CN103304055A - Method for treating production wastewater of naphthol AS and derivatives thereof and recovering useful materials therein - Google Patents
Method for treating production wastewater of naphthol AS and derivatives thereof and recovering useful materials therein Download PDFInfo
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- CN103304055A CN103304055A CN201310237513XA CN201310237513A CN103304055A CN 103304055 A CN103304055 A CN 103304055A CN 201310237513X A CN201310237513X A CN 201310237513XA CN 201310237513 A CN201310237513 A CN 201310237513A CN 103304055 A CN103304055 A CN 103304055A
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses a method for treating production wastewater of naphthol AS and derivatives thereof and recovering useful materials therein. The method comprises the following steps of: diluting the production wastewater of naphthol AS and derivatives by using tap water or water obtained after treatment of the method, adjusting the pH value, feeding ferrous sulfate, stirring for flocculation and separating out the precipitate, recovering naphthol AS and derivatives thereof as well as 2,3-acid in the flocculating constituent A2, feeding hydrogen peroxide to the supernatant A1 at a certain pH, stirring for precipitation separation, recovering ferric phosphate in the flocculating constituent B2, supplementing ferrous sulfate and hydrogen peroxide to the supernatant B1, and then performing ultraviolet radiation for certain time, and then carrying out up-to-standard release of the water or using the water as supplementary water for diluting. The method provided by the invention is capable of recovering useful materials in the wastewater while purifying the wastewater, thereby realizing recycling of pollutants. The method has the characteristics of short process flow, good water quality of the final yielding water, simplicity in operation and management, low equipment investment and operating cost and convenience for popularization and application.
Description
Technical field
The invention belongs to the Industrial Wastewater Treatment field, relate in particular to a kind of azoic coupling component AS and derivative production wastewater treatment thereof and reclaim the wherein method of useful matter.
Background technology
Azoic coupling component AS(3-hydroxy-2-naphthoic acid aniline) and derivative be the coupling component of insoluble azo dye, be one of large-tonnage kind of dye industry, its general structure is seen Fig. 1.Azoic coupling component AS(3-hydroxy-2-naphthoic acid aniline) and derivative be not only the primer of insoluble azo dye, also be the intermediate of synthetic organic pigment and dispersed dye.At present there be more than 20 manufacturer in China, basically all is to adopt 2,3-acid (3-hydroxy-2-naphthoic acid) and aniline or derivative to heat with phosphorus trichloride in solvent to form.In addition, the phosphorus trichloride hydrolysis can produce a large amount of orthophosphites, and enters in the middle of this factory effluent.Azoic coupling component AS(3-hydroxy-2-naphthoic acid aniline) and the derivative factory effluent have the water yield little (50-200 ton/sky), concentration is large, color and luster is dark, the phosphoric acid salinity is large, toxicity is large, difficult for biological degradation, is effectively administered so far.Carry out biochemical treatment after the direct discharging of great majority or the dilution, environment is caused serious pollution, the people's life and health is one of important source of pollution of dye industry always around threatening, and has limited greatly the sustainable development of this kind.
At present, less about the bibliographical information of administering azoic coupling component AS and derivative factory effluent thereof both at home and abroad.Strong meter waits the people to adopt the substep acid-precipitation method to process the azoic coupling component mother liquor and reclaim 2,3-acid [strong meter comes, etc. the substep acid-precipitation method is processed azoic coupling component AS and is reclaimed 2,3-acid. chemical industry environmental protection, 1991,11 (1): 28-30].Other people [the Feng Wenguo such as Feng Wenguo, et.al.Treatment of wastewater from production process of2,3-acid.Chinese Journal of Reactive Polymer, 1999,8 (1-2): 68-75], Qiu Yu equality people [Qiu Yuping, Chen Jinlong, Chen Yiliang, Deng. the superhigh cross-linking resin absorption processes 2, the research of 4-D phenolic wastewater. Treatment of Industrial Water, 2003,23 (4): 50-52] and the people [Zhang Weiming such as Zhang Weiming, Deng. resin adsorption method is processed the research of azoic coupling component waste water A S factory effluent. Treatment of Industrial Water, 2005,25 (4): 49-52] and all adopt resin adsorption method to process azoic coupling component AS and derivative factory effluent thereof.Acid-precipitation method need to consume a large amount of strong acid, and higher for the anticorrosion and operational requirement for the treatment of facility, and the waste water after the processing does not reach emission standard yet, polymeric adsorbent is because price is higher, and loading capacity is limited, is difficult to large-scale application, and the removal effect of phosphorus is unsatisfactory.Therefore, azoic coupling component AS and derivative factory effluent thereof still lack cost-effective treatment process.
Summary of the invention
Technical problem to be solved by this invention provides a kind of azoic coupling component AS and derivative production wastewater treatment thereof and reclaims the wherein method of useful matter, method provided by the present invention is when purifying this waste water, recyclable wherein useful matter, realize pollutant resources, and technical process is short, and final outflow water water quality is better, and operational administrative is simple, facility investment and working cost are low, and be easy to utilize.
A kind of azoic coupling component AS provided by the invention and derivative production wastewater treatment thereof also reclaim the wherein method of useful matter, comprising:
The first step: azoic coupling component AS and derivative factory effluent thereof regulate and diluting tank with tap water or present method processing after, final outflow water is according to the certain volume dilution proportion;
Second step: this waste water enters flocculation sedimentation tank after the dilution, be adjusted to proper pH value with alkaline agent or sour agent, add a certain amount of ferrous sulfate, after the certain way stirring, static free setting certain hour, obtain supernatant A 1 and flocs unit A2, flocs unit A2 is used for reclaiming azoic coupling component AS and derivative and 2,3-acid wherein;
The 3rd step: supernatant A 1 enters settling tank, adds a certain amount of hydrogen peroxide, and after stirring according to certain speed, static free setting certain hour obtains supernatant liquor B1 and flocs unit B2, the recyclable tertiary iron phosphate wherein of flocs unit B2;
The 4th step: supernatant liquor B1 enters photochemical reactor, be adjusted to proper pH value with alkaline agent or sour agent, add a certain amount of hydrogen peroxide and ferrous sulfate, under ultraviolet source irradiation, react certain hour, be adjusted to neutrality with alkaline agent and sour agent, final outflow water is discharged or is back to adjusting and diluting tank according to the certain volume ratio.
Azoic coupling component AS and derivative thereof comprise azoic coupling component AS, Naphthol AS-D, Naphthol AS-OL, azoic coupling component AS-RL, azoic coupling component AS-LT, azoic coupling component AS-BG, azoic coupling component AS-BO, azoic coupling component AS-IRT, apthol AS, azoic coupling component AS-SW in the described the first step.
The volume dilution ratio is 1:0.1-1:20 in the described the first step.
Proper pH value is 5-12 in the described second step.
Ferrous sulfate dosage described in the described second step is 1-100g/L.
Alr mode described in the described second step is to stir certain hour with fast stirring velocity first, then stirs certain hour with slow stirring velocity; Fast stirring velocity is 100-2000 rev/min; Slow stirring velocity is 10-100 rev/min; Fast churning time is 0.1 minute-60 minutes; Slow churning time is 0.1 minute-60 minutes.
The static free setting time is 0.1 minute-180 minutes in the described second step.
The hydrogen peroxide dosage is 1-100g/L in described the 3rd step.
Stirring velocity is 10-300 rev/min in described the 3rd step.
The static free setting time is 0.1 minute-120 minutes in described the 3rd step.
The pH regulator alkaline agent was one or more in sodium hydroxide, ammoniacal liquor, calcium hydroxide, the calcium oxide during the described the first step to the four went on foot.
The described the first step to the in four steps pH regulator be in sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, the acid stack gas one or more with sour agent.
Proper pH value is 1-6 in described the 4th step.
Adding the dioxygen water yield in described the 4th step is 0.01-20g/L.
Adding the ferrous sulfate amount in described the 4th step is 0.001-10g/L.
Described the 4th step medium ultraviolet light source is that emission wavelength is contained artificial lamp source or the sunlight between the 280-380nm.
The reaction times is 1-180 minute in described the 4th step.
Be back in described the 4th step and regulate and volume ratio that the final outflow water of diluting tank accounts for final total displacement is 0.1-100%.
The advantage of each functional zone and effect are among the present invention:
1, in the first step azoic coupling component AS and derivative factory effluent thereof regulate and diluting tank process with tap water or present method after final outflow water according to the reason of certain volume dilution proportion be: without dilution, regardless of the pH value, ferrous sulfate can't produce into flocculation.Its mechanism of action is still not clear, and may be to have deflocculated material, or the Pollutants in Wastewater excessive concentration causes, and final outflow water can further reduce the consumption of tap water, minimizing property cost after processing with present method in addition as diluting water.
2, the application of ferrous sulfate is to generate iron hydroxide in the second step, its flocculation ability is stronger, can with water in the suspended substances such as non-water-soluble azoic coupling component AS and derivative thereof organically combine, and accelerate precipitate and separate, and can reclaim wherein azoic coupling component AS and derivative and 2,3-acid thereof.In addition, remain in removal and the UV-Fenton in the 4th step that iron ion in the supernatant liquor can be used for phosphate radical in the 3rd step in this step iron ion catalyst is provided.
3, the effect of hydrogen peroxide is that the orthophosphite that the phosphorus trichloride hydrolysis generates is oxidized to phosphate radical in the 3rd step, thereby generate water-fast tertiary iron phosphate precipitation with iron ion, in addition recycling, in addition, remain in supernatant liquor hydrogen peroxide can for the 4th the step in UV-Fenton oxygenant is provided.
4, adding with ultraviolet source irradiation of hydrogen peroxide and ferrous sulfate used in the 4th step, is to form UV-Fenton advanced oxidation reaction system.This system can generate the hydroxyl free radical with higher oxygen ability, and it can become carbonic acid gas and water with the residual organic matter oxidative degradation among the supernatant liquor B1.
Beneficial effect of the present invention:
Method provided by the present invention is when purifying this waste water, recyclable wherein azoic coupling component AS and derivative, 2 thereof, the useful matteies such as 3-acid and tertiary iron phosphate, realize pollutant resources, and technical process is short, final outflow water water quality is better, satisfy the emission standard requirement fully, operational administrative is simple, and facility investment and working cost are low, and be easy to utilize.
Description of drawings
Fig. 1 is azoic coupling component AS and derivative molecular structural formula thereof.
Fig. 2 is azoic coupling component AS and derivative production wastewater treatment thereof and reclaims the wherein method process flow sheet of useful matter.
Among the figure, 1, adjusting and diluting tank, 2, flocculation sedimentation tank, 3, settling tank, 4, photochemical reactor.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
Azoic coupling component AS factory effluent is taken from the Feicheng, Shandong Province chemical plant, and its water quality characteristic sees Table 1.
The first step: in adjusting and diluting tank 1,50ml azoic coupling component AS factory effluent is diluted according to the 1:10 volume ratio with the 500ml tap water.
Second step: in flocculation sedimentation tank 2, this waste water is regulated pH value to 9.5 with sodium hydroxide after the dilution, add ferrous sulfate according to 20g/L, fast stirring velocity is 300 rev/mins, fast churning time is 5 minutes, and slow stirring velocity is 50 rev/mins, and slow churning time is 10 minutes, static free setting 120 minutes obtains supernatant A 1 and flocs unit A2; Flocs unit A2 is used for reclaiming azoic coupling component AS and derivative and 2,3-acid wherein.
The 3rd step: in settling tank 3, add the 5g/L hydrogen peroxide to supernatant liquor A1, after 50 rev/mins of stirrings, static free setting 30 minutes obtains supernatant liquor B1 and flocs unit B2; The recyclable tertiary iron phosphate wherein of flocs unit B2.
The 4th step: supernatant liquor B1 enters photochemical reactor 4, with sulphur acid for adjusting pH value to 3.0, add 0.1g/L hydrogen peroxide and 0.02g/L ferrous sulfate, reaction is 60 minutes under 100w predominant wavelength 360nm high voltage mercury lamp irradiation, be adjusted to 7.3 with sodium hydroxide, the final outflow water discharging.Final outflow water water quality is referring to table 1.
Table 1: waste water quality contrast before and after processing
Azoic coupling component AS factory effluent is taken from the Feicheng, Shandong Province chemical plant, and its water quality characteristic sees Table 2.
The first step: 50ml azoic coupling component AS factory effluent dilutes according to the 1:10 volume ratio with final outflow water in the 300ml example 1 and 200ml tap water.
Second step, the 3rd step and the 4th go on foot with example 1 in identical; Final outflow water water quality is referring to table 2.
Table 2: waste water quality contrast before and after processing
Azoic coupling component AS-IRT factory effluent is taken from chemical plant, Zhucheng, Shandong Province, and its water quality characteristic sees Table 3.
The first step: 50ml azoic coupling component AS-IRT factory effluent dilutes according to the 1:8 volume ratio with the 400ml tap water.
Second step: this waste water is regulated pH value to 8.7 with sodium hydroxide after the dilution, add ferrous sulfate according to 15g/L, fast stirring velocity is 400 rev/mins, fast churning time is 5 minutes, slow stirring velocity is 80 rev/mins, slow churning time is 50 minutes, and static free setting 90 minutes obtains supernatant A 1 and flocs unit A2; Flocs unit A2 is used for reclaiming azoic coupling component AS-IRT and derivative and 2,3-acid wherein.
The 3rd step: to supernatant liquor A1, add the 2g/L hydrogen peroxide, according to after 100 rev/mins of stirrings, static free setting 20 minutes obtains supernatant liquor B1 and flocs unit B2; The recyclable tertiary iron phosphate wherein of flocs unit B2.
The 4th step: supernatant liquor B1 enters photochemical reactor 4, with sulphur acid for adjusting pH value to 3.0, add 0.2g/L hydrogen peroxide and 0.04g/L ferrous sulfate, reaction is 40 minutes under 100w predominant wavelength 360nm high voltage mercury lamp irradiation, be adjusted to 7.1 with sodium hydroxide, the final outflow water discharging.Final outflow water water quality is referring to table 3.
Table 3: waste water quality contrast before and after processing
Claims (10)
1. an azoic coupling component AS and derivative production wastewater treatment thereof and reclaim the wherein method of useful matter is characterized in that, concrete steps comprise:
The first step: azoic coupling component AS and derivative factory effluent thereof are processed rear final outflow water according to the certain volume dilution proportion in adjusting and diluting tank (1) with tap water or present method;
Second step: this waste water enters flocculation sedimentation tank (2) after the dilution, be adjusted to proper pH value with alkaline agent or sour agent, add ferrous sulfate, after stirring, static free setting, obtain supernatant liquor (A1) and flocs unit (A2), flocs unit (A2) is used for reclaiming azoic coupling component AS and derivative and 2,3-acid wherein;
The 3rd step: supernatant liquor (A1) enters settling tank (3), adds hydrogen peroxide, and after the stirring, static free setting obtains supernatant liquor (B1) and flocs unit (B2), the recyclable tertiary iron phosphate wherein of flocs unit (B2);
The 4th step: supernatant liquor (B1) enters photochemical reactor (4), be adjusted to proper pH value with alkaline agent or sour agent, add hydrogen peroxide and ferrous sulfate, under ultraviolet source irradiation, react, be adjusted to neutrality with alkaline agent and sour agent, final outflow water is discharged or is back to and regulates and diluting tank (1).
2. a kind of azoic coupling component AS and the derivative production wastewater treatment thereof described in according to claim 1 and reclaim the wherein method of useful matter, it is characterized in that: azoic coupling component AS and derivative thereof comprise azoic coupling component AS in the described the first step, Naphthol AS-D, Naphthol AS-OL, azoic coupling component AS-RL, azoic coupling component AS-LT, azoic coupling component AS-BG, azoic coupling component AS-BO, azoic coupling component AS-IRT, apthol AS, azoic coupling component AS-SW.
3. a kind of azoic coupling component AS and the derivative production wastewater treatment thereof described in according to claim 1 and reclaim the wherein method of useful matter, it is characterized in that: the volume dilution ratio is 1:0.1-1:20 in the described the first step.
4. a kind of azoic coupling component AS and the derivative production wastewater treatment thereof described in according to claim 1 and reclaim the wherein method of useful matter, it is characterized in that: proper pH value is 5-12 in the described second step.
5. a kind of azoic coupling component AS and the derivative production wastewater treatment thereof described in according to claim 1 and reclaim the wherein method of useful matter, it is characterized in that: ferrous sulfate dosage described in the described second step is 1-100g/L.
6. a kind of azoic coupling component AS and the derivative production wastewater treatment thereof described in according to claim 1 and reclaim the wherein method of useful matter, it is characterized in that: then the alr mode described in the described second step stirs with slow stirring velocity for stirring with fast stirring velocity first.
7. the method described in according to claim 6, it is characterized in that: fast stirring velocity is 100-2000 rev/min, and slow stirring velocity is 10-100 rev/min, and fast churning time is 0.1 minute-60 minutes, and slow churning time is 0.1 minute-60 minutes.
8. a kind of azoic coupling component AS and the derivative production wastewater treatment thereof described in according to claim 1 and reclaim the wherein method of useful matter, it is characterized in that: the pH regulator alkaline agent is one or more in sodium hydroxide, ammoniacal liquor, calcium hydroxide, the calcium oxide in described first to fourth step.
9. a kind of azoic coupling component AS and the derivative production wastewater treatment thereof described in according to claim 1 and reclaim the wherein method of useful matter is characterized in that: pH regulator is in sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, the acid stack gas one or more with sour agent in described first to fourth step.
10. a kind of azoic coupling component AS and the derivative production wastewater treatment thereof described in according to claim 1 and reclaim the wherein method of useful matter, it is characterized in that: proper pH value is 1-6 in described the 4th step, adding the dioxygen water yield is 0.01-20g/L, and adding the ferrous sulfate amount is 0.001-10g/L; Ultraviolet source is that emission wavelength is contained artificial lamp source or the sunlight between the 280-380nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104447393A (en) * | 2014-11-28 | 2015-03-25 | 济宁阳光化学有限公司 | Method for producing naphthol AS and recycling wastes |
| CN105906527A (en) * | 2015-09-15 | 2016-08-31 | 雷玉金 | Naphthol AS mother liquor recovery method |
| CN109019542A (en) * | 2018-07-01 | 2018-12-18 | 湖北浩元材料科技有限公司 | The recycling of wastewater treatment method and valuables |
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Cited By (4)
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| CN104447393A (en) * | 2014-11-28 | 2015-03-25 | 济宁阳光化学有限公司 | Method for producing naphthol AS and recycling wastes |
| CN105906527A (en) * | 2015-09-15 | 2016-08-31 | 雷玉金 | Naphthol AS mother liquor recovery method |
| CN109019542A (en) * | 2018-07-01 | 2018-12-18 | 湖北浩元材料科技有限公司 | The recycling of wastewater treatment method and valuables |
| CN109019542B (en) * | 2018-07-01 | 2022-02-25 | 湖北浩元材料科技有限公司 | Method for treating waste water and recovering valuable substances |
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