CN1158332A - Process for purifying meta-hydroxy diethyl-aniline - Google Patents
Process for purifying meta-hydroxy diethyl-aniline Download PDFInfo
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- CN1158332A CN1158332A CN 96116259 CN96116259A CN1158332A CN 1158332 A CN1158332 A CN 1158332A CN 96116259 CN96116259 CN 96116259 CN 96116259 A CN96116259 A CN 96116259A CN 1158332 A CN1158332 A CN 1158332A
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Abstract
A process for purifying meta-hydroxydiethylaniline features that purer material is educed out by control of cooling speed and range in refining pot, then temp is raised at a certain rate to make the content of distillate (meta-hydroxydiethyl amine) increase by gradation, and finally needed product is discharged by steps. Its advantages includes high purity of product (greater than or equal to 99.5%), less loss and no environmental pollution.
Description
The present invention relates to the method for purification of dyestuff intermediate, specifically, it is a kind of purifying technique of meta-hydroxy diethyl-aniline.
Meta-hydroxy diethyl-aniline is a kind of important dyestuff intermediate, and it is to be used to produce basic dyestuff.The important source material of products such as photographic dye, laser dyes and pressure sensitive dye.But the production technique of traditional meta-hydroxy diethyl-aniline is to adopt distillation method to purify, and quality product (purity) is lower, generally only 98%, can't satisfy the requirement of high-quality photographic dye, laser dyes and pressure sensitive dye.In the prior art, adopt further rectifying and absorbing process to purify meta-hydroxy diethyl-aniline, had quality product (purity) instability but should go up skill, the unit consumption height, and produce a large amount of " three wastes " and need to handle.
The inventor finds that by research repeatedly meta-hydroxy diethyl-aniline is easy to generate dealkylation when pyrogenic distillation, and single ethyl product is increased; Adopt rectifying and absorption to go up and plant when purifying, for example, can not remove single ethyl product fully again with charcoal absorption, therefore make quality (purity) instability of purified meta-hydroxy diethyl-aniline, unit consumption is high again, and " three wastes " are serious.
Skill is newly gone up in the purification that the purpose of this invention is to provide a kind of meta-hydroxy diethyl-aniline, and not only unit consumption is low, and product purity height (〉=99.5%), does not have " three wastes " and produces.
The objective of the invention is to realize in the following manner: a kind of purifying technique of meta-hydroxy diethyl-aniline, it is characterized in that the fusion meta-hydroxy diethyl-aniline that content with 100 parts of weight is at least 80% (weight) adds in the treatment tank, apace at 30 minutes internal cooling to more than the fusing point of material 1～2 ℃, lower the temperature by rate of temperature fall then, after cooling finishes, be warming up on the fusing point of material 10 ℃ by temperature rise rate again, the step emission material, obtain the meta-hydroxy diethyl-aniline that is lower than charging content of 20 parts of weight at the most, the meta-hydroxy diethyl-aniline that equals charging content of 30～35 parts of weight and the meta-hydroxy diethyl-aniline greater than charging content of at least 50 parts of weight.
It is characterized in that content with 100 parts of weight is that the fusion meta-hydroxy diethyl-aniline of 98% (weight) is as to treatment tank, in 30 minutes, be cooled to 70 ℃ apace, be cooled to 50 ℃ with 1～5 ℃ speed per hour then, then be warming up to 70 ± 0.5 ℃, and the content that discharges the no more than 20 parts of weight of this fraction is the meta-hydroxy diethyl-aniline of 90 ± 2% (weight) with 2～4 ℃ speed control per hour; Then control is warming up to 73 ± 0.5 ℃ again, and the content that discharges 30～35 parts of weight of this fraction is the meta-hydroxy diethyl-aniline of 98 ± 0.5% (weight); Control is warming up to 86 ℃ again, and the content that discharges at least 45 parts of weight of this fraction is the meta-hydroxy diethyl-aniline of 99.2 ± 0.1% (weight).
It is characterized in that content with 100 parts of weight is that the fusion meta-hydroxy diethyl-aniline of 99.2% (weight) adds in the treatment tank, in 30 minutes, be cooled to 75 ℃ apace, be cooled to 55 ℃ with 1～5 ℃ speed per hour then, then be warming up to 73 ± 0.5 ℃, and the content that discharges the no more than 16 parts of weight of this fraction is the meta-hydroxy diethyl-aniline of 98 ± 0.5% (weight) with 2～4 ℃ speed control per hour; Then control is warming up to 76 ± 0.5 ℃ again, and the content that discharges 30 parts of weight of this fraction is the meta-hydroxy diethyl-aniline of 99.2 ± 0.1% (weight); Control is warming up to 86 ℃ again, and the content that discharges at least 54 parts of weight of this fraction is the meta-hydroxy diethyl-aniline of 99.7 ± 0.1% (weight).
Advantage of the present invention is tangible, not only energy consumption is low than traditional distil process, existing rectifying and absorbing process for purifying technique of the present invention, yield height, and the quality of product (purity) height can satisfy the high-quality requirement of photographic dye, laser dyes and pressure sensitive dye; Adopt purifying technique of the present invention not only the purity of meta-hydroxy diethyl-aniline can reach more than 99.5%, and the meta-hydroxy diethyl-aniline of producing 1 ton of 99.5% above purity only consumes 1.1 tons 98% thick meta-hydroxy diethyl-aniline.In addition, the present invention adopts physical method to purify, and no coupling product produces, and not having " three wastes " needs to handle.
Below, the present invention will be described in further detail in conjunction with specific embodiments, so that advantage of the present invention is more obvious.Embodiment 1:
With the content of 100 parts of weight is that the fusion meta-hydroxy diethyl-aniline of 98% (weight) adds in the shell and tube crystal refining jar, apace at 30 minutes internal cooling to 70 ℃, be cooled to 50 ℃ with 1～5 ℃ speed control per hour then, then be warming up to 69 ℃ with 2～4 ℃ speed control per hour, and 20 parts of weight of meta-hydroxy diethyl-aniline of discharging this fraction, content is 90% (weight); Then control is warming up to 73 ℃ again, and discharges 35 parts of weight of meta-hydroxy diethyl-aniline of this fraction, and content is 98% (weight); Control is warming up to 86 ℃ again, is incubated 1 hour, and discharges 45 parts of weight of meta-hydroxy diethyl-aniline of this fraction, and content is 99.2% (weight).Embodiment 2:
With content among 100 parts of weight embodiment 1 is that the fusion meta-hydroxy diethyl-aniline of 99.2% (weight) adds in the shell and tube crystal refining jar, apace at 30 minutes internal cooling to 75 ℃, be cooled to 55 ℃ with 1～5 ℃ speed control per hour then, then be warming up to 73 ℃ with 2～4 ℃ speed control per hour, and 16 parts of weight of meta-hydroxy diethyl-aniline of discharging this fraction, content is 98% (weight); Then control is warming up to 76 ℃ again, and discharges 25 parts of weight of meta-hydroxy diethyl-aniline of this fraction, and content is 99.2% (weight); Control is warming up to 86 ℃ again, is incubated 1 hour, and discharges 59 parts of weight of meta-hydroxy diethyl-aniline of this fraction, and content is 99.7% (weight).Embodiment 3:
With content among 100 parts of weight embodiment 1 is that the fusion meta-hydroxy diethyl-aniline of 90% (weight) adds in the shell and tube crystal refining jar, apace at 30 minutes internal cooling to 65 ℃, be cooled to 45 ℃ with 1～5 ℃ speed control per hour then, then be warming up to 65 ℃ with 2～4 ℃ speed control per hour, and 15 parts of weight of meta-hydroxy diethyl-aniline of discharging this fraction, content is 80% (weight); Then control is warming up to 69 ℃ again, and discharges 35 parts of weight of meta-hydroxy diethyl-aniline of this fraction, and content is 90% (weight); Control is warming up to 86 ℃ again, is incubated 1 hour, and discharges 50 parts of weight of meta-hydroxy diethyl-aniline of this fraction, and content is 98% (weight).Embodiment 4:
With content among 100 parts of weight embodiment 3 is that the fusion meta-hydroxy diethyl-aniline of 80% (weight) adds in the shell and tube crystal refining jar, apace at 30 minutes internal cooling to 50 ℃, be cooled to 20 ℃ with 1～5 ℃ speed control per hour then, then be warming up to 50 ℃ with 2～4 ℃ speed control per hour, and 18 parts of weight of meta-hydroxy diethyl-aniline of discharging this fraction, content is 70% (weight); Then control is warming up to 65 ℃ again, and discharges 32 parts of weight of meta-hydroxy diethyl-aniline of this fraction, and content is 80% (weight); Control is warming up to 86 ℃ again, is incubated 1 hour, and discharges the 50 parts of weight of meta-hydroxy diethyl-aniline than fraction, and content is 90% (weight).
Claims (3)
1. the purifying technique of a meta-hydroxy diethyl-aniline, it is characterized in that the fusion meta-hydroxy diethyl-aniline that content with 100 parts of weight is at least 80% (weight) adds in the treatment tank, apace at 30 minutes internal cooling to more than the fusing point of material 1～2 ℃, lower the temperature by rate of temperature fall then, after cooling finishes, be warming up on the fusing point of material 10 ℃ by temperature rise rate again, the step emission material, obtain the meta-hydroxy diethyl-aniline that is lower than charging content of 20 parts of weight at the most, the meta-hydroxy diethyl-aniline that equals charging content of 30～35 parts of weight and the meta-hydroxy diethyl-aniline greater than charging content of at least 50 parts of weight.
2. the skill that goes up according to claim 1, it is characterized in that content with 100 parts of weight is that the fusion meta-hydroxy diethyl-aniline of 98% (weight) adds in the treatment tank, in 30 minutes, be cooled to 70 ℃ apace, be cooled to 50 ℃ with 1～5 ℃ speed per hour then, then be warming up to 70 ± 0.5 ℃, and the content that discharges the no more than 20 parts of weight of this fraction is the meta-hydroxy diethyl-aniline of 90 ± 2% (weight) with 2～4 ℃ speed control per hour; Then control is warming up to 73 ± 0.5 ℃ again, and the content that discharges 30～35 parts of weight of this fraction is the meta-hydroxy diethyl-aniline of 98 ± 0.5% (weight); Control is warming up to 86 ℃ again, and the content that discharges at least 45 parts of weight of this fraction is the meta-hydroxy diethyl-aniline of 99.2 ± 0.1% (weight).
3. technology according to claim 1 and 2, it is characterized in that content with 100 parts of weight is that the fusion meta-hydroxy diethyl-aniline of 99.2% (weight) adds in the treatment tank, in 30 minutes, be cooled to 75 ℃ apace, be cooled to 55 ℃ with 1～5 ℃ speed per hour then, then be warming up to 73 ± 0.5 ℃, and the content that discharges the no more than 16 parts of weight of this fraction is the meta-hydroxy diethyl-aniline of 98 ± 0.5% (weight) with 2～4 ℃ speed control per hour; Then control is warming up to 76 ± 0.5 ℃ again, and the content that discharges 30 parts of weight of this fraction is the meta-hydroxy diethyl-aniline of 99.2 ± 0.1% (weight); Control is warming up to 86 ℃ again, and the content that discharges at least 54 parts of weight of this fraction is the meta-hydroxy diethyl-aniline of 99.7 ± 0.1% (weight).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96116259 CN1158332A (en) | 1996-02-26 | 1996-02-26 | Process for purifying meta-hydroxy diethyl-aniline |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96116259 CN1158332A (en) | 1996-02-26 | 1996-02-26 | Process for purifying meta-hydroxy diethyl-aniline |
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| Publication Number | Publication Date |
|---|---|
| CN1158332A true CN1158332A (en) | 1997-09-03 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 96116259 Pending CN1158332A (en) | 1996-02-26 | 1996-02-26 | Process for purifying meta-hydroxy diethyl-aniline |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102086156A (en) * | 2011-01-25 | 2011-06-08 | 河北建新化工股份有限公司 | Preparation method of high-purity m-hydroxl-N,N-diethyl aniline |
-
1996
- 1996-02-26 CN CN 96116259 patent/CN1158332A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102086156A (en) * | 2011-01-25 | 2011-06-08 | 河北建新化工股份有限公司 | Preparation method of high-purity m-hydroxl-N,N-diethyl aniline |
| CN102086156B (en) * | 2011-01-25 | 2012-11-07 | 河北建新化工股份有限公司 | Preparation method of high-purity m-hydroxl-N,N-diethyl aniline |
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