CN107417022A - A kind of EDTA crystalline mother solutions waste water treatment and reclamation technology - Google Patents
A kind of EDTA crystalline mother solutions waste water treatment and reclamation technology Download PDFInfo
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- CN107417022A CN107417022A CN201710365175.6A CN201710365175A CN107417022A CN 107417022 A CN107417022 A CN 107417022A CN 201710365175 A CN201710365175 A CN 201710365175A CN 107417022 A CN107417022 A CN 107417022A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/34—Treatment of water, waste water, or sewage with mechanical oscillations
- C02F1/36—Treatment of water, waste water, or sewage with mechanical oscillations ultrasonic vibrations
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Organic Chemistry (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention relates to EDTA crystalline mother solution waste water treatment and reclamation technologies, ultrafiltration membrance filter processing is carried out after EDTA crystalline mother solutions are adjusted into pH, it is ultrasonically treated while ultrafiltration membrance filter, milipore filter penetrating fluid enters nanofiltration system and removes a small amount of calcium and magnesium plasma, milipore filter trapped fluid carries out EDTA recyclings, nanofiltration water outlet enters catalytic ozonation system and removes useless Organic substance in water, and catalytic ozonation water outlet is evaporated crystallization, the inorganic salts in waste water are recycled.The present invention is using membrane filtration coupling ultrasonic technology, catalytic ozonation, evaporative crystallization combined treatment process, not only realize the processing up to standard of waste water, the recycling of waste water is also achieved simultaneously, the rate of recovery of EDTA fine crystals is improved, there is the advantages of technique is advanced, efficiency high and effect stability are reliable.
Description
Technical field
The invention belongs to environmentally friendly water-treatment technology field, is related to a kind of EDTA crystalline mother solutions waste water treatment and reclamation technology.
Background technology
EDTA（Ethylenediamine tetra-acetic acid）Purposes is extremely wide, is a kind of important complexing agent, can be used as bleach-fixing liquid, dye
Color auxiliary agent, fibre finish, cosmetic additive agent etc., EDTA are also a kind of excellent chelating agent simultaneously.In EDTA production processes
Generation obtains EDTA-4Na in the basic conditions first, is then acidified to obtain EDTA products, the meeting in last crystallization processes
Crystalline mother solution waste water is produced, the water salt content is high, COD contents are high, can also seriously be polluted containing some EDTA, its discharge of wastewater
Environment.Sheet frame and band filter fractional crystallization for crystalline mother solution generally use, separative efficiency is not high, there is penetration phenomenon,
Loss is serious, therefore seeks suitable handling process and be very important.
The existing correlation technique report of processing on the waste water containing EDTA at present.
The Chinese invention patent of Application No. 201210439748.2 provides a kind of Cu（Ⅱ）The processing side of-EDTA waste water
Method, first regulation wastewater pH to 3 ~ 6, then add catalyst and carry out oxidation processes, the waste water regulation pH to 11 ~ 12 after oxidation,
Cupric oxide is reclaimed, reaches the degraded of wastewater through organic matter and the recycling of copper, there are environmental protection and economical effects.
The Chinese invention patent of Application No. 201410336973.2 provides a kind of process for producing EDTA and produces waste water
Method, waste water is handled using the method for extraction, crystallization treatment is evaporated to the waste water after extraction, this method is first taken out
Organic matter in waste water is then evaporated processing, improves evaporation effect, reduces production cost.
The Chinese invention patent of Application No. 201310522414.6 provides a kind of method for removing EDTA in waste water, adopts
Wastewater treatment is carried out with the method including ultraviolet radioactive oxidation, flocculation sediment, pH readjustments, wastewater treatment expense is reduced, subtracts
Few process cycle.
Above-mentioned processing procedure is leading with chemical treatment, and a large amount of chemistry examinations of extra addition are needed in chemical treating process
Agent is effectively to remove COD etc. in waste water, but a large amount of additions of chemical reagent cause secondary pollution and add wastewater treatment hardly possible
Degree and cost input height, long processing period, and because salt content is high, COD is high in EDTA crystalline mother solution waste water and contains a small amount of
The characteristics of EDTA, the above method are difficult to the recovery of Nacl and EDTA recovery, serious waste of resources.
In addition, Membrane Separation for Water Treatment is applied to field of industrial waste water treatment more and more widely, waste water is through ultrafiltration
The solid and part COD in waste water can be effectively removed after processing, therefore, increasing chemical wastewater treatment begins to focus on film
The application of technology is to improve treatment effeciency and effect.
The Chinese invention patent of Application No. 200610147820.9 is related to a kind of Chemical Pretreatment and joined with film processing system
The method for closing processing EDTA chemical rinsing waste waters, is characterized in, being firstly added highly basic makes the heavy metal in waste water with precipitation form
Remove, then adding strong acid separates out most of EDTA, then carries out subsequent treatment with membranous system, makes at EDTA chemical rinsing waste waters
Manage up to standard.The patent application has following features：1. its main body being directed to is EDTA chemical rinsing waste waters, therefore is contained in waste water
A large amount of EDTA；2. salt content is low in its main body being directed to or nothing；3. except reclaiming most of EDTA, remaining resource can not be had
Imitate recycling, serious waste of resources；4. the invented technology is not suitable for, salt content is high, COD contents are high and contain some
The processing of EDTA EDTA production crystalline mother solutions and resource reclaim.
It is rarely reported at present on EDTA crystalline mother solution wastewater treatment and reuse technologies, for the plate of crystalline mother solution generally use
Frame and band filter fractional crystallization, separative efficiency is not high, has penetration phenomenon, loss is serious, therefore seeks suitably to handle work
Skill is very important.
Present invention firstly provides membrane technology and the technologies such as ultrasound are integrated, and with the coupling of evaporative crystallization technique, it is intended to
EDTA crystalline mother solution wastewater treatment and reuse technologies are developed, there will be conventional waste water treatment technology in wastewater treatment and feed liquid recovery
Unrivaled advantage.The characteristics of for the high COD of EDTA crystalline mother solution waste water, high salinity, using membrane separation process, ultrasonic method,
The techniques such as catalytic ozonation method cleverly combine, and can be achieved to EDTA crystalline mother solutions waste water and effectively handle and realize that resource is returned
Receive.
The content of the invention
The purpose of the present invention is to be directed to EDTA crystallizations in EDTA crystalline mother solution waste water recycling processing procedures to lose serious, separation
This low problem of efficiency, EDTA crystalline mother solution waste water treatment and reclamation technologies are proposed, pass through ultrasound and the combination work of membrane separation technique
Skill improves resource utilization to improve the rate of recovery of EDTA crystallizations.
The EDTA crystalline mother solution waste water treatment and reclamation technologies that technical scheme proposes, it is comprised the following steps that：
1）PH regulations are carried out to EDTA crystalline mother solutions waste water；
2）The waste water after pH is adjusted into the processing of ultrafiltration ultrasonic system, trapped fluid enters EDTA recovery units, and penetrating fluid, which enters, to be received
Filter processing unit；
3）Nanofiltration processing is carried out to the penetrating fluid after hyperfiltration treatment, concentrate delivers to pH adjustment units, and per-meate side water outlet enters smelly
Oxygen catalytic oxidation system；
4）Catalytic ozonation processing is carried out to the water outlet of nanofiltration per-meate side, useless Organic substance in water is removed with further；
5）Crystallization treatment is evaporated to the waste water after catalytic ozonation, obtains Nacl, evaporation condensed water returns into technique
Water system.
In above-mentioned EDTA crystalline mother solution waste water treatment and reclamation technologies, pH is adjusted to 3- to crystalline mother solution using hydrochloric acid
7, EDTA in system is further separated out complete.
In above-mentioned EDTA crystalline mother solution waste water treatment and reclamation technologies, in ultrafiltration ultrasonic procedure, ultrafiltration pressure be 0.03 ~
0.4MPa, milipore filter are inorganic ceramic membrane or organic hollow fiber film, preferably ceramic film, Average Pore Size of UF Membrane is 10 ~
200nm, membrane module are tubular type or hollow fiber form；In ultra-filtration process simultaneously be ultrasonically treated online, supersonic frequency be 30 ~
100KHz。
In above-mentioned EDTA crystalline mother solution waste water treatment and reclamation technologies, in nanofiltration process, nanofiltration pressure is 0.4 ~ 0.8MPa,
NF membrane is inoranic membrane or organic film, and film average pore size is 1 ~ 5nm, and membrane module is tubular type, rolling or hollow-fibre membrane.
In above-mentioned EDTA crystalline mother solution waste water treatment and reclamation technologies, during catalytic ozonation, ozone dosage is
10 ~ 100g/h, catalyst are the one or more in the metal oxides such as Al2O3 loads Fe, Mn, Ni, Ce, La, and catalyst is thrown
Dosage is 0.1 ~ 6wt.% of reaction system, and the residence time of accessing pending water in a device is 60 ~ 240min.
In above-mentioned EDTA crystalline mother solution waste water treatment and reclamation technologies, evaporation process is multi-effect evaporator and mechanical vapour pressure
Contracting machine（MVR）One kind in evaporator, 50 ~ 180 DEG C of operation temperature, operating pressure are 0.1 ~ 200kPa.
Pass through above-mentioned technical proposal, the present invention propose ultra-filtration stage carry out being ultrasonically treated online online removing film surface and
Fine crystalline particle in hole, the EDTA fine crystals rate of recovery 0.1 ~ 3% can be improved；Can using UF membrane and catalytic ozonation
Efficiently to remove the COD materials in waste water, and evaporation technique is combined, can effectively reclaim evaporation water and inorganic salts, improve resource
Recycling rate of waterused.
Brief description of the drawings
Fig. 1 is EDTA crystalline mother solution waste water treatment and reclamation technical matters flow charts.
Embodiment
Embodiment 1：
Take EDTA crystalline mother solutions（Mainly contain inorganic salts 15%, EDTA 1.5%, organic matter 0.8%）, use salt acid for adjusting pH to 3
So that the EDTA in crystalline mother solution is further separated out completely, ultrafiltration supersound process is carried out to the crystalline mother solution after regulation pH, used
The tubular ceramic membrane that membrane aperture is 200nm filters under conditions of transmembrane pressure is 0.03MPa, supersonic frequency 30KHz, retention
Liquid carries out EDTA crystallization recovery；Containing inorganic salts 15%, organic matter 0.8% in penetrating fluid after hyperfiltration treatment, pass through high-pressure pump
Nanofiltration membrane system is delivered to, uses average pore size to carry out concentration for 5nm ceramic hollow fibrous membrane, in transmembrane pressure
To be filtered under the conditions of 0.4MP, a small amount of calcium and magnesium plasma is removed；It is single that nanofiltration per-meate side production water enters catalytic ozonation processing
Member, catalyst is used as alumina load manganese oxide, dosage 0.1wt.%, ozone dosage 10g/h, the residence time is
60min；Waste water after catalytic ozonation, containing inorganic salts 15%, into evaporation element, evaporation process uses triple effect evaporator, operation
Temperature 50 C, operating pressure 0.1kPa, the Nacl obtained after evaporation, water vapor condensation water caused by evaporation element enter work
Skill reuse water system.
Embodiment 2：
Take EDTA crystalline mother solutions（Mainly contain inorganic salts 18%, EDTA 0.5%, organic matter 0.3%）, use salt acid for adjusting pH to 5
So that the EDTA in crystalline mother solution is further separated out completely, ultrafiltration supersound process is carried out to the crystalline mother solution after regulation pH, used
The tubular ceramic membrane that membrane aperture is 100nm filters under conditions of transmembrane pressure is 0.2MPa, supersonic frequency 40KHz, retention
Liquid carries out EDTA crystallization recovery；Containing inorganic salts 15%, organic matter 0.1% in penetrating fluid after hyperfiltration treatment, pass through high-pressure pump
Nanofiltration membrane system is delivered to, uses average pore size to carry out concentration for 3nm hollow-fibre membrane, is in transmembrane pressure
Filtered under the conditions of 0.2MP, remove a small amount of calcium and magnesium plasma；It is single that nanofiltration per-meate side production water enters catalytic ozonation processing
Member, catalyst is used as alumina load lanthana, dosage 1wt.%, ozone dosage 50g/h, the residence time is
240min；Waste water contains inorganic salts 15% after catalytic ozonation, and into evaporation element, evaporation process uses Mechanical Vapor Compression
（MVR）Evaporator, 130 DEG C, operating pressure 150kPa of operation temperature, the Nacl obtained after evaporation, caused by evaporation element
Water vapor condensation water enters technique reuse water system.
Embodiment 3：
Take EDTA crystalline mother solutions（Mainly contain inorganic salts 13%, EDTA 0.7%, organic matter 0.6%）, use salt acid for adjusting pH to 7
So that the EDTA in crystalline mother solution is further separated out completely, ultrafiltration supersound process is carried out to the crystalline mother solution after regulation pH, used
The tubular ceramic membrane that membrane aperture is 10nm filters under conditions of transmembrane pressure is 0.4MPa, supersonic frequency 100KHz, retention
Liquid carries out EDTA crystallization recovery；Containing inorganic salts 13%, organic matter 0.2% in penetrating fluid after hyperfiltration treatment, pass through high-pressure pump
Nanofiltration membrane system is delivered to, uses average pore size to carry out concentration for 1nm rolled film, is 0.8MP in transmembrane pressure
Under the conditions of filtered, remove a small amount of calcium and magnesium plasma；Nanofiltration per-meate side production water enters catalytic ozonation processing unit, uses
Catalyst is alumina load cerium oxide, dosage 6wt.%, ozone dosage 100g/h, residence time 180min；Ozone
Waste water contains inorganic salts 13% after catalysis oxidation, and into evaporation element, evaporation process uses Mechanical Vapor Compression（MVR）Evaporator,
180 DEG C, operating pressure 200kPa of operation temperature, the Nacl obtained after evaporation, water vapor condensation water caused by evaporation element
Into technique reuse water system.
The foregoing description of the disclosed embodiments, professional and technical personnel in the field are enable to realize or using the present invention.
A variety of modifications to above-described embodiment will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope caused.
Claims (6)
1. a kind of EDTA crystalline mother solutions waste water treatment and reclamation technology, it is characterised in that comprise the following steps：
1）PH regulations are carried out to EDTA crystalline mother solutions waste water；
2）The waste water after pH is adjusted into the processing of ultrafiltration ultrasonic system, trapped fluid enters EDTA recovery units, and penetrating fluid, which enters, to be received
Filter processing unit；
3）Nanofiltration processing is carried out to the penetrating fluid after hyperfiltration treatment, concentrate delivers to pH adjustment units, and per-meate side water outlet enters smelly
Oxygen catalytic oxidation system；
4）Catalytic ozonation processing is carried out to the water outlet of nanofiltration per-meate side, useless Organic substance in water is removed with further；
5）Crystallization treatment is evaporated to the waste water after catalytic ozonation and obtains Nacl, evaporation condensed water returns into technique
Water system.
A kind of 2. EDTA crystalline mother solutions waste water treatment and reclamation technology according to claim 1, it is characterised in that step 1）
In, use salt acid for adjusting pH to 3 ~ 7.
A kind of 3. EDTA crystalline mother solutions waste water treatment and reclamation technology according to claim 1, it is characterised in that step 2）
In, ultrafiltration ultrasonic system is coupled using ultrafiltration with ultrasound, and hyperfiltration treatment operating pressure is 0.03 ~ 0.4MPa, and milipore filter is put down
Equal aperture is 10 ~ 200nm, and membrane module is tubular type or hollow fiber form；It is ultrasonically treated, is surpassed online simultaneously in ultra-filtration process
Acoustic frequency is 30 ~ 100KHz.
A kind of 4. EDTA crystalline mother solutions waste water treatment and reclamation technology according to claim 1, it is characterised in that step 3）
In, nanofiltration processing operating pressure is 0.4 ~ 0.8MPa, and NF membrane average pore size is 1 ~ 5nm, and membrane module is tubular type, rolling or hollow
Fiber type.
A kind of 5. EDTA crystalline mother solutions waste water treatment and reclamation technology according to claim 1, it is characterised in that step 4）
In, ozone air inflow is 10g/h ~ 100g/h, and catalyst is one in the metal oxides such as Al2O3 loads Fe, Mn, Ni, Ce, La
Kind or it is several, catalyst amountses be reaction system 0.1 ~ 6wt.%, the residence time of accessing pending water in a device be 60 ~
240min。
A kind of 6. EDTA crystalline mother solutions waste water treatment and reclamation technology according to claim 1, it is characterised in that step 5）
In, evaporation and crystal process uses multi-effect evaporator and Mechanical Vapor Compression（MVR）One kind in evaporator, operation temperature 50 ~
180 DEG C, operating pressure is 0.1 ~ 200KPa.
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| CN201710365175.6A CN107417022A (en) | 2017-05-22 | 2017-05-22 | A kind of EDTA crystalline mother solutions waste water treatment and reclamation technology |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116675396A (en) * | 2023-08-01 | 2023-09-01 | 成都瀚川环境科技有限公司 | Organic wastewater treatment system |
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| CN2848838Y (en) * | 2005-12-29 | 2006-12-20 | 东华大学 | Nano-filtering membrane composite deep water purification device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116675396A (en) * | 2023-08-01 | 2023-09-01 | 成都瀚川环境科技有限公司 | Organic wastewater treatment system |
| CN116675396B (en) * | 2023-08-01 | 2023-11-10 | 成都瀚川环境科技有限公司 | Organic wastewater treatment system |
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Effective date of registration: 20180622 Address after: 210000 Jiangbei new district, Nanjing, Jiangsu, No. 1 Applicant after: Nanjing Institute of Membrane Applied Technology Research Institute Co., Ltd. Address before: 215300 508B, No. 268, Deng Yun Road, Yushan Town, Kunshan, Suzhou, Jiangsu. Applicant before: Jiangsu Hui Fang Environmental Technology Co., Ltd. |
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Application publication date: 20171201 |