from flowing to 3
#tower reflux pump P6, pumping hole discharging small portion is from the extraction of side direction extraction mouth, and 1,2-propylene dichloride purity of now extraction is greater than 95%, and most of discharging is back to 3 from refluxing opening
#tower top, 3
#liquid at the bottom of the tower of tower sends into 4
#tower;
S04, from 4
#column overhead separates byproduct epoxy chloropropane, through 4
#after overhead condenser E4 condensation, via 4
#tower return tank V4 is from flowing to 4
#tower reflux pump P8, a pumping hole discharging part is from the extraction of side direction extraction mouth, and the epoxy chloropropane purity of now extraction reaches 99.8%, and rest part discharging is back to 4 from refluxing opening
#tower top, from 4
#discharge heavy constituent and a small amount of residual epoxide chloropropane at the bottom of tower, deliver to incinerator.
Described light constituent comprises the propionic aldehyde 1 ~ 10%, acetone 0.5 ~ 5% and the water 0.1 ~ 3% that compare by impure propylene dichloride gross weight score; Described heavy constituent comprises 2-methyl-2-pentenal serving 0.5 ~ 5%, 3-alkene-1-ketone 0.1 ~ 2%, trichloropropane 0.5 ~ 5%, 1-chloro-2-propanol 0.2 ~ 3%, 2-chloro-1-propanol 0.1 ~ 2%, chloropropane ether 1 ~ 10% by impure propylene dichloride gross weight score ratio; Described trichloropropane also comprises its isomer.
The invention provides four groups of embodiments, treat in embodiment 1-4 that each component in the impure propylene dichloride of rectifying is identical, all comprise following component by weight percentage: propionic aldehyde 3%, acetone 1%, 1,2-propylene dichloride 80%, 2-methyl-2-pentenal serving 0.5%, epoxy chloropropane 10%, 3-alkene-1-ketone 0.5%, trichloropropane 1%, 1-chloro-2-propanol 0.5%, 2-chloro-1-propanol 0.2%, chloropropane ether 3%, water 0.3%.Often to organize in embodiment 1
#tower and 2
#tower is bubble-cap tray column, and the percentage of open area of column plate is respectively 8% and 15%; 3
#tower and 4
#tower is the packing tower being filled with Raschig ring filler, in rectifying, and 1
#~ 4
#tower all adopts pressure-fired rectifying mode to carry out, and must ensure that operating between 40 ~ 200 DEG C of whole rectifying is carried out.
In four embodiments 2
#the overhead fraction that tower is extracted out can as the raw material of organic chlorides.
Embodiment 1
In the present embodiment 1 working conditions of 4 towers and rectifying result as shown in table 1:
The working conditions of 4 towers and rectifying result in table 1 embodiment 1
Embodiment 2
In the present embodiment 2 working conditions of 4 towers and rectifying result as shown in table 2:
The working conditions of 4 towers and rectifying result in table 2 embodiment 2
Embodiment 3
In the present embodiment 3 working conditions of 4 towers and rectifying result as shown in table 3:
The working conditions of 4 towers and rectifying result in table 3 embodiment 3
Embodiment 4
In the present embodiment 4 working conditions of 4 towers and rectifying result as shown in table 3:
The working conditions of 4 towers and rectifying result in table 4 embodiment 4
Data results as can be seen from above-mentioned table 1-4: according to the difference of constitutive property each in impure propylene dichloride, 4 tower continuous rectification methods are adopted to impure propylene dichloride, when selecting suitable tower type, tower top temperature, tower top pressure, reflux ratio and feed entrance point, the object of extraction light constituent, propylene dichloride product, epoxy chloropropane byproduct and heavy constituent can be realized, and isolated product 1, the purity of 2-propylene dichloride all reaches 99.9%, and the purity of its byproduct epoxy chloropropane reaches 99.8%.It is a kind of process for purification obtaining high yield, high purity propylene dichloride.
Above one embodiment of the present of invention have been described in detail, but described content being only preferred embodiment of the present invention, can not being considered to for limiting practical range of the present invention.All equalizations done according to the present patent application scope change and improve, and all should still belong within patent covering scope of the present invention.
Claims (10)
1. the process for purification of an impure propylene dichloride, it is characterized in that: adopt the method for 4 tower continuous rectifications to isolate light constituent, heavy constituent and epoxy chloropropane in described impure propylene dichloride, in described impure propylene dichloride 1,2-propylene dichloride accounts for 50 ~ 90% of gross weight, and the method for described 4 tower continuous rectifications specifically comprises the following steps:
S01, impure propylene dichloride is delivered to 1
#in tower, light constituents whole in charging and a small amount of 1,2-propylene dichloride are from 1
#tower top separates, and liquid at the bottom of tower sends into 2
#tower;
S02, from 2
#column overhead separates 1,2-propylene dichloride, and 2
#liquid at the bottom of the tower of tower sends into 3
#tower;
S03, from 3
#column overhead separates 1,2-a small amount of propylene dichloride of residue, and 3
#liquid at the bottom of the tower of tower sends into 4
#tower;
S04, from 4
#column overhead separates epoxy chloropropane, from 4
#discharge heavy constituent and a small amount of residual epoxide chloropropane at the bottom of tower, deliver to incinerator.
2. the process for purification of a kind of impure propylene dichloride according to claim 1, it is characterized in that: the material outlet place of each tower top of described 4 towers is connected with condenser, return tank and reflux pump in turn, described reflux pump connects refluxing opening and extraction mouth, and described refluxing opening is connected to the top of corresponding tower body.
3. the process for purification of a kind of impure propylene dichloride according to claim 1, is characterized in that: described light constituent accounts for 1.6 ~ 18% of impure propylene dichloride gross weight, and described light constituent comprises propionic aldehyde, acetone and water.
4. the process for purification of a kind of impure propylene dichloride according to claim 1, it is characterized in that: described heavy constituent accounts for 2.4 ~ 22% of impure propylene dichloride gross weight, described heavy constituent comprises 2-methyl-2-pentenal serving, 3-alkene-1-ketone, trichloropropane, 1-chloro-2-propanol, 2-chloro-1-propanol, chloropropane ether;
Described epoxy chloropropane accounts for 1 ~ 20% of impure propylene dichloride gross weight.
5. the process for purification of a kind of impure propylene dichloride according to claim 1, is characterized in that: described 4 towers all adopt the mode of pressure-fired rectifying, and described pressure-fired refers to that working pressure is lower than 10KPa, and the operating temperature of described 4 towers is 40 ~ 200 DEG C.
6. the process for purification of a kind of impure propylene dichloride according to claim 1, is characterized in that: described 1
#tower is float valve tray column, and the percentage of open area of column plate is 6 ~ 20%, and theoretical plate number is 20 ~ 50 pieces, tower top temperature 40 ~ 90 DEG C, tower top pressure 101 ~ 110kPa, and reflux ratio is 5 ~ 20.
7. the process for purification of a kind of impure propylene dichloride according to claim 1, is characterized in that: described 2
#tower is float valve tray column, and the percentage of open area of column plate is 6 ~ 20%, and theoretical plate number is 15 ~ 50 pieces, tower top temperature 70 ~ 120 DEG C, tower top pressure 101 ~ 110kPa, and reflux ratio is 2 ~ 10.
8. the process for purification of a kind of impure propylene dichloride according to claim 1, is characterized in that: described 3
#tower is packing tower, and form of bio-carrier is Raschig ring filler, and theoretical plate number is 30 ~ 60 pieces, tower top temperature 70 ~ 120 DEG C, tower top pressure 101 ~ 110kPa, and reflux ratio is 10 ~ 40.
9. the process for purification of a kind of impure propylene dichloride according to claim 1, is characterized in that: described 4
#tower is packing tower, and form of bio-carrier is Raschig ring filler, and theoretical plate number is 20 ~ 50 pieces, tower top temperature 100 ~ 140 DEG C, tower top pressure 101 ~ 110kPa, and reflux ratio is 1 ~ 15.
10. the process for purification of a kind of impure propylene dichloride according to claim 1, is characterized in that: described 1
#the opening for feed of tower is at 15th ~ 25 pieces of theoretical tray places; Described 2
#the opening for feed of tower is at 15th ~ 25 pieces of theoretical tray places; Described 3
#the opening for feed of tower is at 15th ~ 25 pieces of theoretical tray places; Described 4
#the opening for feed of tower is at 20th ~ 30 pieces of theoretical tray places.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510004499.8A CN104672052B (en) | 2015-01-06 | 2015-01-06 | Refining method of impure dichloropropane |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510004499.8A CN104672052B (en) | 2015-01-06 | 2015-01-06 | Refining method of impure dichloropropane |
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| Publication Number | Publication Date |
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| CN104672052A true CN104672052A (en) | 2015-06-03 |
| CN104672052B CN104672052B (en) | 2017-04-12 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108395364A (en) * | 2018-04-28 | 2018-08-14 | 山东海益化工科技有限公司 | The process for separation and purification of 1,2- dichloropropanes in chloropropene and production of propylene oxide waste liquid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1513820A (en) * | 2002-12-31 | 2004-07-21 | 中国石油化工股份有限公司 | Method of extracting 1,2-dichloropropane |
| CN104211564A (en) * | 2014-09-16 | 2014-12-17 | 天津大学 | Industrial device and continuous rectification method for extracting 1,2-propylene dichloride from chlorohydrin process epoxypropane waste liquid |
-
2015
- 2015-01-06 CN CN201510004499.8A patent/CN104672052B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1513820A (en) * | 2002-12-31 | 2004-07-21 | 中国石油化工股份有限公司 | Method of extracting 1,2-dichloropropane |
| CN104211564A (en) * | 2014-09-16 | 2014-12-17 | 天津大学 | Industrial device and continuous rectification method for extracting 1,2-propylene dichloride from chlorohydrin process epoxypropane waste liquid |
Non-Patent Citations (1)
| Title |
|---|
| 彭海珠等: "环氧丙烷生产废液中1,2-二氯丙烷的回收", 《化工环保》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108395364A (en) * | 2018-04-28 | 2018-08-14 | 山东海益化工科技有限公司 | The process for separation and purification of 1,2- dichloropropanes in chloropropene and production of propylene oxide waste liquid |
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| CN104672052B (en) | 2017-04-12 |
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