CN1865223A - Method for extracting o-phenylendiamine from waste water of o-phenylendiamine production - Google Patents
Method for extracting o-phenylendiamine from waste water of o-phenylendiamine production Download PDFInfo
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- CN1865223A CN1865223A CN 200510043556 CN200510043556A CN1865223A CN 1865223 A CN1865223 A CN 1865223A CN 200510043556 CN200510043556 CN 200510043556 CN 200510043556 A CN200510043556 A CN 200510043556A CN 1865223 A CN1865223 A CN 1865223A
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- phenylene diamine
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Abstract
This invention relates to a method for extracting o-phenylenediamine from waste water of o-phenylenediamine production. Wherein: filtrate the waste water containing o-phenylenediamine, and load it on the absorption column filled with macroreticular resin which absorbs o-phenylenediamine and other organic compounds in the waste water, and then elute with ethanol solution to desorb the o-phenylenediamine and form the desorption solution, distill the desorption solution to remove the ethanol, cool the residual liquid after distillation at controlled temperature to precipitate the o-phenylenediamine crystals, and then obtain the o-phenylenediamine by filtration. This invention is characterized of high clearance of o-phenylenediamine in the waste water, high-purity of recovered o-phenylenediamine, simple and rational process. It accomplishes the object of turning waste to be useful, solves the waste discharging problem, and has a good economical benefit.
Description
Technical field
The present invention relates to wastewater treatment and utilize technology, specifically a kind of method of from the O-Phenylene Diamine factory effluent extracts, extracting O-Phenylene Diamine.
Background technology
O-Phenylene Diamine is a kind of important agricultural chemicals and the intermediate of dyestuff, and it mainly is that raw material makes through High Temperature High Pressure amination, sodium sulfide reducing with the o-Nitrochlorobenzene.Adopt aforesaid method, 1 ton of O-Phenylene Diamine of every production will discharge 8～10 tons of waste water (CODcr is about 10～120,000 mg/l), and wherein main component is: contain O-Phenylene Diamine 0.5～1%, sodium thiosulfate 16～18%, Sodium Sulphide 1～2% etc.The O-Phenylene Diamine factory effluent has higher extraction and application and is worth, and the processing and utilizing approach to such waste water mainly is as the raw material of producing sodium thiosulfate at present.But in utilizing its process of producing sodium thiosulfate, for removing organism wherein, need to add a large amount of gacs, cost is higher.And, because O-Phenylene Diamine has the characteristic of easy distillation, in extracting the sodium thiosulfate process, still containing organism such as a certain amount of O-Phenylene Diamine in the water that steams when waste water carries out evaporation concentration, CODcr is still up to 6000-7000mg/l.The water that steams is directly discharged, still can cause serious pollution.
Chinese patent 89104014.5 discloses a kind of method of extracting O-Phenylene Diamine from the O-Phenylene Diamine factory effluent, it is to the effect that: adopt the O-Phenylene Diamine in the H series large aperture adsorption resin absorption waste water, with dilute hydrochloric acid the O-Phenylene Diamine of resin absorption is carried out desorb then and reclaim, and resin regeneration is handled with low-carbon alcohol.But this method still has the following disadvantages: after 1, adopting the hydrochloric acid desorb, also need again with low-carbon alcohol the resin desorption and regeneration, and complex process, productive expense is higher.2, can only obtain o-phenylendiamine dihydrochloride after the hydrochloric acid desorb, can not directly obtain O-Phenylene Diamine,, need to increase other operations if will make O-Phenylene Diamine; 3, used H series wide aperture its absorption property of resin not good (after the adsorption treatment in the waste water O-Phenylene Diamine content still bigger).
Summary of the invention
The object of the present invention is to provide a kind of method of from the O-Phenylene Diamine factory effluent, extracting O-Phenylene Diamine, this method can directly be extracted O-Phenylene Diamine from waste water, and desorb and desorption process once finish, and make waste water when being used to extract sodium thiosulfate, can save a large amount of gacs follow-up.
For achieving the above object, the scheme of the present invention's employing is as follows:
After will containing the waste water filtering of O-Phenylene Diamine, make it enter the adsorption column that the wide aperture resin is housed and carry out adsorption treatment, organism such as the O-Phenylene Diamine in the waste water are attracted on the resin of wide aperture.When the O-Phenylene Diamine factory effluent carried out adsorption treatment, its temperature was 0～50 ℃, and flow is 0.5～5BV/H.The model of wide aperture resin is XDA-1, XDA-200, LSA-8B or LSA-800C.After the wide aperture resin absorption is saturated, with desorbing agent the O-Phenylene Diamine of wide aperture resin absorption is carried out desorb and reclaim, make wide aperture resin desorption and regeneration.Desorbing agent is an ethanolic soln, and the volume of ethanolic soln consumption is 0.5～2.5 times of macroporous resin volume, and the concentration of volume percent of ethanolic soln is 10～95%, and the temperature of ethanolic soln is that 10～70 ℃, flow are 0.5～5BV/H.Dissolve with ethanol solution after O-Phenylene Diamine forms desorption liquid, desorption liquid is distilled, ethanol is steamed, again the raffinate after the distillation is carried out the temperature control cooling, the O-Phenylene Diamine crystallization is separated out, and temperature control refrigerative speed is 0.1～1 ℃/min, and refrigerative is a normal temperature by temperature.Filter the raffinate that contains O-Phenylene Diamine then, obtain O-Phenylene Diamine.
By such scheme as seen, the present invention adopts ethanolic soln as desorbing agent, when the O-Phenylene Diamine to the wide aperture resin absorption carries out desorb and reclaims, also can make wide aperture resin desorption and regeneration, need not implement the treatment process to the resin desorption and regeneration more separately.And, by method provided by the present invention the O-Phenylene Diamine factory effluent was extracted O-Phenylene Diamine after, when extracting sodium thiosulfate with this waste water again, can save a large amount of gacs.After by the present invention the O-Phenylene Diamine factory effluent being extracted O-Phenylene Diamine, waste water is detected with spectrophotometry, wherein the content of O-Phenylene Diamine can be reduced to below the 5mg/l, other inorganics components unchanged again.And, the waste water that extracted O-Phenylene Diamine is distilled, the CODcr index is reduced to below the 100mg/l in the distillate, and distillate can directly discharge.
The present invention is to the clearance height of O-Phenylene Diamine in the O-Phenylene Diamine factory effluent, and the purity of the O-Phenylene Diamine that is recovered to is better, and technology is simple, rationally, both realized the purpose that turns waste into wealth having solved the problem of disposal of pollutants again, have favorable economic benefit.
Embodiment
Further specify the present invention below in conjunction with specific embodiment.
Embodiment one
The wide aperture resin of measuring 100ml (about 70g) model and be XDA-1 is packed in the glass adsorption column, gets the O-Phenylene Diamine factory effluent, earlier it is filtered, and filtering method is vacuum filtration or press filtration.Waste water after will filtering at normal temperatures passes through the glass adsorption column from bottom to top with the flow of 2BV/H, by the wide aperture resin in the adsorption column post organism such as O-Phenylene Diamine in the waste water are adsorbed, wastewater treatment capacity is 1200ml (12BV), and waste water is faint yellow after flowing out by glass column.
After testing, waste water is before passing through glass column, and wherein the content of O-Phenylene Diamine is 6372mg/l, and to the waste water straight run distillation, the CODcr measured value is 6425mg/l in the distillate.Waste water detects with spectrophotometry by behind the glass column, and wherein the content of O-Phenylene Diamine is 3.5mg/l, the waste water after the absorption is distilled again, and the CODcr measured value is 87mg/l in the distillate.As seen, after waste water passes through the adsorption treatment of wide aperture resin, the clearance of O-Phenylene Diamine＞99.9%, the CODcr of distillate reduces by 98.6%.
After waste water flows through glass column, getting concentration is that 70% (v/v), temperature are 20 ℃ ethanolic soln 200ml, make ethanolic soln with the flow of 2BV/H from bottom to top by glass column, the O-Phenylene Diamine of wide aperture resin absorption is carried out desorb reclaims, and make wide aperture resin desorption and regeneration.Dissolve with ethanol solution after O-Phenylene Diamine forms desorption liquid, collect whole desorption liquids, pour in the matrass, desorption liquid is distilled, ethanol is steamed and reclaims.
When being distilled to no ethanol and steaming, distillation finishes, and the raffinate after the distillation is carried out the temperature control cooling, rate of temperature fall is 0.5 ℃/min, and when raffinate was cooled to normal temperature, the O-Phenylene Diamine sufficient crystallising was separated out, then, the raffinate that contains O-Phenylene Diamine is filtered, obtain O-Phenylene Diamine product 10.6g.By analysis, the purity of O-Phenylene Diamine product is 85.5%, and yield is 95.9%.
Embodiment two
The wide aperture resin of measuring 100ml (about 70g) model and be XDA-200 is packed in the glass adsorption column, get the O-Phenylene Diamine factory effluent, earlier waste water is filtered by the mode of vacuum filtration or press filtration, waste water after will filtering under 25～35 ℃ passes through glass column from bottom to top with the flow of 2.5BV/H, by the wide aperture resin in the glass column organism such as O-Phenylene Diamine in the waste water are adsorbed, wastewater treatment capacity is 1200ml (12BV), and waste water is faint yellow after flowing out by glass column.
After testing, waste water is before passing through glass column, and wherein the content of O-Phenylene Diamine is 5856mg/l, and waste water detects with spectrophotometry by behind the glass column, and wherein the content of O-Phenylene Diamine is reduced to 7.5mg/l, and the clearance of O-Phenylene Diamine reaches 99.8%.By waste water is distilled, the CODcr measured value is 96mg/l in the distillate of acquisition again.
After waste water flow through glass column, getting concentration was that 80% (v/v), temperature are 25 ℃ ethanolic soln 200ml, make ethanolic soln with the flow of 2.5BV/H from bottom to top by glass column, the O-Phenylene Diamine of resin absorption is carried out desorb reclaims, and make the resin desorption and regeneration.Dissolve with ethanol solution after O-Phenylene Diamine forms desorption liquid, collect whole desorption liquids, pour in the matrass, desorption liquid is distilled, ethanol distillation is gone out, and reclaims.
When being distilled to no ethanol and steaming, distillation finishes, and the raffinate after the distillation is carried out the temperature control cooling, rate of temperature fall is 0.7 ℃/min, and when raffinate was cooled to normal temperature, the O-Phenylene Diamine sufficient crystallising was separated out, then, the raffinate that contains O-Phenylene Diamine is filtered, obtain O-Phenylene Diamine product 9.5g.By analysis, the purity of O-Phenylene Diamine product is 83%, and yield is 94%.
Example three
Adopt two adsorption column series connection absorption, the operation scheme of single-column desorption, concrete steps are as follows:
1, the adsorption column (Φ 1000 * 5000) of absorbing process-two same sizes of employing, they are labeled as I post, II post, each adsorption column filling XDA-1 wide aperture resin 2500Kg (about 3600L), under 25～30 ℃, O-Phenylene Diamine factory effluent (content is 6149mg/l) is removed behind the impurity with pump after filtration with 7.2m
3The flow of/h is squeezed into adsorption column.The suction type of I, the series connection of II two posts, adverse current is adopted in absorption, and the I post is that front pillar, II post are rear pillar, and promptly waste water enters through the I column bottom, flows out from I post capital, enters from the II column bottom again, flows out from II post capital.Waste water is after adsorption treatment, and O-Phenylene Diamine content is than the end (being about 4.5mg/l) in the initial water outlet, and water outlet enters basin and stores, as the raw material that extracts sodium thiosulfate.When O-Phenylene Diamine content reached the breakthrough point of 20mg/l in the water outlet of II post, the wide aperture resin absorption was saturated in the I post, stopped absorption, carried out desorb, desorption manipulation.
2, the desorption technique-O-Phenylene Diamine of wide aperture resin absorption in the I post is carried out desorb reclaim, and make wide aperture resin desorption in it, the concrete operations step is as follows: earlier raffinate in the I post is drained, use 7.2m then
3(2BV) concentration be the ethanolic soln of 75% (v/v) under 25～30 ℃, pass through from the following current of I capital with the flow of 2BV/H, the resin in it is carried out desorb, dissolve with ethanol solution O-Phenylene Diamine form desorption liquid, desorption liquid advances Distallation systm.Behind the resin desorption of wide aperture, use 7.2m again
3The clear water following current is washed the resin in it by the I post, and clear water flow is 2～2.5BV/H, the preceding 3.6m of water lotion
3Be used for preparation next time ethanol desorbing agent; Back 3.6m
3Be used for washing next time and apply mechanically, so far, desorb, desorption finish.
When two adsorption columns then used next time, the I post that desorption is finished was as rear pillar, and the II post, flows out from II post capital even waste water enters through the II column bottom as front pillar, enters from the I column bottom again, flows out from I post capital, carries out the counter flow in series adsorption operations.When then using again, be again that front pillar, II post are rear pillar with the I post next time, so circulation.
3, distillation, crystallization-desorption liquid advance the Distallation systm distillation, make ethanol steam, also reclaim, and the ethanol of recovery continues on for next desorb and uses.When being distilled to no ethanol and steaming, distillation finishes.Then raffinate is squeezed in the crystallizing pan, carried out the temperature control cooling, rate of temperature fall is 0.5 ℃/min, stops cooling when temperature is reduced to normal temperature, and the O-Phenylene Diamine sufficient crystallising is separated out.Filter the raffinate, the centrifuge dehydration that contain O-Phenylene Diamine then and get O-Phenylene Diamine product 375Kg, O-Phenylene Diamine content is 83.6%, and the raffinate after the filtration can be used for adsorption treatment once more.
Embodiment four
XDA-1 resin used among the embodiment one is replaced with LSA-8B or LSA-800C wide aperture resin, and the index of wide aperture resin demand, handled waste water and treatment step are all identical with embodiment one with condition, and the result that obtains is as follows:
1, adopts LSA-8B wide aperture resin
The adsorption treatment amount of O-Phenylene Diamine waste water is 1100ml (11BV), obtain O-Phenylene Diamine product 9.8g, by analysis, the purity of O-Phenylene Diamine product is 83.1%, yield is 92.5%, and in the waste water after the absorption, the content of O-Phenylene Diamine is 5.6mg/l, waste water after the processing distills, and the CODcr measured value is 90mg/l in the distillate of acquisition.
2, adopt LSA-800C wide aperture resin
The adsorption treatment amount of O-Phenylene Diamine waste water is 1150ml (11.5BV), obtain O-Phenylene Diamine product 9.6g, by analysis, the purity of O-Phenylene Diamine product is 82.6%, yield is 91.3%, and in the waste water after the absorption, the content of O-Phenylene Diamine is 5.8mg/l, waste water after the processing distills, and the CODcr measured value is 95mg/l in the distillate of acquisition.
Claims (6)
1, from the O-Phenylene Diamine factory effluent, extract the method for O-Phenylene Diamine, after will containing the waste water filtering of O-Phenylene Diamine, make it enter the adsorption column that the wide aperture resin is housed and carry out adsorption treatment, organism such as the O-Phenylene Diamine in the waste water are attracted on the resin of wide aperture, with desorbing agent the O-Phenylene Diamine of wide aperture resin absorption being carried out desorb reclaims, it is characterized in that: desorbing agent is an ethanolic soln, dissolve with ethanol solution after O-Phenylene Diamine forms desorption liquid, desorption liquid is distilled, ethanol is steamed, again the raffinate after the distillation is carried out the temperature control cooling, the O-Phenylene Diamine crystallization is separated out, filter the raffinate that contains O-Phenylene Diamine and obtain O-Phenylene Diamine.
2, the method for extracting O-Phenylene Diamine from the O-Phenylene Diamine factory effluent according to claim 1, it is characterized in that: the model of macroporous resin is XDA-1, XDA-200, LSA-8B or LSA-800C.
3, the method for extracting O-Phenylene Diamine from the O-Phenylene Diamine factory effluent according to claim 1, it is characterized in that: when the O-Phenylene Diamine factory effluent carried out adsorption treatment, its temperature was 0～50 ℃, and flow is 0.5～5BV/H.
4, the method for from the O-Phenylene Diamine factory effluent, extracting O-Phenylene Diamine according to claim 1, it is characterized in that: the volume of ethanolic soln consumption is 0.5～2.5 times of wide aperture resin volume, the concentration of volume percent of ethanolic soln is 10～95%, and the temperature of ethanolic soln is that 10～70 ℃, flow are 0.5～5BV/H.
5, the method for from the O-Phenylene Diamine factory effluent, extracting O-Phenylene Diamine according to claim 1, it is characterized in that: temperature control refrigerative speed is 0.1～1 ℃/min, refrigerative is a normal temperature by temperature.
6, the method for extracting O-Phenylene Diamine from the O-Phenylene Diamine factory effluent according to claim 1 is characterized in that: adopt two adsorption column series connection absorption, the operation scheme of single-column desorption.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200510043556 CN1865223A (en) | 2005-05-16 | 2005-05-16 | Method for extracting o-phenylendiamine from waste water of o-phenylendiamine production |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102887601A (en) * | 2012-11-01 | 2013-01-23 | 华东理工大学 | Method for removing o-phenylenediamine (OPD) in wastewater |
| CN104086440A (en) * | 2014-06-10 | 2014-10-08 | 安徽华润涂料有限公司 | Technology for processing mother liquor of o-phenylenediamine |
| CN104176867A (en) * | 2013-05-22 | 2014-12-03 | 北京思践通科技发展有限公司 | Recovery method for amine |
| 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 |
-
2005
- 2005-05-16 CN CN 200510043556 patent/CN1865223A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102887601A (en) * | 2012-11-01 | 2013-01-23 | 华东理工大学 | Method for removing o-phenylenediamine (OPD) in wastewater |
| CN102887601B (en) * | 2012-11-01 | 2014-01-22 | 华东理工大学 | Method for removing o-phenylenediamine (OPD) in wastewater |
| CN104176867A (en) * | 2013-05-22 | 2014-12-03 | 北京思践通科技发展有限公司 | Recovery method for amine |
| CN104086440A (en) * | 2014-06-10 | 2014-10-08 | 安徽华润涂料有限公司 | Technology for processing mother liquor of o-phenylenediamine |
| 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 |
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