CN101066824B - Process of treating and reusing effluent from 1-amino-8-naphthol-3, 6-disulfonic acid production - Google Patents
Process of treating and reusing effluent from 1-amino-8-naphthol-3, 6-disulfonic acid production Download PDFInfo
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- CN101066824B CN101066824B CN2007100576266A CN200710057626A CN101066824B CN 101066824 B CN101066824 B CN 101066824B CN 2007100576266 A CN2007100576266 A CN 2007100576266A CN 200710057626 A CN200710057626 A CN 200710057626A CN 101066824 B CN101066824 B CN 101066824B
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- naphthol
- amino
- disulfonic acid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
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Abstract
The present invention is process of treating effluent from the production of dye intermediate 1-amino-8-naphthol-3, 6-disulfonic acid and recovering resource. The process includes: distilling pre-treatment of the effluent; adsorbing 1-amino-8-naphthol-3, 6-disulfonic acid, intermediate product and other organic matter from the effluent with macroporous weak alkaline resin ND900 in serially connected three column; neutralizing the adsorbed columns treated water with alkali and decompression distilling; and final aerobic biochemical treatment for the water to reach exhaust standard. The processcan reduce CODcr in the effluent from 16,700 mg/l to below 100 mg/l. The used resin may be desorbed with NaOH+H2O desorbing agent for reuse, and the desorbed liquid may be distilled for recovery.
Description
Technical field
The present invention relates to dyestuff intermediate 1-amino-8-naphthol-3, the improvement of the factory effluent that discharges in the 6-disulfonic acid production process.Particularly, be 1-amino-8-naphthol-3, the recycling of sodium sulfate in the resource utilization of 6-disulfonic acid and intermediate product thereof and the waste water realizes discharged wastewater met the national standard, the final 1-amino-8-naphthol-3 of realizing, the improvement of 6-disulfonic acid factory effluent and resource utilization thereof are recycled.
Background technology
1-amino-8-naphthol-3, the 6-disulfonic acid is a kind of important dyestuff intermediate, is mainly used in to produce acidity, reactive dyestuffs and azoic dyestuff, also can be used for pharmaceutical industry.Be slightly soluble in cold water and be soluble in hot water, be dissolved in the basic solutions such as soda ash and caustic soda.Add sulfuric acid (or hydrochloric acid) and separate out the single sodium salt of H acid in the acid out operation, the waste liquid after the filtration belongs to typical high density, high chroma, and the organic waste water of high bio-toxicity is compared other and is contained the organic waste water of benzene series, has following singularity:
(1) pollutant component complexity, the concentration height.The H acid mother liquor of Pai Chuing in process of production contains the various substitutive derivatives of a large amount of naphthalenes, and COD is up to several ten thousand mg/L, and complicated component contains a large amount of naphthalene derivativess.
(2) acid strong, pH is greatly between 1～2.
(3) colourity is dark, and about 1 * 10
5About, generally be pale brown to chocolate.
(4) toxicity is big, and H acid belongs to condensed-nuclei aromatics, has the intensive bio-toxicity, and waste water is if not treated direct discharging with serious environment pollution, also has very big harm to human body.
(5) readily biodegradable not, because the delocalized conjugated that naphthalene nucleus is made up of 10 carbon atoms, the structure quite stable is difficult to degrade.The BOD of most of waste water in this class waste water
5/ COD is extremely low, and biodegradability is poor, and toxic to microorganism, is difficult to handle with general biochemical method.
Method about this type of production wastewater treatment, mainly contained wet type (catalysis) oxidation style, photocatalytic oxidation, extraction process (comprising liquid film extraction method, complexing abstraction) etc. at present, these methods exist equipment complexity, special substance difficult quality guarantee, medicament costliness, operational condition harshness (as high temperature, high pressure etc.) respectively, energy consumption is high and secondary pollution problems is arranged.
Extraction process is a difference of utilizing pollution substance partition ratio between water and extraction agent in the waste water, fully contact through biphase, toxic substance is transferred to the extraction phase from water, then through stripping, toxic substance and extraction agent are separated, the latter recycles, and the former can realize effective recycling, thereby usually as one of effective way that realizes waste water treatment and resource utilization.According to the difference of the mechanism of action and operating method, can be divided into complexing abstraction and liquid film extraction method.
Wet oxidation process is (under 0.5～20MPa) condition, to be oxygenant (now also have and use other oxygenants, as ozone, hydrogen peroxide etc.) with airborne oxygen, in liquid phase organic pollutant to be oxidized to CO at high temperature (125～320 ℃) and high pressure
2Chemical process with inorganicss such as water or small organic molecule.The catalytic wet oxidation method is to add suitable catalyzer to reduce the temperature and pressure of reaction in traditional wet-type oxidation technology, improves oxidative decomposition capacity, shortens the reaction times.If be used oxygenants such as hydrogen peroxide, ozone, then can increase free-radical generating speed, further improve waste water treatment efficiency.
What photocatalysis oxidation technique research at present was more is heterogeneous conductor photocatalysis oxidation style and homogeneous phase photooxidation method two big classes.(1) heterogeneous conductor photocatalysis oxidation style.TiO
2And SrO
2Can be activated by near ultraviolet radiation Deng semiconductor substance, form hydroxyl, utilize the very high free radical of these activity, can oxidation organism and make it permineralization separately.Using more catalyzer is TiO
2, TiO
2Spectrochemical property is stable, nontoxic, inexpensive and be easy to get.Employing photochemical precipitation methods such as gold development have prepared Ag/TiO
2Photocatalyst, and the organic pollutant H acid of typical difficult for biological degradation carried out photocatalytic degradation research.The result shows that the Ag of massfraction 1.0% loading can significantly improve TiO
2Photocatalytic activity, but realize within a short period of time the higher degradation rate of H acid.(2) homogeneous phase photooxidation method.Compare with the conductor photocatalysis oxidation style, add O
3, H
2O
2, the homogeneous phase photooxidation method that works of oxygenant such as Fenton reagent and light one, its oxidation capacity and photodissociation speed are all considerably beyond simple conductor photocatalysis oxidation style, and do not have the recovery of catalyzer and fixing, and problems such as the pollution of catalyzer and activation.Homogeneous phase photoxidation system commonly used has UV/O
3, UV/H
2O
2, UV/Fenton, UV/H
2O
2/ ironic oxalate complex compound etc.Wherein using more is Fenton reagent, promptly ferrous-hydrogen peroxide method.This method is to wastewater containing phenol, chlorophenol waste water, and municipal effluent, dyeing waste water, difficult decomposing organic matter has good treatment effect in the rubbish water seepage, so Fenton reagent method comes into one's own day by day as a kind of advanced oxidation processes.Zhu Wanpeng etc. have studied possibility and the processing condition of handling the H acid waste liquid with Fenton reagent method, improve its biodegradability, for biochemical treatment creates conditions.
The sorbent material of handling dye intermediate wastewater with absorption method has gac, modified-cellulose, clay mineral, silica gel etc.Yet regenerability, the physical strength of most sorbent materials are not ideal enough.As common gac, though its loading capacity is big, waste water to high and low concentration all has removal effect preferably, but condition harshnesses such as regeneration method of active carbon commonly used such as heat regeneration, regeneration efficiency are low, bad mechanical strength, cost is higher when being used for wastewater treatment, and water pollutant is difficult for realizing resource utilization.And the polymeric adsorbent that development in recent years is got up is subjected to people's attention because of its special advantages, and resin adsorption method has advantages such as advantages of good adsorption effect, desorption and regeneration are easy, simple to operate, recyclable resource, is a kind of effective ways of handling organic waste water.Be characterized in can be from the aqueous solution adsorb organic compound, and desorption and regeneration easily, thus realize organic enrichment in the waste water, separation and recovery.That resin adsorption method has overcome is poor as existing adsorption selectivities of sorbent material such as gac, flyash and cinders, desorption and regeneration difficulty, adsorptive capacity are little, bad mechanical strength, be difficult to realize problem such as comprehensive utilization, and resin also has the scope of application wide, and adsorption effect is not subjected to the influence of contained inorganic salt; Do not produce secondary pollution; Can reclaim organism useful in the waste water, advantage such as the technology simple operations is convenient becomes the research focus of the fractionation by adsorption novel material that is used for environmental pollution improvement.
Polymeric adsorbent is porous, the highly cross-linked high-molecular copolymer of a class, has bigger specific surface area and suitable aperture, can adsorb some material from gas phase or solution.Polymeric adsorbent has many types, and wherein ion exchange resin is used comparatively common.Ion exchange resin (IER) is a kind of complex functionality macromolecular material that contains active group, and it is that crosslinked high-molecular copolymer introducing different properties ion-exchange group forms.Ion exchange resin has functions such as exchange, selection, absorption and catalysis, in Industrial Wastewater Treatment, is mainly used in and reclaims heavy metal and your rare metal, purifies toxic substance, removes acid or alkaline organic substance in the organic waste water such as phenol, acid, amine etc.At present, the ion exchange resin that uses in Industrial Wastewater Treatment has anionite-exchange resin, Zeo-karb, amphoteric ion-exchange resin etc.Difference by the resin form can be divided into gel-type and macroporous type two classes, and wherein the macroporous type polymeric adsorbent is used more extensive.Macroporous adsorbent resin is the polymer bead-like body that inside is cross-linked structure, different with common industrial water supply processing spent ion exchange resin, macroporous adsorbent resin is not with the soda acid functional group, can not carry out ion exchange reaction, but it has good pore structure and very big specific surface area, can from water, adsorb organic solute, thereby realize in the waste water organic enrichment and separate.
Because dyestuff intermediate 1-amino-8-naphthol-3,6-disulfonic acid waste water salt and CODcr are too high, so effective improvement of its factory effluent remains a great problem so far.The domestic and foreign literature retrieval shows that the technology of the present invention had not been seen bibliographical information.
Summary of the invention
The object of the present invention is to provide 1-amino-8-naphthol-3, the recoverying and utilizing method of H-acid sodium-salt in the resource utilization of 6-disulfonic acid and intermediate product thereof and the waste water.For achieving the above object, technical scheme of the present invention is as follows:
A kind of 1-amino-8-naphthol-3, the improvement of 6-disulfonic acid factory effluent and resource utilization recoverying and utilizing method thereof, it is: (1) 1-amino-8-naphthol-3, the methyl alcohol of 6-disulfonic acid factory effluent in distillation removal waste water, methyl alcohol in the elimination waste water is to the influence of ion exchange resin adsorption treatment, processed waste water CODcr drops to about 13200mg/L from about 16700mg/L, and cooling back adjust pH is 3, makes it reach the optimal adsorption condition; (2) waste water is after pre-treatment, at 10～35 ℃, successively by the adsorption column that is filled with macroreticular weakly base resin ND900 polymeric adsorbent of three serial connections, every post need add 3.0BV upper prop liquid and move continuously with the flow of 0.5～1.0BV/h, adsorption column water outlet water white transparency, CODcr is less than 300mg/L; (3) the adsorption column water outlet is in alkali and back underpressure distillation, cooling, filtered and recycled sodium sulfate crystal, and the distillation water outlet is reusable, or CODcr can qualified discharge less than 100mg/L after the aerobic bio-contact oxidation processing; (4) will adsorb 1-amino-8-naphthol-3 in the step (2), organic macroreticular weakly base resin ND900 polymeric adsorbents such as 6-disulfonic acid and intermediate product thereof are with 90～95 ℃ of alkali sodium hydroxide and water 3BV desorption and regeneration, the desorption flow is 1～2BV/h, handle once with 1BV methyl alcohol desorption after using 10 batches, treatment temp is 30～40 ℃, flow is 0.5～1.0BV/h, and the polymeric adsorbent after the 3BV water washing can use repeatedly again.Methyl alcohol is reclaimed in treatment solution distillation, and residue is burning disposal directly, and washing water can qualified discharge after the aerobic bio-contact oxidation processing; (5) with the desorption liquid in the step (4) distillation volume 87%, cooling, filter to reclaim 1-amino-8-naphthol-3,6-disulfonic acid and intermediate product thereof.Filtrate and another batch desorption liquid merge repetition (5) step.The distillation water outlet can be used as the resin washing water and reuses; (6) the 1-amino-8-naphthol-3 that step (5) is reclaimed, 6-disulfonic acid and intermediate product thereof drop into original production process as raw material and use, and do not influence quality product.
Above-mentioned macroreticular weakly base resin ND900 has macropore weak basic anion exchange resin, strong polarity; Specific surface area 934.0m
2/ g; Average pore diameter 4.5nm; Micropore area 8m
2/ g; Micro pore volume 0.003ml/g; Complete exchange capacity 4.90mmol/g;
Adopt the inventive method to handle dyestuff intermediate 1-amino-8-naphthol-3,6-disulfonic acid factory effluent, the CODcr of waste water reduces to below the 100mg/L from about 16700mg/L before and after handling, and can reach national secondary discharge standard, and the sodium sulfate crystal of recovery can use.Resin energy desorption and regeneration, desorption liquid reclaims through distillation, and the distillation water outlet is reused.The 1-amino-8-naphthol-3 that reclaims, 6-disulfonic acid and intermediate product thereof can be used as raw material and get back to original production process, when administering waste water, have realized the changing waste into resources recycling.
The invention has the beneficial effects as follows:
(1) scope of application is wide, and practicality is good.Organic concentration mg/L from several to up to ten thousand all can use this method and handles in the waste water, and adsorption effect is not subjected to the influence of contained inorganic salt in the solution.
(2) adsorption efficiency height, desorption and regeneration is easy.Waste water is general equal after adsorbing to be reached or near emission standard, can reach usually more than 99% organic adsorption rate, does not produce secondary pollutant.Desorption soda acid commonly used or organic solvent, desorption rate generally can reach more than 95%.
(3) resin property is stable, long service life.Resin has the performance of higher resistance to oxidation, acid and alkali-resistance, organic solvent-resistant, can be at life-time service below 150 ℃, and under normal circumstances year wastage rate are less than 5%.
(4) help comprehensive utilization, turn waste into wealth.Pollutants in waste water mostly is raw material, intermediate or the product that runs off in the production, and price general charged is higher, adopts this method can make its major part obtain recycling, and obtains considerable economic.Usually recovery value is suitable with the device running expense, and what have still has a surplus.
(5) technology is simple, does not need specific installation, and technology is grasped easily, and is easy and simple to handle, and heat energy in service and power consumption are lower.
Embodiment
Further specify the present invention by the following examples:
Embodiment 1:
30mL (about 22g) macroreticular weakly base resin ND900 resin is filled in (Φ 20 * 250mm) in the glass column of insulation jacket.Get 55mL xanchromatic factory effluent distillation 5mL postcooling to room temperature, adjust pH is 3.Upper prop liquid CODcr is 16700mg/L, and at room temperature (25 ℃) pass through resin column with the flow of 10mL/h, and it is colourless that absorption effluent is, CODcr reduces to 260mg/L, this water is after neutralization, aerobic bio-contact oxidation are handled, and CODcr reduces to 70mg/L, can reach national secondary discharge standard.
Macroreticular weakly base resin ND900 resin temperature after absorption is that 92 ± 2 ℃ of alkali and hot water 40mL carry out desorption and regeneration, and flow is 10mL/h.Resin behind desorption and regeneration is reused.1-amino-8-naphthol-3, the desorption rate of 6-disulfonic acid are 98%.Desorption liquid (40mL) is behind distillation 30mL, and the water of recovery can continue to serve as desorbing agent.Distillation residual solution cooling back suction filtration reclaims 1-amino-8-naphthol-3,6-disulfonic acid and intermediate product thereof.Filtrate and next batch desorption liquid distill together.
Claims (7)
1. naphthalene series dye intermediate 1-amino-8-naphthol-3, the improvement of 6-disulfonic acid factory effluent and resource utilization recoverying and utilizing method thereof, its principal character may further comprise the steps:
(1) naphthalene series dye intermediate 1-amino-8-naphthol-3, the methyl alcohol of 6-disulfonic acid factory effluent in distillation removal waste water, methyl alcohol in the elimination waste water is handled back CODcr and is dropped to 13200mg/L from 16700mg/L the influence of ion exchange resin adsorption treatment, and cooling back adjust pH is 3; (2) waste water is faint yellow after pre-treatment, at 10～35 ℃, is the adsorption column of the macroreticular weakly base resin of ND-900 by three filling models successively with the flow of 0.5～1.0BV/h, adsorption column water outlet water white transparency, and CODcr is less than 300mg/L; (3) with adsorption column water outlet in the step (2) in alkali and back underpressure distillation, cooling, filtered and recycled sodium sulfate crystal, distillation water outlet repeated use; Or after aerobic bio-contact oxidation is handled CODcr less than 100mg/L, the water outlet qualified discharge; (4) will adsorb 1-amino-8-naphthol-3 in the step (2), the organic ND-900 type of 6-disulfonic acid and intermediate product thereof macroreticular weakly base resin carries out desorption and regeneration, handle once with methyl alcohol after using 10 batches, methyl alcohol, the direct burning disposal of residue are reclaimed in the treatment solution distillation; (5) desorption liquid in the step (4) distilled, cool off, filter with recovery 1-amino-8-naphthol-3,6-disulfonic acid and intermediate product thereof, filtrate and another batch desorption liquid merging repetition (5) step, the distillation water outlet is reused as washing water; (6) the 1-amino-8-naphthol-3 that step (5) is reclaimed, 6-disulfonic acid and intermediate product thereof drop into original production process as raw material and use.
2. method according to claim 1, the general employing of adjust pH adds the method that alkali sodium hydroxide is transferred pH after the cooling of the middle indication of its characterization step (1).
3. method according to claim 1, the 1-amino-8-naphthol-3 of indication in its characterization step (2), 6-disulfonic acid Wastewater Pretreatment transfers pH to separate out the post precipitation supernatant liquor to carry out filtering treatment process for adding alkali sodium hydroxide.
4. the indication desorption and regeneration adopts NaOH+H in the method according to claim 1, its characterization step (4)
2The desorbing agent of O, desorption temperature are 40～80 ℃, and the desorbing agent flow is 1～2BV/h.
5. method according to claim 4, the agent of indication desorption and regeneration, optimum desorption temperature is 75 ℃, the desorbing agent flow is 1.2BV/h; Optimum desorbent combination is: 1BV4%NaOH+2BV2%NaOH+2BVH
2O.
6. method according to claim 1, the ND-900 type macroreticular weakly base resin in its characterization step (2) is the macropore weak basic anion exchange resin, strong polarity; Specific surface area 934.0m
2/ g; Average pore diameter 4.5nm; Micropore area 8m
2/ g; Micro pore volume 0.003ml/g; Complete exchange capacity 4.90mmol/g.
7. method according to claim 1, when handling with methyl alcohol, treatment temp is 30～40 ℃, flow is 0.5～1.0BV/h.
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Families Citing this family (14)
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|---|---|---|---|---|
| CN101863573B (en) * | 2010-06-26 | 2011-08-31 | 上海交通大学 | High-concentration naphthalene series dye and chemical oxygen demand cutting method of intermediate wastewater thereof |
| CN102775808B (en) * | 2012-08-23 | 2013-08-21 | 楚源高新科技集团股份有限公司 | Process for recycling ammonium sulfate and synthesizing acidic dye by T-acid mother liquor wastewater |
| CN102863053A (en) * | 2012-09-14 | 2013-01-09 | 东南大学 | Treatment and resource recovery method for treating rinsing wastewater in production process of 2-naphthylamine-3,6,8-trisulfonic acid |
| CN103979730B (en) * | 2014-06-05 | 2015-08-05 | 华东理工大学 | Purify penicillin production waste liquid and the method for reclaim(ed) sulfuric acid sodium |
| CN104086017B (en) * | 2014-06-13 | 2016-03-09 | 通辽市龙盛化工有限公司 | A kind for the treatment of process of H acid segregation waste water |
| CN104743722B (en) * | 2015-03-19 | 2017-01-11 | 上海应用技术学院 | Comprehensive treatment method for high-concentration sodium sulfate wastewater generated in dicumyl peroxide production |
| CN105060565B (en) * | 2015-08-19 | 2017-11-14 | 聊城大学 | A kind of technique of high-efficiency and economic processing J acid mother liquors |
| CN106380023A (en) * | 2016-11-29 | 2017-02-08 | 蓬莱嘉信染料化工股份有限公司 | Decolorization method of disperse dye production wastewater |
| CN108217814A (en) * | 2018-02-12 | 2018-06-29 | 浙江工业大学 | A kind of method using brilliant glue adsorption treatment on sewage |
| CN108911289B (en) * | 2018-07-27 | 2021-06-01 | 南京大学盐城环保技术与工程研究院 | Recovery processing device and method for methanol-containing alkaline resin desorption liquid |
| CN110981059A (en) * | 2019-12-09 | 2020-04-10 | 常州中源工程技术有限公司 | System and process for treating waste water containing sodium sulfate salt and sodium sulfite salt dinaphthol |
| CN111704284B (en) * | 2020-05-29 | 2023-02-17 | 闽南师范大学 | Method for treating 2-amino-8-naphthol-6-sulfonic acid industrial wastewater |
| CN114212947A (en) * | 2021-11-24 | 2022-03-22 | 杭州深瑞水务有限公司 | Process for recycling waste acid containing organic matters |
| CN114291916A (en) * | 2021-12-31 | 2022-04-08 | 天富凯业(辽宁)新材料有限公司 | System and method for recycling o-aminophenol from o-aminophenol acidification wastewater |
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| CN1313247A (en) * | 2000-12-19 | 2001-09-19 | 河南中原环保工程有限公司 | Process for treating waste mother liquid of H acid in dye factory |
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