CN1347871A - Continuous rectification method of refining 4-amino diphenylamine - Google Patents
Continuous rectification method of refining 4-amino diphenylamine Download PDFInfo
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- CN1347871A CN1347871A CN 01134116 CN01134116A CN1347871A CN 1347871 A CN1347871 A CN 1347871A CN 01134116 CN01134116 CN 01134116 CN 01134116 A CN01134116 A CN 01134116A CN 1347871 A CN1347871 A CN 1347871A
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Abstract
The present invention relates to the preparation of dye and assistant intermediate. The continuous 4-amino diphenylamine refining process is one in two serially connected towers, including the front fraction tower and the back product tower. In vacuum condition, preheated coarse 4-amino diphenylamine is fed to the front fraction tower continuously, light component is picked out from the top of the tower and the lower bottoms is fed to the product tower for further refining. The technological parameters includes preheating temperature 100-150 deg.c, top temperature of the front tower 80-100 deg.c, temperature in the product tower 200-240 deg.c reflux ratio 1-10, tower top temperature 180-220 deg.c and tower bottom temperature 240-300 deg.c. The front tower is heated in hot siphonal reboiler, the product tower in falling film evaporator, and heat medium is high temperature heat conducting oil.
Description
One, technical field
The present invention is a kind of dyestuff and auxiliary agent intermediates preparation, the especially method of 4-aminodiphenylamine.
Two, background technology
4-aminodiphenylamine (4-Aminodiphenylamine) is commonly called as RT training department, is important dyestuff and auxiliary agent intermediate, is mainly used in synthetic Ursol D class rubber antioxidant.The production route of employing generally is with p-Nitrophenyl chloride and aniline condensation both at home and abroad, makes p-nitrodiphenylamine, through reduction, can get 4-aminodiphenylamine crude product, and crude product gets finished product again through washing, distill refining.
Existing 4-aminodiphenylamine production technology, make with extra care and all adopt single tower batch distillation separating technology, the tower still generally adopts infrared ray heating, boiling point reaches 354 ℃ under the 4-aminodiphenylamine normal pressure, so Heating temperature is up to more than 400～600 ℃, the energy consumption height, device fabrication intensity is low, poor product quality and instability (＜98.5%), and the product coking is serious under the high temperature.
Three, technology contents
(1) goal of the invention
Purpose of the present invention just provides a kind of product production, steady quality, and energy consumption is low, the method for the continuous rectification refining 4-amino pentanoic that yield is high.
(2) technical scheme
The method of continuous rectification refining 4-amino pentanoic of the present invention is to adopt the method for two towers series connection continuous rectification, first is the front-end volatiles tower, one of back is a finishing column, under vacuum condition, enter the front-end volatiles tower continuously after the preheating of crude product 4-aminodiphenylamine, light component is from the cat head extraction, tower bottoms is delivered to finishing column, from finishing column extraction finished product 4-aminodiphenylamine.The preheating temperature of crude product 4-aminodiphenylamine is 100 ℃～150 ℃, and the tower top temperature of front-end volatiles tower is 80 ℃～100 ℃.The temperature of finishing column is 200 ℃～240 ℃, and reflux ratio is 1～10, and tower top temperature is 180 ℃～220 ℃, and tower still temperature is 240 ℃～300 ℃.The front-end volatiles tower adopts the thermosyphon reboiler heating, and finishing column adopts the falling-film evaporator heating, and heating agent adopts high temperature heat conductive oil.
(3) technique effect
The more existing single tower batch distillation technology of continuous rectificating technique of the present invention, its advantage are that refining back final product quality significantly improves, and purity reaches more than 99.1%, and it is big to have output, advantages such as steady quality, and ton product separation energy consumption reduces by 50%.Because Heating temperature is below 300 ℃, product coking situation alleviates, and tar content descends 30%.The investment of this technology and floor space have all obtained saving, and identical size investment descends 50%.
Four, embodiment
Embodiments of the invention are as follows:
The present invention substitutes the process for purification of former single tower batch distillation with multitower series connection continuous rectificating technique, and according to processing condition and material characteristic after changing change is made in type of heating, reboiler lectotype selection aspect, so that treating process is more scientific and reasonable, efficient.
This process for refining adopts the series connection of two towers, and one is the front-end volatiles tower, and one is finishing column.Under 0～50mm mercury column working pressure, crude product 4-aminodiphenylamine is preheated to 100～150 ℃, enters the front-end volatiles tower continuously, about 90 ℃ of tower top temperatures, and light constituent is adopted from cat head, applies mechanically to 4-aminodiphenylamine technological process of production conversion zone; Finishing column is delivered in the tower bottoms extraction.About 220 ℃ of finishing column temperature, reflux ratio is 1～10, and tower top temperature is about 200 ℃, extraction finished product 4-aminodiphenylamine; 240～300 ℃ of tower still temperature, tower bottoms go three cut pots to reclaim the 4-aminodiphenylamine.
According to above-mentioned processing condition and material characteristic, the front-end volatiles tower adopts the thermosyphon reboiler heating, and finishing column adopts the falling-film evaporator heating, and heating agent adopts high temperature heat conductive oil.Rectifying tower top condenser recovered steam has improved heat transfer efficiency, has reclaimed the energy simultaneously.
Claims (4)
1. the method for a continuous rectification refining 4-amino pentanoic, it is characterized in that adopting the method for two towers series connection continuous rectification, first is the front-end volatiles tower, one of back is a finishing column, under vacuum condition, enter the front-end volatiles tower continuously after the preheating of crude product 4-aminodiphenylamine, light component is from the cat head extraction, and tower bottoms is delivered to finishing column, from finishing column extraction finished product 4-aminodiphenylamine.
2. the method for continuous rectification refining 4-amino pentanoic according to claim 1, the preheating temperature that it is characterized in that crude product 4-aminodiphenylamine are 100 ℃～150 ℃, and the tower top temperature of front-end volatiles tower is 80 ℃～100 ℃.
3. the method for continuous rectification refining 4-amino pentanoic according to claim 1 and 2, the temperature that it is characterized in that finishing column are 200 ℃～240 ℃, and reflux ratio is 1～10, and tower top temperature is 180 ℃～220 ℃, and tower still temperature is 240 ℃～300 ℃.
4. the method for continuous rectification refining 4-amino pentanoic according to claim 1 and 2 is characterized in that the front-end volatiles tower adopts the thermosyphon reboiler heating, and finishing column adopts the falling-film evaporator heating, and heating agent adopts high temperature heat conductive oil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011341165A CN1156436C (en) | 2001-10-30 | 2001-10-30 | Continuous rectification method of refining 4-amino diphenylamine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011341165A CN1156436C (en) | 2001-10-30 | 2001-10-30 | Continuous rectification method of refining 4-amino diphenylamine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1347871A true CN1347871A (en) | 2002-05-08 |
| CN1156436C CN1156436C (en) | 2004-07-07 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011341165A Expired - Fee Related CN1156436C (en) | 2001-10-30 | 2001-10-30 | Continuous rectification method of refining 4-amino diphenylamine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1156436C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114685362A (en) * | 2020-12-31 | 2022-07-01 | 中国石油化工股份有限公司 | Separation method of 2-methylpyridine |
-
2001
- 2001-10-30 CN CNB011341165A patent/CN1156436C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114685362A (en) * | 2020-12-31 | 2022-07-01 | 中国石油化工股份有限公司 | Separation method of 2-methylpyridine |
| CN114685362B (en) * | 2020-12-31 | 2024-05-03 | 中国石油化工股份有限公司 | Separation method of 2-methylpyridine |
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| Publication number | Publication date |
|---|---|
| CN1156436C (en) | 2004-07-07 |
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