CN100999440A - Separation method of chloro isoamylene - Google Patents
Separation method of chloro isoamylene Download PDFInfo
- Publication number
- CN100999440A CN100999440A CN 200610147815 CN200610147815A CN100999440A CN 100999440 A CN100999440 A CN 100999440A CN 200610147815 CN200610147815 CN 200610147815 CN 200610147815 A CN200610147815 A CN 200610147815A CN 100999440 A CN100999440 A CN 100999440A
- Authority
- CN
- China
- Prior art keywords
- tower
- temperature
- separation method
- reflux ratio
- towers
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
This invention relates to a separation method of chlor-isoamylene. First preheats the output of isoprene react with hydrogen chloride; then send the output into the first tower central of continuous distillation tower which includes two series towers for vacuum distillation; the first tower pressure is -0.070 ~ - 0.100MPa, the top temperature of 30 ~ 60 deg C, the temperature of the tower reactor is 50 ~ 70 deg C, reflux ratio is 2 ~ 5; reflux pot of first tower has a Layered device for regular separating water; outputs component of reflux pot enter isomerism reactor for isomerism reaction, after water separating return to first tower; tower reactor components enter central of second tower, pressure is - 0.08 ~ 0.10MPa, the top temperature of 30 ~ 50deg, tower reactor temperature of 60 ~ 80 deg C, reflux ratio is 1-3, store the products of consecutive distillation in the tank with cooling jacket. Compared with existing technologies, this invention has energy-saving, high purity features.
Description
Technical field
The present invention relates to the chemical intermediate production field, chemical separation technology, especially relate to by isoprene and hydrogenchloride adduct through rectification under vacuum separate the method for chloroisoamylene.
Background technology
Chloroisoamylene is meant 1-chloro-3-methyl-butene-2 (being called for short " 1-chlorine "), is the important intermediate of synthetic medicine, spices and Pesticidal products.The product that is generated by isoprene and hcl reaction be itself and 3-chloro-3-methyl-butene-1 mixture of (being called for short " 3-chlorine "), and with the by product dichloro iso-pentane of connecting on a small quantity.
The general two tower separation methods that adopt, a tower takes off gently, and the cat head component is returned and is advanced tower rectifying again after isomery improves the 1-cl content, and component is advanced two towers and is taken off weight, overhead collection 1-chlorine products at the bottom of the tower.Because the isomery of 1-chlorine to 3-chlorine takes place in the rectifying, exist a tower amount of returning big, two tower product purities are put forward not high defective.
Summary of the invention
Purpose of the present invention is exactly the separation method that a kind of highly purified chloroisoamylene is provided for the weak point that overcomes above-mentioned prior art existence.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of separation method of chloroisoamylene, it is characterized in that this method is sent into the tower middle part that two towers of connecting are formed continuous rectification with the product that isoprene and hcl reaction generate through preheating, carries out rectification under vacuum, one pressure tower is-0.070～-0.100Mpa, tower top temperature is 30～60 ℃, and tower still temperature is 50～70 ℃, reflux ratio 2～5, one tower return tank has quantizer, regularly divide water, return tank output component enters the isomerization reaction still and carries out isomerization reaction, returns a tower behind the branch water; Tower still component is entered two towers middle parts, and two pressure towers be-0.08～-0.100Mpa, 30～50 ℃ of tower top temperatures, 60～80 ℃ of tower still temperature, reflux ratio 1～3, the continuous rectification products obtained therefrom is stored in strap clamp and overlaps the refrigerative storage tank.
Described quantizer place tower return tank bottom or with the return tank one.
Described isomerization reaction is that a column overhead component is advanced reactor and added small amount of acid and carry out, and temperature of reaction is 25～35 ℃, 1～3 hour reaction times.
A described pressure tower is-0.080～-0.095Mpa, tower top temperature is 35～50 ℃, tower still temperature is 57～68 ℃, reflux ratio 2～4.
Described two pressure towers are-0.09～-0.096Mpa, 38～45 ℃ of tower top temperatures, 68～72 ℃ of tower still temperature, reflux ratio 1～2.
Compared with prior art, this separation method of the present invention increases the measure of branch water (acid), and a column overhead phlegma is entered the quantizer layering, advancing tower after dewatering again refluxes, thereby reduce the group component that a tower needs isomery, play tangible energy-conserving action, the rectifying yield is greatly improved; Two towers are because of the minimizing of moisture content in the feed component, and product purity is significantly improved.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
Addition liquid (1-cl content 70%) is sent into the tower middle part that series connection two towers are formed continuous rectification through preheating, one pressure tower control-0.092Mpa, 35 ℃ of tower top temperature controls, 57 ℃ of tower still temperature, reflux ratio 3, continuous rectification, return tank regularly divides water, to guarantee that entering tower backflow component does not contain free acid, return tank output component is returned a tower after isomery divides water; Tower still component is entered two towers middle part, two pressure tower control-0.094Mpa, and 39 ℃ of tower top temperature controls, 65 ℃ of tower still temperature, reflux ratio 1, continuous rectification must be to 98% 1-chlorine products, and the rectifying yield is 91%.
Embodiment 2
Addition liquid (1-cl content 70%) is sent into the tower middle part that series connection two towers are formed continuous rectification through preheating, one pressure tower control-0.082Mpa, 48 ℃ of tower top temperature controls, 67 ℃ of tower still temperature, reflux ratio 3, continuous rectification, return tank regularly divides water, to guarantee that entering tower backflow component does not contain free acid, return tank output component is returned a tower after isomery divides water; Tower still component is entered two towers middle part, two pressure tower control-0.092Mpa, and 45 ℃ of tower top temperature controls, 70 ℃ of tower still temperature, reflux ratio 1, continuous rectification must be to 97.2% 1-chlorine products, and the rectifying yield is 91%.
Embodiment 3
Addition liquid (1-cl content 70%) is sent into the tower middle part that series connection two towers are formed continuous rectification through preheating, one pressure tower control-0.095Mpa, 32 ℃ of tower top temperature controls, 55 ℃ of tower still temperature, reflux ratio 4, continuous rectification, return tank regularly divides water, to guarantee that entering tower backflow component does not contain free acid, return tank output component is returned a tower after isomery divides water; Tower still component is entered two towers middle part, two pressure tower control-0.096Mpa, and 38 ℃ of tower top temperature controls, 65 ℃ of tower still temperature, reflux ratio 2, continuous rectification must be to 97.2% 1-chlorine products, and the rectifying yield is 91%.
Claims (5)
1. the separation method of a chloroisoamylene, it is characterized in that this method is sent into the tower middle part that two towers of connecting are formed continuous rectification with the product that isoprene and hcl reaction generate through preheating, carries out rectification under vacuum, one pressure tower is-0.070～-0.100Mpa, tower top temperature is 30～60 ℃, and tower still temperature is 50～70 ℃, reflux ratio 2～5, one tower return tank has quantizer, regularly divide water, return tank output component enters the isomerization reaction still and carries out isomerization reaction, returns a tower behind the branch water; Tower still component is entered two towers middle parts, and two pressure towers be-0.08～-0.100Mpa, 30～50 ℃ of tower top temperatures, 60～80 ℃ of tower still temperature, reflux ratio 1～3, the continuous rectification products obtained therefrom is stored in strap clamp and overlaps the refrigerative storage tank.
2. the separation method of a kind of chloroisoamylene according to claim 1 is characterized in that, described quantizer place tower return tank bottom or with the return tank one.
3. the separation method of a kind of chloroisoamylene according to claim 1 is characterized in that, described isomerization reaction is that a column overhead component is advanced reactor and added small amount of acid and carry out, and temperature of reaction is 25～35 ℃, 1～3 hour reaction times.
4. the separation method of a kind of chloroisoamylene according to claim 1 is characterized in that, a described pressure tower is-0.080～-0.095Mpa, tower top temperature is 35～50 ℃, tower still temperature is 57～68 ℃, reflux ratio 2～4.
5. the separation method of a kind of chloroisoamylene according to claim 1 is characterized in that, described two pressure towers are-0.09～-0.096Mpa, 38～45 ℃ of tower top temperatures, 68～72 ℃ of tower still temperature, reflux ratio 1～2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610147815 CN100999440A (en) | 2006-12-22 | 2006-12-22 | Separation method of chloro isoamylene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610147815 CN100999440A (en) | 2006-12-22 | 2006-12-22 | Separation method of chloro isoamylene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN100999440A true CN100999440A (en) | 2007-07-18 |
Family
ID=38258277
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610147815 Pending CN100999440A (en) | 2006-12-22 | 2006-12-22 | Separation method of chloro isoamylene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100999440A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040481A (en) * | 2009-10-23 | 2011-05-04 | 中国石油化工股份有限公司 | Method for utilizing production waste liquor generated during preparing 1-chloroisopentene from isoprene |
| CN102367219A (en) * | 2011-07-19 | 2012-03-07 | 赵明江 | Preparation method of chloroisopentene |
-
2006
- 2006-12-22 CN CN 200610147815 patent/CN100999440A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040481A (en) * | 2009-10-23 | 2011-05-04 | 中国石油化工股份有限公司 | Method for utilizing production waste liquor generated during preparing 1-chloroisopentene from isoprene |
| CN102367219A (en) * | 2011-07-19 | 2012-03-07 | 赵明江 | Preparation method of chloroisopentene |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4418589B2 (en) | Method and apparatus for producing butyl acetate and isobutyl acetate | |
| CN104529763A (en) | Process and device for synthesizing ethyl formate with reactive distillation dividing wall column | |
| CN203923057U (en) | Improved Butanol Recycling device | |
| CN103664516B (en) | The ethylene glycol separating technology of synthetic gas preparing ethylene glycol | |
| TWI322801B (en) | Separation system and method for hydrolysis of methyl acetate | |
| CN101857201A (en) | Device for producing high-purity oxygen and krypton-xenon concentrate and using method thereof | |
| CN105712839A (en) | Separation method simultaneously suitable for preparing isopropanol by propylene hydration and acetone hydrogenation | |
| CN100999440A (en) | Separation method of chloro isoamylene | |
| EP0031097A1 (en) | Method for distilling ethyl alcohol | |
| CN103706136B (en) | For the double rectification column separation method of purification of methyl tertiary butyl ether(MTBE) in statins building-up process waste liquid-tetrahydrofuran recycling | |
| CN103360216A (en) | Device and method for preparing fatty alcohol by carboxylate hydrolysis | |
| EP3010878B1 (en) | Dividing wall in ethanol purification process | |
| CN108947774A (en) | A kind of method and device of separating isopropanol | |
| CN202315373U (en) | Novel continuous dimethylacetylamide rectifying device | |
| CN102091432B (en) | 3-methyl-2-penten-4-yn-1-ol vitamin A intermediate purifying method and device | |
| CN103523756A (en) | Production method and device of high-concentration hydrogen peroxide | |
| CN104961624B (en) | Octyl alconyl produces the recoverying and utilizing method of waste liquid | |
| US9150473B2 (en) | Method for producing allyl alcohol | |
| CN103073412A (en) | PAT solvent dehydration system and dehydration technology | |
| CN102992930B (en) | Recovery process and separation device of toluene solvent in production process of alpha-acetyl-gamma butyrolactone | |
| CN201762096U (en) | Device for producing high-purity oxygen and krypton xenon concentrate | |
| CN105669445A (en) | Production technology of ethyl acetate | |
| CN206232637U (en) | A kind of ethylene carbonate purification system | |
| CN205635422U (en) | Device for separating isopropanol from water-containing acetone hydrogenation product | |
| CN105582811B (en) | A kind of purification of raw materials method for Separation of Boron Isotopes |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20070718 |