CN103922507B - A kind of method adopting complexometric extraction process TDA waste water - Google Patents
A kind of method adopting complexometric extraction process TDA waste water Download PDFInfo
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- 238000000605 extraction Methods 0.000 title claims abstract description 108
- 239000002351 wastewater Substances 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 53
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 55
- 239000002253 acid Substances 0.000 claims abstract description 27
- 239000008139 complexing agent Substances 0.000 claims abstract description 23
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 20
- 239000011707 mineral Substances 0.000 claims abstract description 20
- 239000000284 extract Substances 0.000 claims abstract description 17
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- 230000008929 regeneration Effects 0.000 claims abstract description 13
- 238000011069 regeneration method Methods 0.000 claims abstract description 13
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- SJWFXCIHNDVPSH-UHFFFAOYSA-N octan-2-ol Chemical compound CCCCCCC(C)O SJWFXCIHNDVPSH-UHFFFAOYSA-N 0.000 claims abstract description 9
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims abstract description 8
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims abstract description 8
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000002699 waste material Substances 0.000 claims description 8
- FIHFWXNMOWDPBM-UHFFFAOYSA-N 2,4,4-trimethylpentylphosphonic acid Chemical class CC(C)(C)CC(C)CP(O)(O)=O FIHFWXNMOWDPBM-UHFFFAOYSA-N 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 6
- VOZKAJLKRJDJLL-UHFFFAOYSA-N 2,4-diaminotoluene Chemical compound CC1=CC=C(N)C=C1N VOZKAJLKRJDJLL-UHFFFAOYSA-N 0.000 abstract description 3
- 150000003009 phosphonic acids Chemical class 0.000 abstract description 3
- 230000000536 complexating effect Effects 0.000 abstract description 2
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- 238000002360 preparation method Methods 0.000 abstract 1
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
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- HGXVKAPCSIXGAK-UHFFFAOYSA-N 2,4-diethyl-6-methylbenzene-1,3-diamine;4,6-diethyl-2-methylbenzene-1,3-diamine Chemical compound CCC1=CC(CC)=C(N)C(C)=C1N.CCC1=CC(C)=C(N)C(CC)=C1N HGXVKAPCSIXGAK-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
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- 239000004721 Polyphenylene oxide Substances 0.000 description 1
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Abstract
The present invention is a kind of method adopting complexometric extraction process 2,4 di amino toluene (TDA) waste water, it is characterized in that: the method mainly comprises pH value and regulates, extracts and extractant regeneration treatment process.The present invention is with 2-ethylhexyl phosphonic acid-2-(ethyl hexyl) ester, two (2,4,4-tri-methyl-amyl) one or both are complexing agent in phosphonic acids, one or more of n-Octanol, isooctyl alcohol, sec-octyl alcohol are solubility promoter, kerosene or hexanaphthene are thinner, preparation complexing extractant is separated difficult biochemical TDA compound in waste water, and extraction agent is reused after adopting mineral acid regeneration.Present invention process advantages of simple, workable, easy to operate, processing cost is low.Waste water TDA concentration after present invention process process significantly reduces, and TDA one-level extraction clearance 95 ~ 99%, is with a wide range of applications.
Description
Technical field
The invention belongs to technical field of waste water processing, relate to a kind of method adopting complexometric extraction process TDA waste water.
Background technology
TDA chemical name 2,4 di amino toluene is light yellow solid under normal temperature, and standing storage or exposure can become intense violet color or black in atmosphere, have ammonia odor.TDA is mainly used in the raw material and the polyether initiator that synthesize tolylene diisocyanate (TDI), and it can also be used as epoxy curing agent, dyestuff intermediate.Meanwhile, also can synthesize the aromatic diamine curing agent for polyurethane elastomer and epoxy resin, as dimethythiotoluene diamine DMTDA, diethyltoluene two ammonium DETDA.
TDA waste water belongs to the toxic organic pollutant waste water of difficult degradation, due to the toxicity that it is stronger, in process containing in the Practical Project of this material waste water, is difficult to obtain gratifying removal effect by the technique of routine or bioremediation.At present, there is no, effective means ripe to TDA wastewater treatment both at home and abroad.For the process of TDA waste water, the research reported comprises (1) weak electrolysis mechanism; (2) Ozonation; (3) Fenton oxidation method.These methods are all destroy TDA organic constitution by chemical reaction, make it be converted into the small organic molecule of easily degraded, improve the biodegradability of waste water, reach the object of wastewater treatment.But it is relatively high to carry out oxide treatment cost for the waste water containing high density TDA.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, a kind of method of new complexing abstraction process TDA waste water is proposed, Coal Gas Washing Cycling Water, difficult biochemical, that toxicity is large TDA are separated by the mode of two-phase laminated flow, reach the object that contaminated wastewater controls, make the waste water after process meet biochemical processing process requirement.
Technical problem to be solved by this invention is achieved through the following technical solutions.The present invention is a kind of method adopting complexometric extraction process TDA waste water, is characterized in: its step is as follows:
(1) pH value regulates: regulate TDA waste water ph to 7 ~ 10 with mineral acid;
(2) extract: be 4:1 ~ 1:8 by volume by extraction agent and waste water, at temperature 0 ~ 60 DEG C, be uniformly mixed 5 ~ 60min, standing 20 ~ 120min layering, upper strata is loaded extractant, and lower floor is the waste water after extraction treatment;
Extract the extraction agent adopted and comprise complexing agent, or at least one ratio on demand added again in solubility promoter, thinner mixes; Described complexing agent to be selected from 2-ethylhexyl phosphonic acid-2-(ethyl hexyl) ester, two (2,4,4-tri-methyl-amyl) phosphonic acids one or both; Described solubility promoter is selected from one or more in n-Octanol, isooctyl alcohol, sec-octyl alcohol; Described thinner is selected from kerosene or hexanaphthene.
In the method for a kind of complexometric extraction process TDA waste water of the present invention, preferred technical scheme or technical characteristic are further:
1. can also carry out reextraction regeneration by the following method after step (2) extraction terminates: loaded extractant and reverse-extraction agent are 20:1 ~ 1:2 by volume, 5 ~ 60min is uniformly mixed at temperature 0 ~ 80 DEG C, leave standstill 20 ~ 120min layering, upper strata is the extraction agent regenerated of stripping, and recycles; Lower floor is concentrated pollutent waste liquid; Described reverse-extraction agent is mineral acid; Described mineral acid can for disclosed in prior art, any one is applicable to conventional mineral acid of the present invention, particularly preferably 10% ~ 31% hydrochloric acid or 10% ~ 98% sulfuric acid.
2. extract the extraction agent that adopts in step (2) by complexing agent and thinner or add solubility promoter again and form.
3. the mineral acid described in step (1) for disclosed in prior art, any one is applicable to conventional mineral acid of the present invention, can be particularly preferably 10% ~ 31% hydrochloric acid or 10% ~ 98% sulfuric acid.
When 4, stripping, the volume ratio of loaded extractant and hydrochloric acid or sulfuric acid is preferably 5:1 ~ 10:1, and acid strength is preferably 10% ~ 30%, and reextraction temperature is preferably 20 ~ 40 DEG C; Loaded extractant and acid solution mixing time are preferably 10 ~ 20min, and after mixing, separation time is preferably 30 ~ 40min.
In the present invention, after extraction tower layering, supernatant liquor loaded extractant drains into extractant regeneration system, lower floor's waste water is delivered to waste water processing station after discharging and carrying out Two-step neutralization to neutrality and carried out biochemical treatment.In back extraction tower loaded extractant, extraction agent and pollutent carry out separation regeneration, and extraction workshop section sent continuously back to by the extraction agent of regeneration, and the concentrated remaining recyclable wherein TDA of liquid of pollutent back extraction also can mix coal-fired boiler combustion process or coal-fired thermal oil furnace burn processing.
In the present invention, TDA is typical lewis alkaline matter, Lewis acidic extractant is adopted to carry out complexometric extraction, the partition ratio of TDA in extraction agent can be improved, waste water is made to reach the object of extracting and separating, adopt the method for complexometric extraction to be expected to the TDA in waste water to separate, reach the object of wastewater treatment.
Compared with prior art, present invention process advantages of simple, workable, easy to operate, processing cost is low.Waste water TDA concentration after present invention process process significantly reduces, and TDA one-level extraction clearance 95 ~ 99%, is with a wide range of applications.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Referring to accompanying drawing, further describe concrete technical scheme of the present invention, so that those skilled in the art understands the present invention further, and do not form the restriction to its right.
Embodiment 1, a kind of method adopting complexometric extraction process TDA waste water, its step is as follows:
(1) pH value regulates: regulate TDA waste water ph to 7 with mineral acid;
(2) extract: be 4:1 by volume by extraction agent and waste water, at temperature 0 ~ 10 DEG C, be uniformly mixed 5 ~ 60min, standing 20 ~ 120min layering, upper strata is loaded extractant, and lower floor is the waste water after extraction treatment;
Extract the extraction agent that adopts and comprise complexing agent, described complexing agent to be selected from 2-ethylhexyl phosphonic acid-2-(ethyl hexyl) ester, two (2,4,4-tri-methyl-amyl) phosphonic acids one or both.
Embodiment 2, a kind of method adopting complexometric extraction process TDA waste water, its step is as follows:
(1) pH value regulates: regulate TDA waste water ph to 10 with mineral acid;
(2) extract: be 1:8 by volume by extraction agent and waste water, at temperature 10 ~ 20 DEG C, be uniformly mixed 5 ~ 60min, standing 20 ~ 120min layering, upper strata is loaded extractant, and lower floor is the waste water after extraction treatment;
Extract the extraction agent adopted and comprise complexing agent, then add the one in solubility promoter, thinner, ratio on demand mixes; Described complexing agent to be selected from 2-ethylhexyl phosphonic acid-2-(ethyl hexyl) ester, two (2,4,4-tri-methyl-amyl) phosphonic acids one or both; Described solubility promoter is selected from one or more in n-Octanol, isooctyl alcohol, sec-octyl alcohol; Described thinner is selected from kerosene or hexanaphthene.
Embodiment 3, a kind of method adopting complexometric extraction process TDA waste water, its step is as follows:
(1) pH value regulates: regulate TDA waste water ph to 8 ~ 9 with mineral acid;
(2) extract: be 4:1 ~ 1:8 by volume by extraction agent and waste water, at temperature 20 ~ 30 DEG C, be uniformly mixed 5 ~ 60min, standing 20 ~ 120min layering, upper strata is loaded extractant, and lower floor is the waste water after extraction treatment;
Extract the extraction agent adopted and comprise complexing agent, then add solubility promoter, thinner, ratio on demand mixes; Described complexing agent to be selected from 2-ethylhexyl phosphonic acid-2-(ethyl hexyl) ester, two (2,4,4-tri-methyl-amyl) phosphonic acids one or both; Described solubility promoter is selected from one or more in n-Octanol, isooctyl alcohol, sec-octyl alcohol; Described thinner is selected from kerosene or hexanaphthene.
Embodiment 4, a kind of method adopting complexometric extraction process TDA waste water, its step is as follows:
(1) pH value regulates: regulate TDA waste water ph to 8 with mineral acid;
(2) extract: be 1:1 by volume by extraction agent and waste water, at temperature 40 ~ 50 DEG C, be uniformly mixed 5 ~ 60min, standing 20 ~ 120min layering, upper strata is loaded extractant, and lower floor is the waste water after extraction treatment;
Extract the extraction agent adopted and comprise complexing agent, or at least one ratio on demand added again in solubility promoter, thinner mixes; Described complexing agent to be selected from 2-ethylhexyl phosphonic acid-2-(ethyl hexyl) ester, two (2,4,4-tri-methyl-amyl) phosphonic acids one or both; Described solubility promoter is selected from one or more in n-Octanol, isooctyl alcohol, sec-octyl alcohol; Described thinner is selected from kerosene or hexanaphthene.
Embodiment 5, in the method for a kind of complexometric extraction process TDA waste water of embodiment 1-4 described in any one: carry out reextractions regeneration by the following method after step (2) extraction terminates: loaded extractant and reverse-extraction agent are 20:1 by volume, 5 ~ 60min is uniformly mixed at temperature 0 ~ 10 DEG C, leave standstill 20 ~ 120min layering, upper strata is the extraction agent regenerated of stripping, and recycles; Lower floor is concentrated pollutent waste liquid; Described reverse-extraction agent is mineral acid.
Embodiment 6, in the method for a kind of complexometric extraction process TDA waste water of embodiment 1-4 described in any one: carry out reextractions regeneration by the following method after step (2) extraction terminates: loaded extractant and reverse-extraction agent are 1:2 by volume, 5 ~ 60min is uniformly mixed at temperature 10 ~ 30 DEG C, leave standstill 20 ~ 120min layering, upper strata is the extraction agent regenerated of stripping, and recycles; Lower floor is concentrated pollutent waste liquid; Described reverse-extraction agent is mineral acid.
Embodiment 7, in the method for a kind of complexometric extraction process TDA waste water of embodiment 1-4 described in any one: carry out reextractions by the following method and regenerate after step (2) extraction terminates: loaded extractant and reverse-extraction agent are 10 ~ 1 by volume, 5 ~ 60min is uniformly mixed at temperature 20 ~ 40 DEG C, leave standstill 20 ~ 120min layering, upper strata is the extraction agent regenerated of stripping, and recycles; Lower floor is concentrated pollutent waste liquid; Described reverse-extraction agent is mineral acid.Acid strength is 10% ~ 30%.
Embodiment 8, in the method for a kind of complexometric extraction process TDA waste water of embodiment 1-4 described in any one: carry out reextractions regeneration by the following method after step (2) extraction terminates: loaded extractant and reverse-extraction agent are 5:1 by volume, 5 ~ 60min is uniformly mixed at temperature 30 ~ 50 DEG C, leave standstill 20 ~ 120min layering, upper strata is the extraction agent regenerated of stripping, and recycles; Lower floor is concentrated pollutent waste liquid; Described reverse-extraction agent is mineral acid.
Embodiment 9, in the method for a kind of complexometric extraction process TDA waste water in embodiment 5-8 described in any one: loaded extractant and acid solution mixing time are 10 ~ 20min, after mixing, separation time is 30 ~ 40min.
Embodiment 10, in the method for a kind of complexometric extraction process TDA waste water in embodiment 5-9 described in any one: described reverse-extraction agent is 10% ~ 31% hydrochloric acid or 10% ~ 98% sulfuric acid.
Embodiment 11, in the method for a kind of complexometric extraction process TDA waste water in embodiment 1-10 described in any one: the mineral acid described in step (1) is 10% ~ 31% hydrochloric acid or 10% ~ 98% sulfuric acid.
Embodiment 12, a kind of method of complexometric extraction process TDA waste water, its step is as follows:
(1) pH value regulates, and regulates TDA waste water ph to 7 with hydrochloric acid;
(2) extract, be 4:1 by volume, at temperature 0 DEG C, be uniformly mixed 5min by extraction agent and waste water, leave standstill 20min layering, upper strata is loaded extractant, and lower floor is the waste water after extraction treatment;
(3) reextraction regeneration, loaded extractant and reverse-extraction agent are 20:1 by volume, and reverse-extraction agent is mass percentage concentration 40% sulfuric acid, at temperature 0 DEG C, be uniformly mixed 5min, leave standstill 20min layering, and upper strata is the extraction agent regenerated of stripping, and recycles; Lower floor is concentrated pollutent waste liquid.
Described extraction agent is with 2-ethylhexyl phosphonic acid-2-(ethyl hexyl) ester, two (2,4,4-tri-methyl-amyl) one or both are complexing agent in phosphonic acids, one or more of n-Octanol, isooctyl alcohol, sec-octyl alcohol are solubility promoter, kerosene or hexanaphthene are thinner, complexing agent, solubility promoter, thinner can be mixed by different ratios and combination, as complexing agent+thinner or complexing agent+solubility promoter+thinner;
Embodiment 13, a kind of method of complexometric extraction process TDA waste water, its step is as follows:
(1) pH value regulates, and regulates TDA waste water ph to 10 with mineral acid;
(2) extract, be 1:8 by volume, under temperature 60 C, be uniformly mixed 60min by extraction agent and waste water, leave standstill 120min layering, upper strata is loaded extractant, and lower floor is the waste water after extraction treatment;
(3) reextraction regeneration, loaded extractant and reverse-extraction agent are 1:2 by volume, and reverse-extraction agent is mass percentage concentration 10% sulfuric acid, at temperature 80 DEG C, be uniformly mixed 60min, leave standstill 120min layering, and upper strata is the extraction agent regenerated of stripping, and recycles; Lower floor is concentrated pollutent waste liquid.
Described extraction agent is with 2-ethylhexyl phosphonic acid-2-(ethyl hexyl) ester, two (2,4,4-tri-methyl-amyl) one or both are complexing agent in phosphonic acids, one or more of n-Octanol, isooctyl alcohol, sec-octyl alcohol are solubility promoter, kerosene or hexanaphthene are thinner, complexing agent, solubility promoter, thinner can be mixed by different ratios and combination, as complexing agent+thinner or complexing agent+solubility promoter+thinner;
Embodiment 14, a kind of complexometric extraction process TDA waste water experiment:
Certain 2,4 di amino toluene (TDA) manufacturing enterprise, high concentrated organic wastewater 2000m3 discharges every day in production workshop section of enterprise, waste water TDA concentration 1545mg/L, water outlet TDA concentration 21mg/L after the extraction of following steps one-level, phenyl amines organic removal rate 98.6%.
(1) first pH value adjustment is carried out to waste water, regulate waste water ph to 8 with hydrochloric acid;
(2) adopt extraction process to process, extracting the extraction agent adopted is volumetric concentration 20%2-ethylhexyl phosphonic acids-2-(ethyl hexyl) ester+40% two (2,4,4-tri-methyl-amyl) phosphonic acids+5% sec-octyl alcohol+35% kerosene; During extraction, the volume ratio of extraction agent and waste water is 1:1, and extraction temperature is 25 DEG C; Layering in extraction tower after extraction agent and waste water are uniformly mixed; Extraction agent and waste water mixing time are 5min; Separation time 20min after extraction agent mixes with waste water; Upper strata is loaded extractant, and lower floor is pretreated waste water;
(3) anti-extraction process is adopted to process; In loaded extractant, hydrochloric acid is added during reextraction; The volume ratio of loaded extractant and hydrochloric acid is 20:1, and concentration of hydrochloric acid is 15%, and reextraction temperature is 25 DEG C; Layering in stripping column after loaded extractant and acid solution are uniformly mixed, reextraction mixing time is 5min, separation time 20min after mixing; Strip pollutent disengaging in loaded extractant, make extractant regeneration, recycle.
Claims (7)
1. adopt a method for complexometric extraction process TDA waste water, it is characterized in that: its step is as follows:
(1) pH value regulates: regulate TDA waste water ph to 7 ~ 10 with mineral acid;
(2) extract: be 4:1 ~ 1:8 by volume by extraction agent and waste water, at temperature 0 ~ 60 DEG C, be uniformly mixed 5 ~ 60min, standing 20 ~ 120min layering, upper strata is loaded extractant, and lower floor is the waste water after extraction treatment;
Extract the extraction agent adopted and comprise complexing agent, then at least one ratio on demand added in solubility promoter, thinner mixes; Described complexing agent to be selected from 2-ethylhexyl phosphonic acid-2-(ethyl hexyl) ester, two (2,4,4-tri-methyl-amyl) phosphonic acids one or both; Described solubility promoter is selected from one or more in n-Octanol, isooctyl alcohol, sec-octyl alcohol; Described thinner is selected from kerosene or hexanaphthene.
2. a kind of method adopting complexometric extraction process TDA waste water according to claim 1, it is characterized in that: after step (2) extraction terminates, carry out reextraction regeneration by the following method: loaded extractant and reverse-extraction agent are 20:1 ~ 1:2 by volume, 5 ~ 60min is uniformly mixed at temperature 0 ~ 80 DEG C, leave standstill 20 ~ 120min layering, upper strata is the extraction agent regenerated of stripping, and recycles; Lower floor is concentrated pollutent waste liquid; Described reverse-extraction agent is mineral acid.
3. a kind of method adopting complexometric extraction process TDA waste water according to claim 2, it is characterized in that: during reextraction, the volume ratio of loaded extractant and hydrochloric acid or sulfuric acid is 5:1 ~ 10:1, and acid strength is 10% ~ 30%, and reextraction temperature is 20 ~ 40 DEG C.
4. a kind of method adopting complexometric extraction process TDA waste water according to Claims 2 or 3, is characterized in that: loaded extractant and acid solution mixing time are 10 ~ 20min, and after mixing, separation time is 30 ~ 40min.
5. a kind of method adopting complexometric extraction process TDA waste water according to claim 2, is characterized in that: described reverse-extraction agent is 10% ~ 31% hydrochloric acid or 10% ~ 98% sulfuric acid.
6. a kind of method adopting complexometric extraction process TDA waste water according to claim 1 or 2 or 3 or 5, is characterized in that: extract the extraction agent adopted in step (2) and add solubility promoter again by complexing agent and thinner and form.
7. a kind of method adopting complexometric extraction process TDA waste water according to claim 1 or 2 or 3 or 5, is characterized in that: the mineral acid described in step (1) is 10% ~ 31% hydrochloric acid or 10% ~ 98% sulfuric acid.
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| CN104211132B (en) * | 2014-09-05 | 2016-02-03 | 广东溢达纺织有限公司 | A kind of method of extraction agent and process reactive dyed wastewater |
| CN105417814A (en) * | 2015-11-06 | 2016-03-23 | 南京师范大学 | Method for treating wastewater with nitrogen-containing organic matters in pymetrozine production procedures |
| CN111072120A (en) * | 2018-10-19 | 2020-04-28 | 上海申英环保科技有限公司 | O-aminobenzene and m-aminobenzene wastewater treatment agent and wastewater treatment method |
| CN110981866B (en) * | 2019-12-17 | 2022-08-12 | 邯郸市瑞田农药有限公司 | Thiamethoxam production method and extracting agent |
| CN112479495A (en) * | 2020-11-20 | 2021-03-12 | 青岛凤凰东翔印染有限公司 | Wax printing thick slurry wastewater treatment method |
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| GB831745A (en) * | 1956-08-09 | 1960-03-30 | Little Inc A | Process for the recovery of dissolved metal values |
| CN1289725A (en) * | 2000-10-13 | 2001-04-04 | 清华大学 | Process for pre-treating waste liquid of p-benzoic acid by complexing and extraction |
| CN103601328A (en) * | 2013-10-15 | 2014-02-26 | 内蒙古常盛制药有限公司 | Process for 6-APA or 7-ADCA production waste water recycling resource and biochemistry pretreatment |
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| CN103922507A (en) | 2014-07-16 |
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