CN1024460C - Process for wastewater treatment and the recovery of 0-phenylenediamine - Google Patents
Process for wastewater treatment and the recovery of 0-phenylenediamine Download PDFInfo
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- CN1024460C CN1024460C CN 89104014 CN89104014A CN1024460C CN 1024460 C CN1024460 C CN 1024460C CN 89104014 CN89104014 CN 89104014 CN 89104014 A CN89104014 A CN 89104014A CN 1024460 C CN1024460 C CN 1024460C
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- waste water
- phenylene diamine
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Abstract
The present invention relates to a method for treating waste water and recovering 0-phenylenediamine, which is a new technology capable of realizing the combination of waste water treatment and comprehensive utilization. The method is composed of optimized processes of sand (charcoal) filtering, absorption of macroporous resin, selective desorption and recovering, regeneration treatment of resin by low-carbon alcohols, etc. The quantity of resin absorption is high, the desorption is complete, the reification has high stability, the absorption removing rate of o-phenylenediamine in waste water can reach 95%, the total recovery rate can reach 90%, and the cycling property of the waste water is greatly improved; not only pollution is treated, but also resources are recovered, and the present invention has very high social, environmental and economic benefits; the present invention is suitable for treating waste water generated in the process of producing or using o-phenylenediamine.
Description
The invention belongs to a kind of Technology of from waste water, removing and reclaiming O-Phenylene Diamine, can make waste water reclaiming, be applicable to the waste water that contains O-Phenylene Diamine that processing produces in production or use O-Phenylene Diamine process.
The method of removing of O-Phenylene Diamine is in the prior art data in the waste water, and for example industrial colling is handled Scientific And Technical Intelligence Center station 14-B-2223-8 and the 278(1987 of Beijing Chemical Research Institute's environmental protection institute " chemical industry environmental protection " (5)) in occurred.The treatment process of introducing among the data 14-B-2223-8 is: contain the waste water dosing ultrasonic wave air-flow vibration of O-Phenylene Diamine, and the pressure filter press filtration, the cinder activation is filtered, and the total clearance of O-Phenylene Diamine can reach 90%." chemical industry environmental protection " (5) 278(1987) treatment process of introducing in is: the waste water that contains O-Phenylene Diamine is transferred alkali, flocculation, active sludge-activation charcoal biomembrane biochemistry, the total clearance of O-Phenylene Diamine can reach more than 60%, prior art is the simple improvement of adopting the another kind of resource of a kind of destruction Of resources, though can remove O-Phenylene Diamine wherein, but consume and the waste resource, processing cost is also high, also produces secondary pollution.
The present invention has overcome above-mentioned these weak points, has reclaimed the O-Phenylene Diamine in the waste water, realizes waste water reclaiming, has created the condition of such waste water recycled, reduces processing cost, even can produce certain economic benefits.
A kind of wastewater treatment is also reclaimed the method for O-Phenylene Diamine, the waste water that will contain O-Phenylene Diamine enters the adsorption column adsorption treatment that H series macroporous adsorbent resin is housed after sand filtration, remove the organic pollutants such as O-Phenylene Diamine in the waste water, after this sorbent material reaches certain work adsorptive capacity, with dilute hydrochloric acid the O-Phenylene Diamine of its absorption is carried out the selectivity desorb and reclaim, use low-carbon alcohol (as industrial methanol or ethanol) to make solvent then sorbent material is made manipulation of regeneration.
The pre-treatment of waste water: the O-Phenylene Diamine waste water suction subsider of taking from the workshop, filtration enters waste water tank through filter pocket to get supernatant liquor through one day natural subsidence, enter quartz sand (granularity is about 5 orders) post filtration treatment with the 3-6BV/H filtering velocity then, filtered wastewater is made reference with distilled water, at wavelength X=610nm place, reach more than 80% with 721 spectrophotometric instrumentation transmittances.This filtered liquid is the feed liquid for the treatment of adsorption treatment.
The adsorption treatment of waste water: with the macroporous resin of high-ratio surface as sorbent material, it is that 14: 1 resin column carries out adsorption treatment that feed liquid enters aspect ratio by the flow velocity of 3-6BV/H, and once the wastewater flow rate that circulation institute can adsorption treatment is the accumulative total treatment capacity of controlling when O-Phenylene Diamine concentration reaches breakthrough point (adsorptive capacity of promptly working) in the adsorption treatment liquid.Under different waste strengths, the resin absorption treatment capacity changes to some extent, needs to adjust when debugging.O-Phenylene Diamine concentration adopts acetylacetone colorimetry.
The selectivity desorb is reclaimed: make strippant with dilute hydrochloric acid, adopt the 2-4BV/H flow velocity to reclaim O-Phenylene Diamine, its principle is:
Acidolysis vapor consumption is determined by following formula:
W＝K·2·X·36.5/C
In the formula: W-acidolysis vapor consumption (kg)
K-acidolysis vapor coefficient of excess is selected in the 1.5-2.5 scope according to the pH value of waste water.
The amount of the O-Phenylene Diamine of X-resin absorption (mol)
The 2-mol ratio
36.5-hydrochloric acid molar weight
C-acidolysis vapor percentage concentration
Acidolysis is inhaled the high dense fraction of gained and is stored in recovery o-phenylendiamine dihydrochloride storage tank, is directly used in refining O-Phenylene Diamine or synthetic derosal, recycled behind the additional hydrochloric acid of the low dense level lease making of acidolysis suction gained.
Regeneration of resin: after acidolysis sucks back the receipts O-Phenylene Diamine, adopt industrial methanol or industrial alcohol to carry out the regeneration of resin desorb with the flow velocity of 1-3BV/H.Use repeatedly again after the resin regeneration, methyl alcohol or ethanol are for recycling.
The invention has the advantages that: administer waste water, reclaim O-Phenylene Diamine simultaneously, realized waste water reclaiming, administer waste water and only include organic pollutants, substantially do not change waste water Central Plains forming and content by inorganic pollutant, help continuing to reclaim of the processing of back roads such as industrial sodium thiosulfate, broken away from the abominable operating environment of deriving and being caused of such purification of waste water treating processes organic pollutant mineral compound.
Technical process signal of the present invention is as accompanying drawing.O-Phenylene Diamine waste water suction subsider (1) from the workshop, through natural subsidence, supernatant liquor is stored in waste water tank (3) after filtering through filter (2), use pump (4) to squeeze into by a quartz sand column (5) then with the flow velocity of 3-6BV/H, the adsorption unit that resin absorption post (6), (7), (8) form of connecting with three is handled, and absorption back waste water enters waste water tank (13) and awaits further processing.Absorption finishes, from hydrochloric acid storage tank (9), hydrochloric acid is squeezed into three resin columns and carry out desorb with pump (10), flow velocity is 2-4BV/H, stripping liquid enters acid and takes off liquid storage tank (11), feed the desorb of regenerating of three series connection resin columns with industrial methanol or industrial alcohol by header tank (15) adverse current then, flow velocity is 1-3BV/H.The alcohol stripping liquid is collected in alcohol and takes off liquid storage tank (12), advances rectification cell (14) rectifying then and recycles, and rectification residue goes burning disposal.
Example 1: with the ortho-nitrochlorobenzene is raw material, adopt the pressurization amination, the sodium sulfide reducing method is produced O-Phenylene Diamine and the waste water of association, be O-Phenylene Diamine waste water, get O-Phenylene Diamine concentration and be the O-Phenylene Diamine waste water of 13257mg/l and store in subsider, through one day natural subsidence, get that to enter waste water tank after supernatant liquor filters through filter pending.
Absorption: get this waste water and enter at normal temperatures by a quartz sand column and three adsorption units that resin column is together in series with the flow velocity of 5BV/H.Feed liquid is made reference with distilled water after quartz sand column filters, wavelength 610nm place, recording transmittance with 721 spectrophotometers is 80%, to enter total aspect ratio be 14: 1 to waste water after the sand filtration, one kilogram of H-103 macroporous adsorbent resin (hygrometric state) is housed carries out adsorption treatment for the resin column of sorbent material, the treatment of o-phenylenediamine wastewater flow rate is 18l, and water outlet O-Phenylene Diamine mean concns is 354mg/l, each pollutent data following (mg/l of unit) before and after the adsorption treatment:
Loss pollutent CODcr O-Phenylene Diamine nitro thing sodium thiosulfate
The concentration title
Adsorb preceding 92,478 13,257 39.52 11%
Absorption back 80,800 354 34.82 11%
By above-mentioned data as can be known: resin is 232.6mg/g to the work adsorptive capacity of O-Phenylene Diamine, and the absorption total volume is 232.6g, and absorption back waste water enters waste water tank and awaits reclaiming the technological process that sodium thiosulfate or cover are used to produce O-Phenylene Diamine.
The hydrochloric acid desorb: the hydrochloric acid with 8% is made strippant, enter resin column with the flow velocity of 4BV/H at normal temperatures and carry out the selectivity desorb, acidolysis vapor consumption is 4.5l, the O-Phenylene Diamine mean concns is up to 49247mg/l in the acidolysis imbibition, the desorb total volume of hydrochloric acid is 221.6g, to the adsorbed O-Phenylene Diamine desorption efficiency of resin is 95.26%, the stripping liquid of hydrochloric acid is made up of 2.5l high density o-phenylendiamine dihydrochloride and the low dense o-phenylendiamine dihydrochloride of 2.0l, the high salt concentration hydrochlorate can reach 82.6% through the content of refining gained O-Phenylene Diamine, if the directly synthetic derosal product of this high salt concentration hydrochlorate, derosal content can reach 97.1%, and the lower concentration o-phenylendiamine dihydrochloride is used as the strippant of next batch desorb behind complex acid.
The methyl alcohol desorption and regeneration: the industrial methanol with 95% carries out the counter-current regeneration desorb to resin at normal temperatures with the flow velocity of 3BV/H, methanol usage is 3.5l, desorption efficiency to O-Phenylene Diamine is 0.41%, and the methyl alcohol stripping liquid is stored in and entered rectifying tower again after alcohol takes off the liquid storage tank, and rectifying is reclaimed methanol loop and used.At this moment, resin just can be used for the next batch adsorption treatment.
Example 2: with the O-Phenylene Diamine is that the waste water that raw material and the condensation of cyanamide base methyl formate generation derosal derives out is carbendazim wastewater, getting this carbendazim wastewater transfers alkali to pH=8, place the waste water subsider heavy naturally clear this waste water, it is pending to enter waste water tank after supernatant liquor filters through filter.
Absorption: get the flow velocity of this waste water, at normal temperatures, enter by a quartz sand column and three adsorption units that resin column is together in series with 5BV/H.Feed liquid is made reference with distilled water after quartz sand column filters, at wavelength 610nm place, recording transmittance with 721 spectrophotometers is 95%, to enter total aspect ratio be 14: 1 to waste water after the sand filtration, the resin column that one kilogram of H-103 macroporous adsorbent resin is housed carries out adsorption treatment, handling the carbendazim wastewater amount is 15.0l, each pollutent data following (mg/l of unit) before and after the adsorption treatment:
The loss pollutent
Concentration title CODcr O-Phenylene Diamine nitro thing
Adsorb preceding 26,009 1,200 150
Absorption back 19,310 83 11
By above-mentioned data as can be known, resin is 93% to the O-Phenylene Diamine adsorption rate, is 26% to the CODcr clearance in the carbendazim wastewater, to ArNO wherein
2Clearance 93%, resin is 16.76mg/g to the work adsorptive capacity of O-Phenylene Diamine, absorption total volume 16.76g.The carbendazim wastewater of handling through resin absorption divides storage two storage tanks, 10BV waste water before first storage tank is deposited and handled, and this waste water can directly overlap the lime nitrogen hydrolysis that is used for the derosal production process.Second storage tank is deposited 10BV with aftertreatment waste water, and this waste water drains into biochemical treatment system, and available other low concentration wastewater mixes regulates the back biochemical treatment.
The hydrochloric acid desorb: the concentration with O-Phenylene Diamine in the adsorption treatment water outlet is effluent index, when O-Phenylene Diamine concentration has reached breakthrough point in the water outlet, adsorption operations finishes, change desorb operation over to, make strippant, enter resin column with the flow velocity of 4BV/H at normal temperatures resin is carried out the selectivity desorb with 10% hydrochloric acid, acidolysis vapor consumption 2.0l, mean concns is 8067mg/l, and desorption efficiency is 96%, but the O-Phenylene Diamine direct reuse of recovery is in production.
The methyl alcohol desorption and regeneration: the industrial methanol with 95% with the flow velocity of 3BV/H at normal temperatures to the desorb of resin counter-current regeneration, desorption efficiency to O-Phenylene Diamine is 0.66%, the methyl alcohol stripping liquid is stored in and is entered rectifying tower again after alcohol takes off the liquid storage tank, and rectifying is reclaimed methanol loop and used, and methanol usage is 2.0l.
By above two examples as can be known, adopt high-ratio surface H-103 macroporous resin can adsorb the organic pollutant of removing in the O-Phenylene Diamine waste water effectively, created the condition that O-Phenylene Diamine waste water is applied mechanically or partly cover is used for technological process, adopt high-ratio surface H-103 macroporous resin adsorption to handle carbendazim wastewater, waste water after helping handling is applied mechanically, reduce discharging, and can reclaim useful matter wherein, improve the biodegradability energy of carbendazim wastewater significantly, be convenient to further biochemical treatment.
Claims (3)
1, a kind of wastewater treatment and reclaim the method and apparatus of O-Phenylene Diamine, the waste water that will contain O-Phenylene Diamine is after the clear liquid processing, entering the adsorption column that H series polymeric adsorbent is housed handles, remove the organic pollutants such as O-Phenylene Diamine in the waste water, with dilute hydrochloric acid the O-Phenylene Diamine of resin absorption is carried out desorb and reclaim, make solvent with low-carbon alcohol then resin is made manipulation of regeneration.
2, the method for a kind of processing according to claim 1 and recovery O-Phenylene Diamine, it is characterized in that: waste water in clarifying tank natural subsidence after sand filtration obtains clear liquor, waste water is handled by adsorption column, reach certain work adsorptive capacity to resin, the high dense fraction of dilute hydrochloric acid desorb gained is directly recycled, low dense fraction cover is used for the next batch desorb, and the low-carbon alcohol stripping liquid reclaims through rectifying, and solvent cycle is used for resin regeneration and handles.
3, a kind of device that adopts the described method of claim 1 to handle and reclaim O-Phenylene Diamine, its feature comprises: the sand filtration post, the several adsorption columns and the solvent distillation recovery tower of filling H series polymeric adsorbent are composed in series.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89104014 CN1024460C (en) | 1989-06-14 | 1989-06-14 | Process for wastewater treatment and the recovery of 0-phenylenediamine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89104014 CN1024460C (en) | 1989-06-14 | 1989-06-14 | Process for wastewater treatment and the recovery of 0-phenylenediamine |
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| Publication Number | Publication Date |
|---|---|
| CN1048019A CN1048019A (en) | 1990-12-26 |
| CN1024460C true CN1024460C (en) | 1994-05-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 89104014 Expired - Fee Related CN1024460C (en) | 1989-06-14 | 1989-06-14 | Process for wastewater treatment and the recovery of 0-phenylenediamine |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101200336B (en) * | 2007-12-18 | 2010-12-08 | 赵志军 | Process for zero-discharge treatment of o-phenylenediamine sodium sulfide reduction wastewater |
| CN101962236B (en) * | 2010-08-12 | 2012-09-26 | 河北圣雪大成制药有限责任公司 | Process for recovering streptomycin sulphate from waste water by coupling foam separation and ion exchange |
| CN102887601B (en) * | 2012-11-01 | 2014-01-22 | 华东理工大学 | Method for removing o-phenylenediamine (OPD) in wastewater |
| CN103274538A (en) * | 2013-06-14 | 2013-09-04 | 陕西蓝深特种树脂有限公司 | System and method for recovering and treating p-phenylenediamine industrial wastewater |
| CN106984139A (en) * | 2017-04-25 | 2017-07-28 | 安徽三星树脂科技有限公司 | Anion exchange resin produces the handling process of waste gas |
| CN108892300A (en) * | 2018-06-29 | 2018-11-27 | 江苏力波兴水务科技有限公司 | A kind of processing method of carbendazim production utilization of wastewater resource |
| CN109607888A (en) * | 2019-02-25 | 2019-04-12 | 安徽国星生物化学有限公司 | A kind of wastewater treatment method and system of two villaumite containing paraquat |
| CN109956514A (en) * | 2019-04-04 | 2019-07-02 | 运城晋腾化学科技有限公司临猗分公司 | A kind of industrial wastewater resin adsorption device and its absorbing process |
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1989
- 1989-06-14 CN CN 89104014 patent/CN1024460C/en not_active Expired - Fee Related
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| CN1048019A (en) | 1990-12-26 |
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