CN103145302A - Pre-treatment process of imidacloprid wastewater - Google Patents
Pre-treatment process of imidacloprid wastewater Download PDFInfo
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- CN103145302A CN103145302A CN2013101031125A CN201310103112A CN103145302A CN 103145302 A CN103145302 A CN 103145302A CN 2013101031125 A CN2013101031125 A CN 2013101031125A CN 201310103112 A CN201310103112 A CN 201310103112A CN 103145302 A CN103145302 A CN 103145302A
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- waste water
- provado
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- imidacloprid
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- 239000002351 wastewater Substances 0.000 title claims abstract description 92
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000002203 pretreatment Methods 0.000 title claims abstract description 14
- 239000005906 Imidacloprid Substances 0.000 title claims abstract description 9
- 229940056881 imidacloprid Drugs 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 title abstract description 26
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 230000003647 oxidation Effects 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 37
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 19
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 17
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 16
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 15
- 229910052698 phosphorus Inorganic materials 0.000 claims description 15
- 239000011574 phosphorus Substances 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- 159000000007 calcium salts Chemical class 0.000 claims description 9
- 239000000920 calcium hydroxide Substances 0.000 claims description 8
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 8
- 239000006260 foam Substances 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 3
- 239000010914 pesticide waste Substances 0.000 claims description 3
- 239000012028 Fenton's reagent Substances 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical group [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000011282 treatment Methods 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 239000000575 pesticide Substances 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 238000006731 degradation reaction Methods 0.000 abstract 1
- 238000007865 diluting Methods 0.000 abstract 1
- 238000005868 electrolysis reaction Methods 0.000 description 5
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- 230000001580 bacterial effect Effects 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 2
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 2
- 210000000481 breast Anatomy 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- -1 reacts 4 hours Substances 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 229910017112 Fe—C Inorganic materials 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000031018 biological processes and functions Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 238000009279 wet oxidation reaction Methods 0.000 description 1
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Abstract
The invention relates to a pre-treatment process of imidacloprid wastewater. The pre-treatment process is characterized by being used for collecting wastewater generated in the production process of the imidacloprid pesticide by classifying, and comprising the following steps of: firstly treating according to quality and then mixing the wastewater to carry out oxidation treatment on account of the characteristics of blasts of wastewater. Due to the pre-treatment process of imidacloprid wastewater, the classified collection of the imidacloprid wastewater, quality-distinguishing efficient pre-treatment, strong pertinence and good treatment effect can be realized, the concentration of degradation-resistant organic matters is greatly reduced, the biodegradability of the wastewater is improved and the economical efficiency is improved; the pre-treatment process has the advantages of being wild in reaction condition, simple to operate, good in treatment effect and low in operation cost; and the pre-treatment process of imidacloprid wastewater disclosed by the invention can be used for overcoming the defects of high reaction condition requirement, unstable water quality and the need of great amount of water for diluting after pre-treating of the existing pre-treatment method of the imidacloprid wastewater.
Description
Technical field
The present invention relates to a kind of pretreatment technology of Provado waste water, especially relate to the pretreatment technology that a kind of Provado waste water divides qualitative classification.
Background technology
Provado is a kind of novel nitro-methylene-type systemic insecticide, as Pesticidal products of new generation, yet has good market outlook. the processing problem of pesticide wastewater is a great problem of puzzlement enterprise always.Because waste water quality is complicated, organic concentration is high, hardly degraded organic substance is many, toxicity is large, and biodegradability is poor, adopts conventional process, and waste water can't reach emission standard at all, and environment is caused ill effect.
Organic pesticide wastewater treatment difficulty is large, and cost is high, is difficult to reach the emission standard of country always, is the bottleneck of restriction pesticide industry develop rapidly.The treatment process of organic pesticide waste water has a lot, because its biochemical is poor, is all generally to adopt materialization to process to improve its biochemical, then carries out biochemical treatment process.
Materilization freatment method commonly used has calcium salt precipitation method, distillation method, catalytic oxidation, wet oxidation process etc.General is all to remove inorganic phosphorus in water with calcium salt precipitation method after several strands of Provado waste water are mixed, and then utilizes organic content in oxidation style reduction water, improves its biochemical.Do not carry out respectively pre-treatment for the characteristic of each strand waste water, processing cost is high, and poor processing effect.
The toxicity of Provado waste water is large, and biochemical is poor, needs extension rate large before biochemistry, has wasted a large amount of water resourcess.High to the bacterial classification requirement in biological process, need to carry out the screening of bacterial classification.Waste water after biochemistry often can not reach emission standard, still needs a large amount of water to dilute, and makes Provado manufacturer that headache is more than always.
Patent CN102040318A adopts chemical dephosphorization, the little electrolysis of Fe-C, fenton oxidation and catalyzed oxidation, then cultivates dominant bacteria and carries out biochemical treatment process.Oxidation together after each strand waste water mixes does not have specific aim, poor processing effect, and catalyzed oxidation is high to equipment requirements, and processing cost is large.Pretreated wastewater biochemical difficulty is large, also needs to do the extensive works such as bacterial screening, cultivation.Above-mentioned deficiency still has is worth improved place.
Summary of the invention
The objective of the invention is in order to overcome existing Provado preconditioning technique processing cost highly, reaction conditions requires high, and biochemical water inlet extension rate is large, processing is difficult to shortcoming up to standard, and a kind of processing efficiency that provides is high, and cost is low, the pretreatment technology of the simple Provado waste water of equipment requirements.Get rid of most COD through the pretreated Provado waste water of the present invention, greatly reduced biochemical toxicity, improved biochemical, reached the requirement of follow-up biochemical B/C ratio.
The technology used in the present invention solution is: a kind of pretreatment technology of Provado waste water, and its concrete steps are as follows:
(1) imidacloprid pesticide waste water being divided into three classes by its production workshop section collects: be respectively Provado high phosphorus waste water, the high DMF waste water of Provado, other strands of Provado waste water;
(2) pre-treatment of Provado high phosphorus waste water: add calcium salt in Provado high phosphorus waste water, after regulating the pH to 7 of waste water～8 with alkali lye, filter out the residue of generation; Then the pH to 5 of waste water～6 are regulated in acid, regulate pressure to 0.03MPa～0.06MPa with vacuum pump, carry out underpressure distillation, obtain to heat up in a steamer rear liquid and be for further processing;
(3) pre-treatment of the high DMF waste water of Provado: regulate the pH to 11 of the high DMF waste water of Provado～12 with alkali lye, after 2～4 hours, the quiescent setting filtration obtains filtrate being for further processing with 60～80 degree heating in water bath;
(4) learn from else's experience step (2) and (3) waste water after processing with after other strands of Provado waste water mixes, with acid for adjusting pH to 3～5, carry out the combination oxidation of little electrolysis-Fenton, then regulate pH to 8～9 with alkali lye, sedimentation and filtration obtains pretreated Provado waste water.Get filtrate and carry out follow-up biochemical treatment.Waste water after process step (2) and (3) and other strands of Provado waste water generally by every day each strand waste water output all handle and mix.
The calcium salt that adds in preferred steps (2) is the calcium carbonate solid; Calcium salt add quality with 80～100g/L of the volume of Provado high phosphorus waste water; Alkali lye described in step (2) is milk of lime or caustic soda; Acid described in step (2) is hydrochloric acid.
Alkali lye in preferred steps (3) is milk of lime or caustic soda, and heat-processed needs to stir, and needs suitable additional alkali lye to keep the alkaline level of waste water.Acid described in preferred steps (4) is hydrochloric acid or sulfuric acid.
The combination of preferred little electrolysis-Fenton is oxidized to first carries out little electrolytic oxidation reaction, then carries out the Fenton oxidation reaction; What little electrolytic oxidation reaction adopted is foam iron, and wherein the dosage of foam iron is 5%～10% of wastewater quality; 2～4 hours time of little electrolytic oxidation reaction; Fenton oxidation reaction Fenton reagent is ferrous sulfate and hydrogen peroxide, wherein Fe
2+/ H
2O
2Mol ratio be 1:(5～10), the dosage of hydrogen peroxide is for take the volume ratio of the hydrogen peroxide of mass concentration 30% and waste water as 0.3%～0.5%; 2～4 hours Fenton oxidation reaction times.
Beneficial effect:
1. divide qualitative classification to carry out pre-treatment to Provado waste water, with strong points, treatment effect is good, has very effectively reduced COD, the bio-toxicity of waste water, has improved the biochemical of waste water.
2. first add calcium carbonate to what Provado high phosphorus waste water adopted, after add the calcium salt precipitation method of milk of lime, greatly saved the dosage of milk of lime, reduced the possibility of milk of lime blocking pipe.
3. adopt distillation under vacuum to process Provado high phosphorus waste water, not only effectively reduced COD, also subsidiary ammonia nitrogen, the salinity of having reduced.
4. adopt the alkaline water solution to process high DMF waste water with strong points, treatment effect is good, has greatly reduced the bio-toxicity of waste water, has alleviated the load of follow-up biochemistry.
5. adopt foam iron to do the material of micro-electrolysis reaction, because foam iron has very large specific surface area, and the contact area of waste water is large, reacts more complete, better effects if.
6. little electrolysis-Fenton combination oxidation is better to water treatment effect, and both reaction conditionss are similar, can directly carry out the latter reaction after the former reaction.Ferrous ion after micro-electrolysis reaction in water has also raise much, and this has just reduced ferrous dosage in Fenton's reaction, has further saved processing cost.
Description of drawings
Fig. 1 is process flow diagram of the present invention.
Embodiment
The process flow sheet of following examples is as shown in Figure 1:
Embodiment 1
Yancheng agricultural chemicals producer Provado factory effluent:
(1) the Provado factory effluent is divided into three strands by production technique, is respectively Provado high phosphorus waste water, the high DMF waste water of Provado, other strands of Provado waste water.First add calcium carbonate 90g/L toward high phosphorus waste water.The feeding lime breast is regulated pH to 7 again, after quiescent setting, gets supernatant liquor.Regulate waste water to pH to 5 with hydrochloric acid, regulate vacuum tightness, distill under pressure 0.03MPa, obtain and heat up in a steamer rear liquid.The COD of this moment is down to 24440mg/L by the 107000mg/L of water inlet.
(2) regulate the pH to 11 of high DMF waste water with milk of lime, 60 degree water-bath alkaline hydrolysis are after 2 hours, COD by the 54700mg/L of water inlet to 33110mg/L.
(3) after the waste water after (1) (2) are processed and remaining waste water mix, sulphur acid for adjusting pH to 3 is arranged, add the foam iron of wastewater quality mark 10%, reacted 3 hours.The COD of waste water drops to 18940mg/L by mixed 26500mg/L.
(4) get waste water after little electrolysis, according to Fe
2+/ H
2O
2Mol ratio be the ratio of 1:5, the hydrogen peroxide that adds 30% massfraction is 5ml/L with the volume ratio of waste water, reacts 4 hours, waste water COD is down to 7200mg/L, the B/C ratio reaches 0.48.
Before and after the 1 Provado wastewater treatment of table 1 example, water-quality guideline changes contrast
Embodiment 2
Yangzhou agricultural chemicals producer Provado factory effluent:
(1) the Provado factory effluent is divided into three strands by production technique, one is high phosphorus waste water, first adds calcium carbonate 80g/L toward high phosphorus waste water.The feeding lime breast is regulated pH to 8 again, after quiescent setting, gets supernatant liquor.Regulate waste water to pH to 6 with hydrochloric acid, regulate vacuum tightness, distill under vacuum tightness 0.04MPa, obtain and heat up in a steamer rear liquid.The COD of this moment is down to 16440mg/L by the 90000mg/L of water inlet.
(2) regulate the pH to 12 of high DMF waste water with the stone caustic soda, 70 degree water-bath alkaline hydrolysis are after 3.5 hours, COD by the 36700mg/L of water inlet to 18240mg/L.
(3) after the waste water after (1) (2) are processed and remaining waste water mix, salt acid for adjusting pH to 2 is arranged, add the foam iron of wastewater quality mark 5%, reacted 2 hours.The COD of waste water drops to 11460mg/L by mixed 17700mg/L.
(4) getting waste water after little electrolysis, is the ratio of 1:10 according to the mol ratio of Fe2+/H2O2, and the hydrogen peroxide that adds 30% massfraction is 3ml/L with the volume ratio of waste water, reacts 3 hours, and waste water COD is down to 5400mg/L, and the B/C ratio reaches 0.53.
Before and after the 2 Provado wastewater treatments of table 2 example, water-quality guideline changes contrast
Above-described embodiment is two embodiment of the present invention, but embodiments of the present invention are not restricted to the described embodiments, and does not anyly deviate from change, the modification that above-mentioned treatment process essence is made, within all belonging to the protection domain of this patent.
Claims (5)
1. the pretreatment technology of a Provado waste water, its concrete steps are as follows:
(1) imidacloprid pesticide waste water being divided into respectively three classes by its production workshop section collects: Provado high phosphorus waste water, the high DMF waste water of Provado, other waste water of Provado;
(2) pre-treatment of Provado high phosphorus waste water: add calcium salt in Provado high phosphorus waste water, after regulating the pH to 7 of waste water～8 with alkali lye, filter out the residue of generation; Then the pH to 5 of waste water～6 are regulated in acid, regulate pressure to 0.03MPa～0.06MPa with vacuum pump, carry out underpressure distillation, obtain to heat up in a steamer rear liquid and be for further processing;
(3) pre-treatment of the high DMF waste water of Provado: regulate the pH to 11 of the high DMF waste water of Provado～12 with alkali lye, after 2～4 hours, the quiescent setting filtration obtains filtrate being for further processing with 60～80 degree heating in water bath;
(4) learn from else's experience after step (2) and (3) other waste water of waste water and Provado after processing mix, with acid for adjusting pH to 3～5, carry out the combination oxidation of little electrolysis-Fenton, then regulate pH to 8～9 with alkali lye, sedimentation and filtration obtains pretreated Provado waste water.
2. pretreatment technology according to claim 1, is characterized in that the calcium salt that adds in step (2) is the calcium carbonate solid; Calcium salt add quality with 80～100g/L of the volume of Provado high phosphorus waste water; Alkali lye described in step (2) is milk of lime or caustic soda; Acid described in step (2) is hydrochloric acid.
3. pretreatment technology according to claim 1, is characterized in that the alkali lye in step (3) is milk of lime or caustic soda.
4. pretreatment technology according to claim 1, is characterized in that the acid described in step (4) is hydrochloric acid or sulfuric acid.
5. pretreatment technology according to claim 1, the combination that it is characterized in that little electrolysis-Fenton is oxidized to first carries out little electrolytic oxidation reaction, then carries out the Fenton oxidation reaction; What little electrolytic oxidation reaction adopted is foam iron, and wherein the dosage of foam iron is 5%～10% of wastewater quality; 2～4 hours time of little electrolytic oxidation reaction; In the Fenton oxidation reaction, Fenton reagent is ferrous sulfate and hydrogen peroxide, wherein Fe
2+/ H
2O
2Mol ratio be 1:(5～10), the dosage of hydrogen peroxide is for take the volume ratio of the hydrogen peroxide of mass concentration 30% and waste water as 0.3%～0.5%; 2～4 hours Fenton oxidation reaction times.
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| CN2013101031125A CN103145302A (en) | 2013-03-27 | 2013-03-27 | Pre-treatment process of imidacloprid wastewater |
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| CN2013101031125A CN103145302A (en) | 2013-03-27 | 2013-03-27 | Pre-treatment process of imidacloprid wastewater |
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| CN103145302A true CN103145302A (en) | 2013-06-12 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105000759A (en) * | 2015-08-05 | 2015-10-28 | 丁德凤 | Imidacloprid waste water treating technology |
| CN105198175A (en) * | 2015-10-29 | 2015-12-30 | 广东省工程技术研究所 | Treatment method of dimethoate pesticide production wastewater |
| CN106167481A (en) * | 2016-07-11 | 2016-11-30 | 河北威远生化农药有限公司 | A kind of production method of imidacloprid synthesis technique wastewater zero discharge |
| CN106277630A (en) * | 2016-08-31 | 2017-01-04 | 江苏省农垦生物化学有限公司 | High skilful production waste decoloration treatment method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105000759A (en) * | 2015-08-05 | 2015-10-28 | 丁德凤 | Imidacloprid waste water treating technology |
| CN105198175A (en) * | 2015-10-29 | 2015-12-30 | 广东省工程技术研究所 | Treatment method of dimethoate pesticide production wastewater |
| CN106167481A (en) * | 2016-07-11 | 2016-11-30 | 河北威远生化农药有限公司 | A kind of production method of imidacloprid synthesis technique wastewater zero discharge |
| CN106167481B (en) * | 2016-07-11 | 2018-12-25 | 河北威远生物化工有限公司 | A kind of production method of imidacloprid synthesis technology wastewater zero discharge |
| CN106277630A (en) * | 2016-08-31 | 2017-01-04 | 江苏省农垦生物化学有限公司 | High skilful production waste decoloration treatment method |
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Application publication date: 20130612 |