CN111777238A - Integrated treatment process for 3, 6-dichlorosalicylic acid synthetic wastewater - Google Patents
Integrated treatment process for 3, 6-dichlorosalicylic acid synthetic wastewater Download PDFInfo
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- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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Abstract
The invention discloses an integrated treatment process of 3, 6-dichlorosalicylic acid synthetic wastewater, which solves the defect of unstable system operation in the prior art. The specific process comprises the following steps: 3, 6-dichloro salicylic acid synthetic wastewater is subjected to homogenization, Fenton oxidation, electrocoagulation-flotation treatment, advanced fine filtration, electrocatalytic oxidation and DTRO water treatment in sequence, so that the serious phenomenon of secondary pollution after treatment is reduced, the discharge amount is reduced, the near-zero emission purpose is realized, and further the water resource is saved. The invention provides a stable combined system process technology. The wastewater treated by the process can reach the national emission standard, realizes the process advantages of high treatment efficiency, water resource saving, stable operation, convenient maintenance and the like, and really solves the problem of difficult treatment of the wastewater in the production of 3, 6-dichlorosalicylic acid.
Description
Technical Field
The invention belongs to the technical field of wastewater treatment, and particularly relates to an integrated treatment process of 3, 6-dichlorosalicylic acid synthetic wastewater.
Background
The main components of the 3, 6-dichlorosalicylic acid synthetic wastewater comprise high molecular organic substances such as 2, 5-dichloroaniline, 2, 5-dichlorophenol, o-xylene and the like, and Na2SO4、K2CO3Inorganic salts, the water quantity is 15T/day, the water quality is acidic, the appearance is light yellow, the COD is about 1000mg/L, and the ammonia nitrogen is 15 mg/L; the waste water has low ss value, low water quantity and poor biochemical property, and the contained organic matters are difficult to decompose and difficult to reach the standard.
The wastewater belongs to chemical wastewater which is difficult to treat, and the selection of treatment process technology is the key of construction and normal operation of the project. Whether the treatment process is reasonable or not is directly related to the treatment effect of the wastewater, the quality of the discharged water, the operation stability, the investment, the operation cost, the management operation level and the like. Therefore, the practical situation must be combined, all factors should be considered, and the proper treatment process should be carefully selected to achieve the best treatment effect and economic benefit
The treatment method is different due to different compositions, acidity and alkalinity and concentration of the waste water containing phenol and benzene, and the current industrial treatment methods of the waste water containing phenol and benzene are generally divided into three major methods, namely physical chemical methods, biochemical methods and the like. The most common methods are mainly described. The domestic process technology for the 3, 6-dichlorosalicylic acid production wastewater comprises the following steps:
1. flocculation air flotation, micro-electrolysis, dilution and biochemistry: the defects are that (1) the occupied area is large, and (2) the system stability is poor, the water outlet index is not easy to reach the standard, and the water resource waste is caused.
2. Neutralization precipitation, ozone oxidation, chemical oxidation, dilution and biochemistry: the defects are that (1) the occupied area is large, (2) the system stability is poor, the effluent quality is not easy to reach the standard, and (3) the water resource is wasted.
3. The resin adsorption method treatment process comprises the following steps: the advantages are (1) the process line is short and short, and (2) the occupied area is small; the disadvantages are (1) complex operation and poor controllability of the system and (2) secondary pollution.
In actual operation, the above methods have obvious defects, cause great troubles to the normal operation of production of enterprises, and bring great pressure to the environmental protection work of the enterprises; therefore, there is a need for a simple and practical method for treating waste water containing phenol and formaldehyde to reach the discharge standard. And the operation is easy in the operation process, the occupied area is small, the operation is stable, and the like.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an integrated treatment process of 3, 6-dichlorosalicylic acid synthetic wastewater, which really solves the problem of difficult treatment of 3, 6-dichlorosalicylic acid production wastewater.
In order to solve the technical problems, the invention adopts the following technical scheme:
an integrated treatment process of 3, 6-dichlorosalicylic acid synthetic wastewater comprises the following steps:
(1) homogenizing: wastewater generated in the production process of 3, 6-dichlorosalicylic acid firstly enters a homogenizing tank, and liquid alkali is added to adjust the pH = 5-6; the homogenizing tank has the function of precipitation, and the precipitated solid is removed periodically;
(2) fenton oxidation: pumping the homogenized wastewater into a Fenton oxidation treatment system for Fenton oxidation after passing through a coarse filter;
(3) electric flocculation air flotation treatment: pumping effluent of the Fenton oxidation system into an electrocoagulation treatment system for electrocoagulation-flotation treatment;
(4) high-level precise filtration: performing efficient precise filtration on the effluent after the electrocoagulation-flotation treatment, and further reducing the SS of a water system after the filtration;
(5) electrocatalytic oxidation: the high-grade precision filtered water is pumped into an electro-catalytic oxidation system for electro-catalytic oxidation;
(6) DTRO water treatment: the effluent of the electrocatalytic oxidation enters a DTRO water treatment system, purified water (85%) is collected in a water storage tank after being treated by the DTRO water treatment system, and the purified water is recycled for production after being detected to meet the indexes of process water for production; part of the concentrated water (15%) flows back to the front-stage Fenton oxidation system, and deep circulation treatment is continuously carried out.
Further, the 3, 6-dichlorosalicylic acid synthetic wastewater is diazonium salt hydrolysis, water washing wastewater and o-xylene recovery dilution wastewater generated in the 3, 6-dichlorosalicylic acid production process.
Further, the Fenton oxidation Fenton reagent in the step (2) is selected from hydrogen peroxide and ferrous sulfate, the hydrogen peroxide is 35% of industrial-grade hydrogen peroxide in mass fraction, the adding amount is equimolar amount of chemical oxygen demand, the molar ratio of the ferrous sulfate to the hydrogen peroxide is 1:1.2, and the oxidation reaction time is 2.5 hours.
Further, in the step (3), electric flocculation air flotation treatment is carried out, and AL is selected as an anode plate; a variable-pole direct-current electrode plate is adopted, and PAS and PAM are selected as flocculating agents.
Further, the filter element of the high-grade precise filtering system in the step (4) is made of PP material, the filtering precision is 0.5um, and the SS of the water system is further reduced after filtering.
Further, in the step (5), the pH of the inlet water is adjusted to be 6.5-7.5, 30% of hydrogen peroxide is used as an oxidant of an electrocatalytic oxidation system, the addition amount of the hydrogen peroxide is 30mg/L, and the current density is 20-30mA/cm2And the catalytic oxidation retention time is 10-30 min.
Further, in the step (6), two-stage DTRO filtration is adopted, a disc type tubular membrane is adopted as an ultrafiltration membrane, the pressure resistance value is 25-50 MPa, and the temperature of inlet water is ensured to be above 5 ℃.
The invention has the beneficial effects that: the invention solves the defects of imperfect and unreasonable system configuration of the prior 3, 6-dichlorosalicylic acid production wastewater treatment technology. The serious phenomenon of secondary pollution after treatment is reduced. The defect of unstable system operation in the prior art is solved. Reduce the discharge amount, realize the near zero emission purpose and further save water resources. The invention provides a stable combined system process technology. The wastewater treated by the process can reach the national emission standard, realizes the process advantages of high treatment efficiency, water resource saving, stable operation, convenient maintenance and the like, and really solves the problem of difficult treatment of the wastewater in the production of 3, 6-dichlorosalicylic acid.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.
Example 1
As shown in fig. 1, the integrated treatment process of the 3, 6-dichlorosalicylic acid synthetic wastewater of the present example is as follows:
(1) firstly, enabling diazonium salt generated in the production process of 3, 6-dichlorosalicylic acid to hydrolyze, wash waste water and recycle suction filtration mother liquor waste water to enter a homogenizing tank, and adding liquid caustic soda to adjust the pH = 5-6; the homogenizing tank has the function of precipitation, and the precipitated solid is removed periodically;
(2) filtering the homogenized wastewater by a coarse filter, pumping the wastewater into a Fenton oxidation treatment system, selecting hydrogen peroxide and ferrous sulfate as Fenton reagents, wherein the hydrogen peroxide is 35% of industrial-grade hydrogen peroxide in mass fraction, the adding amount is equimolar amount of chemical oxygen demand, the molar ratio of the ferrous sulfate to the hydrogen peroxide is 1:1.2, and the oxidation reaction time is 2.5 hours; detecting water indexes after stable operation of the project: the COD removal rate is 55 percent, and the BOD removal rate is 65 percent.
(3) Pumping the effluent of the Fenton system into an electric flocculation treatment system, and selecting AL as an anode plate; PAS and PAM are selected as flocculating agents, and the water indexes are detected as follows: the COD removal rate is 50 percent, the BOD removal rate is 45 percent, the removal rate of suspended matters and turbidity reaches more than 85 percent, and the chroma is reduced by about 80 percent.
(4) The clear water after filtering and deslagging enters a high-grade filtering system, a filter element is made of PP material, the filtering precision is 0.5 mu m, the SS of a water system is further reduced after filtering, and the detected SS average value of the effluent is 100-plus 150mg/L, and the effluent is pumped into an electrocatalytic oxidation system.
(5) Adjusting pH of inlet water to about =7.0, selecting 30% hydrogen peroxide as oxidant of electrocatalytic oxidation system, adding 30mg/L, and current density of about 20-30mA/cm2The catalytic oxidation retention time is 10-30 min, the COD removal rate is 75%, and the effluent passes throughThe cartridge filter is pumped into the DTRO water treatment system under high pressure.
(6) The DTRO water treatment system adopts two-stage DTRO filtration, the ultrafiltration membrane adopts a disc type tubular membrane, the pressure resistance value is 25-50 MPa, and the temperature of inlet water is ensured to be above 5 ℃; collecting purified water (85%) in a water storage tank, and recycling production after detecting that the purified water meets the indexes of process water for production; part of the concentrated water (15%) flows back to the front-stage Fenton oxidation system, and deep circulation treatment is continuously carried out.
After the 3, 6-dichlorosalicylic acid production wastewater is treated by the treatment process combined system, near zero emission is basically realized, the automation degree of system operation is higher, and the stability is good! The defect investment cost is slightly higher, the operation cost is higher, but because the production ton water amount is smaller, the mixed wastewater has definite components and low COD, the total treatment cost is in an economic and controllable range, and the treatment process is a better choice for the wastewater produced by 3, 6-dichlorosalicylic acid from the viewpoint of environmental protection and once and for all.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. An integrated treatment process of 3, 6-dichlorosalicylic acid synthetic wastewater is characterized by comprising the following steps:
(1) homogenizing: wastewater generated in the production process of 3, 6-dichlorosalicylic acid firstly enters a homogenizing tank, and liquid alkali is added to adjust the pH = 5-6;
(2) fenton oxidation: pumping the homogenized wastewater into a Fenton oxidation treatment system for Fenton oxidation after passing through a coarse filter;
(3) electric flocculation air flotation treatment: pumping effluent of the Fenton oxidation system into an electrocoagulation treatment system for electrocoagulation-flotation treatment;
(4) high-level precise filtration: performing efficient precise filtration on the effluent after the electrocoagulation-flotation treatment, and further reducing the SS of a water system after the filtration;
(5) electrocatalytic oxidation: the high-grade precision filtered water is pumped into an electro-catalytic oxidation system for electro-catalytic oxidation;
(6) DTRO water treatment: the effluent of the electrocatalytic oxidation enters a DTRO water treatment system, is treated by the DTRO water treatment system, and then is collected in a water storage tank, and is recycled for production after being detected to meet the indexes of process water for production; and part of the concentrated water flows back to the front-section Fenton oxidation system, and deep circulation treatment is continuously carried out.
2. The integrated treatment process of 3, 6-dichlorosalicylic acid synthetic wastewater according to claim 1, characterized in that: the 3, 6-dichlorosalicylic acid synthetic wastewater is diazonium salt hydrolysis, water washing wastewater and o-xylene recovery dilution wastewater generated in the 3, 6-dichlorosalicylic acid production process.
3. The integrated treatment process of 3, 6-dichlorosalicylic acid synthetic wastewater according to claim 1, characterized in that: in the step (2), hydrogen peroxide and ferrous sulfate are selected as Fenton oxidation Fenton reagents, wherein the hydrogen peroxide is 35% of industrial-grade hydrogen peroxide in mass fraction, the adding amount is equal molar amount of chemical oxygen demand, the molar ratio of the ferrous sulfate to the hydrogen peroxide is 1:1.2, and the oxidation reaction time is 2.5 hours.
4. The integrated treatment process of 3, 6-dichlorosalicylic acid synthetic wastewater according to claim 1, characterized in that: and (3) performing electric flocculation air floatation treatment, wherein AL is selected as an anode plate, and PAS and PAM are selected as flocculating agents.
5. The integrated treatment process of 3, 6-dichlorosalicylic acid synthetic wastewater according to claim 1, characterized in that: and (4) selecting a filter element of the high-grade filtration system from PP material, wherein the filtration precision is 50 μm.
6. 3, 6-dichloro-water according to claim 1The integrated treatment process of the salicylic acid synthetic wastewater is characterized by comprising the following steps of: in the step (5), the pH of the inlet water is adjusted to be 6.5-7.5, the oxidant of the electrocatalytic oxidation system is 30% of hydrogen peroxide by mass fraction, the addition amount is 30mg/L, and the current density is about 20-30mA/cm2And the catalytic oxidation retention time is 10-30 min.
7. The integrated treatment process of 3, 6-dichlorosalicylic acid synthetic wastewater according to claim 1, characterized in that: and (3) filtering by adopting two-stage DTRO (double-stage reverse osmosis) in the step (6), wherein the ultrafiltration membrane adopts a disc type tubular membrane, the pressure resistance value is 25-50 MPa, and the temperature of inlet water is ensured to be above 5 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN204702628U (en) * | 2015-05-27 | 2015-10-14 | 苏州澄江节能科技有限公司 | Water color ink liquid waste treatment system |
| CN111423032A (en) * | 2020-03-31 | 2020-07-17 | 埃尔博工业设备(北京)有限公司 | Treatment method of CTP (computer to plate) flushing water in printing factory |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN204702628U (en) * | 2015-05-27 | 2015-10-14 | 苏州澄江节能科技有限公司 | Water color ink liquid waste treatment system |
| CN111423032A (en) * | 2020-03-31 | 2020-07-17 | 埃尔博工业设备(北京)有限公司 | Treatment method of CTP (computer to plate) flushing water in printing factory |
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