CN102108055A - Processing for recovering methyl anthranilate - Google Patents
Processing for recovering methyl anthranilate Download PDFInfo
- Publication number
- CN102108055A CN102108055A CN2009102450492A CN200910245049A CN102108055A CN 102108055 A CN102108055 A CN 102108055A CN 2009102450492 A CN2009102450492 A CN 2009102450492A CN 200910245049 A CN200910245049 A CN 200910245049A CN 102108055 A CN102108055 A CN 102108055A
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- CN
- China
- Prior art keywords
- methyl
- aminobenzoate
- waste water
- technology
- described step
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- 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.)
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a process for recovering methyl anthranilate, which comprises the following steps: (1) mixing treated waste water and an organic solvent, and splitting phases, wherein an extraction phase containing methyl ester oil is at the bottom, and waste water is on the top; and (2) separating extracting agent in the extraction phase from methyl ester by distillation. In the process for recovering methyl anthranilate, the low-toxicity and environmentally-friendly extracting agent is adopted to recover the methyl anthranilate from waste water, so environmental pollution is reduced, operation conditions are improved, and requirements for scale industrial production are met.
Description
Technical field
The present invention relates to relate to the recovery of methyl o-aminobenzoate, especially a kind of technology that reclaims methyl o-aminobenzoate.
Background technology
In the process that methyl o-aminobenzoate is produced, produce a large amount of waste water that contains methyl o-aminobenzoate.What the recovery methyl o-aminobenzoate generally used at present is the benzene extraction process, after promptly with the very big benzene of toxicity the methyl o-aminobenzoate in the waste water being extracted, separates obtaining methyl o-aminobenzoate again with the distillatory method.This technology easily causes occupational illness because employing benzene is that extraction agent produces harm to operator in process of production, has great potential safety hazard.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of technology that reclaims methyl o-aminobenzoate.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of technology that reclaims methyl o-aminobenzoate, concrete steps are as follows:
(1) handled waste water is mixed phase-splitting then with the hypotoxicity organic solvent, lower floor obtains containing the extraction phase of methyl o-aminobenzoate, and the upper strata is a waste water;
(2) extraction agent in the extraction phase is separated with methyl esters by distillation.
Preferably, organic solvent (being extraction agent) is toluene, hexanaphthene or hexane in the technology of above-mentioned recovery methyl o-aminobenzoate, described step (1).
Preferably, the temperature of extraction process is 20～60 ℃ in the technology of above-mentioned recovery methyl o-aminobenzoate, described step (1).
Preferably, waste water is 1～10: 1 with the volume of organic solvent ratio in the technology of above-mentioned recovery methyl o-aminobenzoate, described step (1).
Preferably, waste water is 4～10: 1 with the volume of organic solvent ratio in the technology of above-mentioned recovery methyl o-aminobenzoate, described step (1).
Preferably, the distillatory operational condition is normal pressure or decompression in the technology of above-mentioned recovery methyl o-aminobenzoate, described step (2).
Beneficial effect of the present invention:
The technology of above-mentioned recovery methyl o-aminobenzoate is passed through methyl o-aminobenzoate in the extraction agent recovery waste water employing low toxicity, eco-friendly, thereby has reduced environmental pollution, improves operational condition, is fit to requirements of large-scale industrial production.
Embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is further described.
Embodiment 1
The waste water that adds 600ml in the flask of the 1000ml that has thermometer and stirring arm adds the toluene of 60ml again, opens agitator and begins to stir, open constant temperature water bath, equitemperature picks up counting when reaching 40 ℃, stirs after half hour, leaves standstill one hour again; Layering, oil phase underpressure distillation are deviate from extraction agent and are obtained the methyl o-aminobenzoate oil phase.
The rate of recovery 98.2% through gas chromatographic analysis methyl o-aminobenzoate content is: 99.2%.
Embodiment 2-8
Processing method adopts different additional proportions with embodiment 1, and different temperature condition obtains the results are shown in following table.
| Embodiment | Extraction agent | The ratio of waste water and extraction agent | Rate of recovery % | Product content % | Toxicity | Extraction temperature ℃ |
| 2 3 4 | Toluene toluene hexanaphthene | 10∶1 10∶1 10∶1 | 98.1 98.2 88.1 | 99.2 99.1 99.2 | Low toxicity low toxicity low toxicity | 55 20 40 |
| 5 | Hexanaphthene | 7∶1 | 90.3 | 99.2 | Low toxicity | 40 |
| 6 7 8 | Cyclohexane ring hexane hexane | 5∶1 4∶1 4∶1 | 92.2 94.3 94.3 | 99.3 99.4 99.1 | Low toxicity low toxicity low toxicity | 40 40 40 |
Embodiment 9
Compare as extraction agent with original stupid (moderate toxicity, carcinogenic)
The waste water that adds 600ml in the flask of the 1000ml that has thermometer and stirring arm adds the benzene of 60ml again, opens agitator and begins to stir, and opens constant temperature water bath, and equitemperature picks up counting when reaching 40 ℃, stirs after half hour, leaves standstill one hour again; Layering, oil phase underpressure distillation are deviate from extraction agent and are obtained the MA oil phase.
The rate of recovery 93.5% through gas chromatographic analysis methyl esters content is: 99.1%.
As seen, after having adopted extraction agent to the human body low toxicity, the rate of recovery of methyl o-aminobenzoate and product content have still reached the requirement of existing production level, but significantly reduced pollution for environment, improve operational condition, reduce the harm that in the production process operator is produced, had very important production practice meaning.
Above-mentioned detailed description of this a kind of technology that reclaims methyl o-aminobenzoate being carried out with reference to embodiment; be illustrative rather than determinate; can list several embodiment according to institute's limited range; therefore in the variation and the modification that do not break away under the general plotting of the present invention, should belong within protection scope of the present invention.
Claims (6)
1. technology that reclaims methyl o-aminobenzoate, it is characterized in that: concrete steps are as follows:
(1) handled waste water is mixed phase-splitting then with the hypotoxicity organic solvent, lower floor obtains containing the extraction phase of methyl esters oil, and the upper strata is a waste water;
(2) extraction agent in the extraction phase is separated with methyl esters by distillation.
2. a kind of technology that reclaims methyl o-aminobenzoate according to claim 1 is characterized in that: organic solvent is toluene, hexanaphthene or hexane in the described step (1).
3. a kind of technology that reclaims methyl o-aminobenzoate according to claim 1 is characterized in that: the temperature of extraction process is 20～60 ℃ in the described step (1).
4. a kind of technology that reclaims methyl o-aminobenzoate according to claim 1 is characterized in that: waste water is 1～10: 1 with the volume of organic solvent ratio in the described step (1).
5. according to claim 1 or 4 described a kind of technologies that reclaim methyl o-aminobenzoate, it is characterized in that: waste water is 4～10: 1 with the volume of organic solvent ratio in the described step (1).
6. a kind of technology that reclaims methyl o-aminobenzoate according to claim 1 is characterized in that: the distillatory operational condition is normal pressure or decompression in the described step (2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102450492A CN102108055A (en) | 2009-12-23 | 2009-12-23 | Processing for recovering methyl anthranilate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102450492A CN102108055A (en) | 2009-12-23 | 2009-12-23 | Processing for recovering methyl anthranilate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102108055A true CN102108055A (en) | 2011-06-29 |
Family
ID=44172347
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009102450492A Pending CN102108055A (en) | 2009-12-23 | 2009-12-23 | Processing for recovering methyl anthranilate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102108055A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193631A (en) * | 2014-07-31 | 2014-12-10 | 中国平煤神马集团开封兴化精细化工有限公司 | Method for recovering methyl ester in waste esterified solution by continuous extraction process |
| CN104478028A (en) * | 2014-12-11 | 2015-04-01 | 沈阳化工研究院有限公司 | Treatment method of saccharin production wastewater |
-
2009
- 2009-12-23 CN CN2009102450492A patent/CN102108055A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 齐枫楠: "甲酯母液中回收邻-氨基苯甲酸甲酯的新工艺", 《河南科技》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193631A (en) * | 2014-07-31 | 2014-12-10 | 中国平煤神马集团开封兴化精细化工有限公司 | Method for recovering methyl ester in waste esterified solution by continuous extraction process |
| CN104193631B (en) * | 2014-07-31 | 2016-01-13 | 中国平煤神马集团开封兴化精细化工有限公司 | Sequential extractions reclaims the method for methyl esters in esterification waste liquid |
| CN104478028A (en) * | 2014-12-11 | 2015-04-01 | 沈阳化工研究院有限公司 | Treatment method of saccharin production wastewater |
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Application publication date: 20110629 |