CN102161629A - Treatment method for recycling isatin wastewater - Google Patents
Treatment method for recycling isatin wastewater Download PDFInfo
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- CN102161629A CN102161629A CN2010106242928A CN201010624292A CN102161629A CN 102161629 A CN102161629 A CN 102161629A CN 2010106242928 A CN2010106242928 A CN 2010106242928A CN 201010624292 A CN201010624292 A CN 201010624292A CN 102161629 A CN102161629 A CN 102161629A
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- isatin
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- aniline
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- wastewater
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Abstract
The invention relates to a treatment method for recycling isatin wastewater. The invention provides the treatment method for recycling the isatin wastewater, in order to solve the technical problem of filling in the gap of the prior art. The method comprises the following steps of: (1) controlling the mass concentration of sulfuric acid to be between 10 and 40 percent when materials are precipitated from the isatin, filtering a product, collecting waste liquid, neutralizing until the waste liquid is neutral by using inorganic base, and absorbing and filtering to remove impurities to obtain light yellow solution; and (2) taking 100 weight parts of light yellow solution obtained in step (1), adding 6 weight parts of hydroxylamine sulfate, dripping 11 weight parts of trichloracetic aldehyde, dripping 6 weight parts of aniline at normal temperature, raising the temperature to be between 75 and 100 DEG C after the materials are added, keeping the temperature for 1 to 3 hours, reducing to room temperature, filtering, collecting a filter cake, and drying to obtain a dry N-acetaldoxime aniline product. The method has the advantages of simple structure, environment friendliness and economization, and is a powerful weapon of economization, potential tapping and reduction of wastewater discharge of the conventional isatin production enterprises.
Description
Technical field
The present invention relates to the treatment process that a kind of isatin waste water reclamation utilizes again.
Background technology
In the isatin production process, produce the waste water that contains the lower concentration mineral acid in a large number, these direct discharging of waste water influence environment, and the useful matter in the waste water can not get effective utilization.
Summary of the invention
The technical problem to be solved in the present invention is how to fill up the above-mentioned blank of prior art, the treatment process that provides a kind of isatin waste water reclamation to utilize again.
For solving the problems of the technologies described above, the treatment process that isatin waste water reclamation of the present invention utilizes again comprises the steps:
1., when the isatin analysis of material, h 2 so 4 concentration is controlled at 10-40%, behind the filtering product, collect waste liquid, with in the mineral alkali and waste liquid to neutral, add an amount of sorbent material and fully adsorb impurity, filter, obtain pale yellow solution (interior contains sodium sulfate);
2., get 1. gained pale yellow solution 100 weight parts of step, adding oxammonium sulfate 6 weight parts, dropping trichoro-aldehyde 11 weight parts, normal temperature drips aniline 6 weight parts down, behind reinforced the finishing, be warming up to 75-100 ℃, insulation is 1-3 hour under this temperature, be cooled to room temperature, filter, collect filter cake, put into oven for drying, promptly get N-acetaldehyde oximido aniline dry product, wherein: oxammonium sulfate, trichoro-aldehyde, aniline purity are 99.9%.Annotate: N-acetaldehyde oximido aniline is the front end product of producing isatin, can be converted into isatin.
As optimization, step is 1. used to be selected from sodium hydroxide, potassium hydroxide, calcium hydroxide, yellow soda ash, sodium bicarbonate, salt of wormwood, saleratus, the magnesium oxide etc. one or more: step is 1. sorbent used to be diatomite, gac or ion exchange resin.
The treatment process that isatin waste water reclamation of the present invention utilizes again has simple in structurely, and the advantage of environmental protection and saving is that existing isatin manufacturing enterprise saves, taps the latent power, and reduces the powerful mean of discharge of wastewater.
Embodiment
Embodiment one: 1., when the isatin analysis of material, h 2 so 4 concentration is controlled at 10-40%, behind the filtering product, collect waste liquid, with in the yellow soda ash and waste liquid to neutral, add an amount of fully absorption of activated carbon impurity, filter, obtain pale yellow solution;
2., get the 1. gained pale yellow solution 400kg, add oxammonium sulfate 24kg, drip trichoro-aldehyde 44kg, normal temperature drips aniline 24kg down, behind reinforced the finishing, be warming up to 75 ℃, insulation is 1 hour under this temperature, is cooled to room temperature, filter, collect filter cake, put into oven for drying.Get N-acetaldehyde oximido aniline dry product 40.2kg, product purity 99.0%.Wherein: oxammonium sulfate, trichoro-aldehyde, aniline purity are 99.9%, and the aniline transformation efficiency is 94.2%.
Embodiment two: 1., replace yellow soda ash with saleratus, replace activated carbon with diatomite, repeat the 1. described operation of embodiment one step;
2., get the 1. gained pale yellow solution 1500kg, add oxammonium sulfate 90kg, drip trichoro-aldehyde 165kg, normal temperature drips aniline 90kg down, behind reinforced the finishing, be warming up to 90 ℃, insulation is 2 hours under this temperature, is cooled to room temperature, filter, collect filter cake, put into oven for drying.Get N-acetaldehyde oximido aniline dry product 148kg, product purity 99.2%.Wherein: oxammonium sulfate, trichoro-aldehyde, aniline purity are 99.9%, and the aniline transformation efficiency is 92.67%.
Embodiment three: replace yellow soda ash with magnesium oxide, spent ion exchange resin replaces activated carbon, repeats the 1. described operation of embodiment one step;
2., get the 1. gained pale yellow solution 2000kg, add oxammonium sulfate 120kg, drip trichoro-aldehyde 220kg, normal temperature drips aniline 120kg down, behind reinforced the finishing, be warming up to 100 ℃, insulation is 3 hours under this temperature, is cooled to room temperature, filter, collect filter cake, put into oven for drying.Get N-acetaldehyde oximido aniline dry product 200kg, product purity 99.1%.Wherein: oxammonium sulfate, trichoro-aldehyde, aniline purity are 99.9%, and the aniline transformation efficiency is 93.88%.
Comparative Examples: water intaking 400kg, add oxammonium sulfate 24kg, drip trichoro-aldehyde 43kg, normal temperature drips aniline 24kg down, behind reinforced the finishing, is warming up to 75 ℃, and insulation is 1 hour under this temperature, is cooled to room temperature, filters, and collects filter cake, puts into oven for drying.Get N-acetaldehyde oximido aniline dry product 38.7kg, product purity 99.0%.Wherein: oxammonium sulfate, trichoro-aldehyde, aniline purity are 99.9%, and the aniline transformation efficiency is 90.69%.
Embodiment 1-3 and Comparative Examples are compared, be not difficult to find, use the present invention and not only can recycle waste water, save the water source, subtract not discharge of wastewater, and the aniline transformation efficiency is significantly increased also.
Claims (2)
1. the treatment process that the isatin waste water reclamation utilizes again comprises the steps:
1., when the isatin analysis of material, h 2 so 4 concentration is controlled at 10-40%, behind the filtering product, collect waste liquid, with in the mineral alkali and waste liquid to neutral, add an amount of sorbent material and fully adsorb impurity, filter, obtain pale yellow solution;
2., get 1. gained pale yellow solution 100 weight parts of step, adding oxammonium sulfate 6 weight parts, dropping trichoro-aldehyde 11 weight parts, normal temperature drips aniline 6 weight parts down, behind reinforced the finishing, be warming up to 75-100 ℃, insulation is 1-3 hour under this temperature, be cooled to room temperature, filter, collect filter cake, put into oven for drying, promptly get N-acetaldehyde oximido aniline dry product, wherein: oxammonium sulfate, trichoro-aldehyde, aniline purity are 99.9%.
2. the treatment process that isatin waste water reclamation according to claim 1 utilizes again is characterized in that: step is 1. used to be selected from sodium hydroxide, potassium hydroxide, calcium hydroxide, yellow soda ash, sodium bicarbonate, salt of wormwood, saleratus, the magnesium oxide etc. one or more: step is 1. sorbent used to be diatomite, gac or ion exchange resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106242928A CN102161629A (en) | 2010-12-30 | 2010-12-30 | Treatment method for recycling isatin wastewater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106242928A CN102161629A (en) | 2010-12-30 | 2010-12-30 | Treatment method for recycling isatin wastewater |
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| Publication Number | Publication Date |
|---|---|
| CN102161629A true CN102161629A (en) | 2011-08-24 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN2010106242928A Pending CN102161629A (en) | 2010-12-30 | 2010-12-30 | Treatment method for recycling isatin wastewater |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3203855A (en) * | 1962-07-17 | 1965-08-31 | Ciba Ltd | Method for combating fungi with 2-(2, 2, 2-trichloro-1-hydroxyethylamino) pyridine |
| JPS50160229A (en) * | 1974-05-20 | 1975-12-25 | ||
| JPH11147863A (en) * | 1997-11-13 | 1999-06-02 | Mitsui Chem Inc | Production of isonitrosoacetanilide |
| CN1626514A (en) * | 2003-12-10 | 2005-06-15 | 上海化学试剂研究所 | Method for preparing-4-bromine-7-methyl isatin |
| CN101157651A (en) * | 2007-09-19 | 2008-04-09 | 吴江梅堰三友染料化工厂 | Method for preparing isatin |
-
2010
- 2010-12-30 CN CN2010106242928A patent/CN102161629A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3203855A (en) * | 1962-07-17 | 1965-08-31 | Ciba Ltd | Method for combating fungi with 2-(2, 2, 2-trichloro-1-hydroxyethylamino) pyridine |
| JPS50160229A (en) * | 1974-05-20 | 1975-12-25 | ||
| JPH11147863A (en) * | 1997-11-13 | 1999-06-02 | Mitsui Chem Inc | Production of isonitrosoacetanilide |
| CN1626514A (en) * | 2003-12-10 | 2005-06-15 | 上海化学试剂研究所 | Method for preparing-4-bromine-7-methyl isatin |
| CN101157651A (en) * | 2007-09-19 | 2008-04-09 | 吴江梅堰三友染料化工厂 | Method for preparing isatin |
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Application publication date: 20110824 |