CN104447520A - Pretreatment process of synthetic waste liquid of 3,5-6-trichloropyridin-2-ol sodium - Google Patents
Pretreatment process of synthetic waste liquid of 3,5-6-trichloropyridin-2-ol sodium Download PDFInfo
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- CN104447520A CN104447520A CN201410638485.7A CN201410638485A CN104447520A CN 104447520 A CN104447520 A CN 104447520A CN 201410638485 A CN201410638485 A CN 201410638485A CN 104447520 A CN104447520 A CN 104447520A
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- waste liquid
- trichloropyridine
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- sodium alkoxide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/62—Oxygen or sulfur atoms
- C07D213/63—One oxygen atom
- C07D213/64—One oxygen atom attached in position 2 or 6
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Pyridine Compounds (AREA)
Abstract
The invention relates to a treatment process of a synthetic waste liquid of 3,5-6-trichloropyridin-2-ol sodium. The treatment process comprises an oxidation-adsorption treatment procedure. The process has the effects that 3,5-6-trichloropyridin-2-ol sodium and acrylonitrile in wastewater and the chroma of the wastewater can be effectively reduced, biochemical properties can be improved, and the process is simple to operate and is low in cost.
Description
Technical field
The present invention relates to a kind of pretreatment technology of synthesis waste liquid of 3,5,6-trichloropyridine-2-sodium alkoxide, belong to field of environment protection.
Background technology
3,5,6-trichloropyridine-2-alcohol sodium pure product is lurid solid, and be that the huge legendary turtle of a kind of important industrial chemicals and excellent property closes flotation agent, synthesize the important intermediate of Multiple Pesticides especially, topmost application is that production broad-spectrum organophosphorous pesticide poisons cicada with poison.
Poisoning cicada with poison applies very extensive at present, have efficient, wide spectrum, low residue and low drug-fast characteristic by tagging, stomach toxicity and stifling mode, can effectively prevent and treat the over one hundred kind of insects such as snout moth's larva, tortrix moth, mythimna separata, scale insect, aphid, be one of pesticide species that output is maximum in the world.
The synthetic method of 3,5,6-trichloropyridine-2-sodium alkoxide is divided by starting raw material and is mainly contained pyridine or derivatives thereof method trichoroacetic chloride method, trichoroacetic acid(TCA) phenyl ester method and propylene acid system etc.The advantages such as trichoroacetic chloride one-step synthesis method 3,5,6-trichloropyridine-2-sodium alkoxide has raw material and is cheaply easy to get, and easy to operate, yield is good, and purity is high are that current China adopts maximum synthetic methods.
Trichoroacetic chloride synthesis method be with trichoroacetic chloride and acrylonitrile for raw material, under the effect of cuprous chloride catalyst, finally obtain product trichloro pyridyl sodium alcoholate through addition, cyclisation and aromizing three-step reaction.Complicated component in one-step synthesis method waste liquid, concentration is high.Wherein 3,5,6-trichloropyridine-2-sodium alkoxide are about 0.5%, and vinyl cyanide is about 0.01%.3,5,6-trichloropyridine-2-sodium alkoxide is unstable, in concentration higher than water can be made during 2mg/L aobvious red, and biochemical difficulty.Vinyl cyanide toxicity is large, needs strictly to control.
Summary of the invention
The technical matters that the present invention will adopt is a kind of 3,5,6-trichloropyridine-2-sodium alkoxide pretreatment technology, can realize the recovery of 3,5,6-trichloropyridine-2-sodium alkoxide, the degraded of 3,5,6-trichloropyridine-2-sodium alkoxide and vinyl cyanide, reduce wastewater toxicity.
1, a kind for the treatment of process of synthesis waste liquid of 3,5,6-trichloropyridine-2-sodium alkoxide, it is characterized in that, it comprises the steps:
(1) in trichloro pyridyl sodium alcoholate synthesis waste liquid 37% concentrated hydrochloric acid adjust ph to 2 ~ 3, after precipitation 30min ~ 60min, filter, reclaim 3,5,6-trichloropyridine-2-sodium alkoxide;
(2) in filtrate, add potassium permanganate rapid stirring, carry out oxidizing reaction 40min ~ 95min, then filter under 40 DEG C ~ 85 DEG C water-baths, described potassium permanganate add-on and the mass ratio of waste water are 2.5% ~ 3%;
(3) add sorbent material in filtrate, at 75 DEG C ~ 85 DEG C, adsorb 20min ~ 40min, be then cooled to room temperature, filter out filter residue.
The pretreatment technology of the synthesis waste liquid of described one 3,5,6-trichloropyridine-2-sodium alkoxide, it is characterized in that, the synthesis waste liquid of 3,5,6-described trichloropyridine-2-sodium alkoxide, for the waste liquid that trichoroacetic chloride one-step synthesis method produces, wherein alcohol sodium content is about 5000mg/L, and vinyl cyanide is 100 mg/L, ammonia nitrogen 100 mg/L, alkalescence, reddish black.
The pretreatment technology of the synthesis waste liquid of described one 3,5,6-trichloropyridine-2-sodium alkoxide, it is characterized in that, described sorbent material is activated carbon.
Agents useful for same of the present invention is conventional dose.
Positive progressive effect of the present invention is: 3,5,6-trichloropyridine-2-sodium alkoxide in energy efficient recovery waste water of the present invention, the rate of recovery 70% ~ 80%, purity more than 95%.3,5,6-trichloropyridine-2-sodium alkoxide in waste water and vinyl cyanide are effectively degraded and are adsorbed, and in the waste water after process, 3,5,6-trichloropyridine-2-sodium alkoxide are lower than 0.6mg/L, and vinyl cyanide is lower than 0.5mg/L, and waste water light yellow clear, has reached in line index.Substantially increase the biodegradability of waste water.
Embodiment
For a better understanding of the present invention, the present invention is further illustrated below in conjunction with embodiment.
The synthesis waste liquid of 3,5,6-trichloropyridine-2-sodium alkoxide, be the waste liquid that trichoroacetic chloride one-step synthesis method produces, before pre-treatment, wherein alcohol sodium content is about 5000mg/L, and vinyl cyanide is 100 mg/L, ammonia nitrogen 100 mg/L, and alkalescence, waste liquid is reddish black.
Embodiment 1:
Trichoroacetic chloride one-step synthesis method 3,5,6-trichloropyridine-2-sodium alkoxide waste water 1L, adds 37% hydrochloric acid 27g, places 30min after stirring a little, filters.Potassium permanganate 27.0g is added in filtrate, rapid stirring is caught up with and is reacted 90min except putting into 80 DEG C of water-baths after a large amount of foam, filter, filtrate adds 25g gac, in 1000 milliliters of autoclaves that thermometer, agitator are housed, adds Chlorpyrifos 94 waste water 500mL, 80 DEG C of stirring in water bath 30min, stop stirring, be cooled to room temperature, filter.
It is 0, CN that filtrate records 3,5,6-trichloropyridine-2-sodium alkoxide
-for 0.37mg/L, total manganese is 1.67mg/L, and light yellow clear obtains in line index.
Embodiment 2:
Trichoroacetic chloride one-step synthesis method 3,5,6-trichloropyridine-2-sodium alkoxide waste water 1L, adds 37% hydrochloric acid 27g, places 30min after stirring a little, filters.Potassium permanganate 28.2g is added in filtrate, rapid stirring is caught up with and is reacted 40min except putting into 80 DEG C of water-baths after a large amount of foam, filter, filtrate adds 25g gac, in 1000 milliliters of autoclaves that thermometer, agitator are housed, adds Chlorpyrifos 94 waste water 500mL, 80 DEG C of stirring in water bath 30min, stop stirring, be cooled to room temperature, filter.
It is 0.53, CN that filtrate records 3,5,6-trichloropyridine-2-sodium alkoxide
-for 0.47mg/L, total manganese is 1.87mg/L, obtains in line index.
Embodiment 3:
Trichoroacetic chloride one-step synthesis method 3,5,6-trichloropyridine-2-sodium alkoxide waste water 1L, adds 37% hydrochloric acid 27g, places 30min after stirring a little, filters.Potassium permanganate 29.1g is added in filtrate, rapid stirring is caught up with and is reacted 90min except putting into 40 DEG C of water-baths after a large amount of foam, filter, filtrate adds 25g gac, in 1000 milliliters of autoclaves that thermometer, agitator are housed, adds Chlorpyrifos 94 waste water 500mL, 80 DEG C of stirring in water bath 90min, stop stirring, be cooled to room temperature, filter.
It is 0.59, CN that filtrate records 3,5,6-trichloropyridine-2-sodium alkoxide
-for 0.17mg/L, total manganese is 1.68mg/L, obtains in line index.
Claims (3)
1. the treatment process of the synthesis waste liquid of a trichloropyridine-2-sodium alkoxide, it is characterized in that, it comprises the steps:
(1) in trichloro pyridyl sodium alcoholate synthesis waste liquid 37% concentrated hydrochloric acid adjust ph to 2 ~ 3, after precipitation 30min ~ 60min, filter, reclaim 3,5,6-trichloropyridine-2-sodium alkoxide;
(2) in filtrate, add potassium permanganate rapid stirring, carry out oxidizing reaction 40min ~ 95min, then filter under 40 DEG C ~ 85 DEG C water-baths, described potassium permanganate add-on and the mass ratio of waste water are 2.5% ~ 3%;
(3) add sorbent material in filtrate, at 75 DEG C ~ 85 DEG C, adsorb 20min ~ 40min, be then cooled to room temperature, filter out filter residue.
2. the pretreatment technology of the synthesis waste liquid of a kind of 3,5,6-trichloropyridine-2-sodium alkoxide as claimed in claim 1, it is characterized in that, the synthesis waste liquid of 3,5,6-described trichloropyridine-2-sodium alkoxide, for the waste liquid that trichoroacetic chloride one-step synthesis method produces, wherein alcohol sodium content is about 5000mg/L, and vinyl cyanide is 100 mg/L, ammonia nitrogen 100 mg/L, alkalescence, reddish black.
3. the pretreatment technology of the synthesis waste liquid of a kind of 3,5,6-trichloropyridine-2-sodium alkoxide as claimed in claim 1, it is characterized in that, described sorbent material is activated carbon.
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| CN201410638485.7A CN104447520A (en) | 2014-11-13 | 2014-11-13 | Pretreatment process of synthetic waste liquid of 3,5-6-trichloropyridin-2-ol sodium |
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| CN201410638485.7A CN104447520A (en) | 2014-11-13 | 2014-11-13 | Pretreatment process of synthetic waste liquid of 3,5-6-trichloropyridin-2-ol sodium |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876394A (en) * | 2015-05-13 | 2015-09-02 | 安徽国星生物化学有限公司 | Deep treatment method for wastewater containing 3,5,6-trichloropyridine-2-sodium alcoholate |
| CN105174627A (en) * | 2015-09-21 | 2015-12-23 | 重庆华歌生物化学有限公司 | Method for treating 3,5,6-trichloropyridine-2-sodium alkoxide production waste water |
| CN105481137A (en) * | 2015-12-04 | 2016-04-13 | 安徽国星生物化学有限公司 | Recycling treatment process for wastewater from chlorpyrifos production |
| CN105967312A (en) * | 2015-04-09 | 2016-09-28 | 江苏九九久科技股份有限公司 | 3,5,6-trichloropyridine-2-sodium alcohol wastewater treatment method convenient to operate |
| CN115321707A (en) * | 2022-08-04 | 2022-11-11 | 内蒙古犇星化学有限公司 | Method for treating alkaline hydrolysis wastewater of mother liquor of sodium trichloropyridinol |
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| WO2005070534A1 (en) * | 2004-01-22 | 2005-08-04 | Indian Institute Of Technology | Adsorbent composition, a device and a method for decontaminating water containing pesticides |
| CN102603094A (en) * | 2011-12-14 | 2012-07-25 | 湖北犇星农化有限责任公司 | Method for treating waste water during production of chlorpyrifos |
| CN103771657A (en) * | 2013-12-20 | 2014-05-07 | 安徽国星生物化学有限公司 | Treatment method for chlorpyrifos wastewater |
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2014
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| WO2005070534A1 (en) * | 2004-01-22 | 2005-08-04 | Indian Institute Of Technology | Adsorbent composition, a device and a method for decontaminating water containing pesticides |
| CN102603094A (en) * | 2011-12-14 | 2012-07-25 | 湖北犇星农化有限责任公司 | Method for treating waste water during production of chlorpyrifos |
| CN103771657A (en) * | 2013-12-20 | 2014-05-07 | 安徽国星生物化学有限公司 | Treatment method for chlorpyrifos wastewater |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105967312A (en) * | 2015-04-09 | 2016-09-28 | 江苏九九久科技股份有限公司 | 3,5,6-trichloropyridine-2-sodium alcohol wastewater treatment method convenient to operate |
| CN105967312B (en) * | 2015-04-09 | 2018-10-02 | 江苏九九久科技有限公司 | A kind of processing method of 3,5,6- trichloropyridines -2- sodium alkoxide waste water |
| CN104876394A (en) * | 2015-05-13 | 2015-09-02 | 安徽国星生物化学有限公司 | Deep treatment method for wastewater containing 3,5,6-trichloropyridine-2-sodium alcoholate |
| CN105174627A (en) * | 2015-09-21 | 2015-12-23 | 重庆华歌生物化学有限公司 | Method for treating 3,5,6-trichloropyridine-2-sodium alkoxide production waste water |
| CN105481137A (en) * | 2015-12-04 | 2016-04-13 | 安徽国星生物化学有限公司 | Recycling treatment process for wastewater from chlorpyrifos production |
| CN115321707A (en) * | 2022-08-04 | 2022-11-11 | 内蒙古犇星化学有限公司 | Method for treating alkaline hydrolysis wastewater of mother liquor of sodium trichloropyridinol |
| CN115321707B (en) * | 2022-08-04 | 2023-11-21 | 内蒙古犇星化学有限公司 | Mother liquor alkaline hydrolysis wastewater treatment method of sodium trichloropyridine alkoxide |
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Application publication date: 20150325 |
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