CN103663774A - Method for treating low-concentration ammonia-containing wastewater by use of membrane separation technology - Google Patents
Method for treating low-concentration ammonia-containing wastewater by use of membrane separation technology Download PDFInfo
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Abstract
The invention relates to a treatment method for low-concentration ammonia-containing wastewater, and particularly relates to a technical method taking a membrane separation technology as a core treatment unit. Low-concentration ammonia-containing wastewater often occurs in the production process of the chemical industry; although the concentration is relatively low, the low-concentration ammonia-containing wastewater is hard to treat and not easy to recycle. According to the characteristics, the invention provides a method for treating low-concentration ammonia-containing wastewater by use of a membrane separation technology, which specifically comprises the steps of neutralization with sulfuric acid, ultrafiltration separation, nanofiltration concentration and separation and reverse osmosis concentration and separation. The concentrated solution of nanofiltration can be recycled as a concentrated ammonium sulfate solution and is utilized in a production process; the yielding water of reverse osmosis can reach relatively high yielding water quality and can be discharged or recycled; the thick water of reverse osmosis flows back to the incoming water of nanofiltration so that the whole process basically realizes zero discharge and is environmentally friendly and energy-saving.
Description
Technical field
The present invention relates to a kind for the treatment of process of lower concentration ammonia-containing water, refer in particular to and take the technological method that membrane separation technique is core processing unit, belong to water-treatment technology field.
Background technology
Ammonia-containing water major part derives among the process procedure of large-size chemical production, and typical industry, for example, will produce a large amount of ammonia-containing waters among the production technique of persulphate.Persulphate, claims again peroxydisulfate, comprises the persulphates such as lithium, sodium, potassium, rubidium, caesium, ammonium, manganese, calcium, strontium, barium.Wherein, purposes is comparatively extensive, and what form commercial production scale is sodium, potassium, three kinds of persulphates of ammonium, is referred to as alkali metal persulphate.Persulphate is mainly used in the polymerization starter of synthetic resins, synthon, compound probability rubber, also for industrial sectors such as dyestuff, food preservation, burning surface treatment, bleaching, photograph, store battery, grease-decolor, sugarings.
The production method of persulphate is divided into electrolytic process and chemical method substantially, and order first two method all has use, and Process for Electrosynthesis of Ammonium Persulfate has obtained good effect, and the production of other persulphates both can have been used electrolytic process, can use chemical method again.Electrolytic process equipment is complicated, investment is large, power consumption is large, impurity is more in product, but cost is lower.And chemical process is simple, stable operation, less investment.
The general production technique of Process for Electrosynthesis of Ammonium Persulfate is: the cathode compartment that enters electrolyzer after industrial sulphuric acid dilute with water, the catholyte flowing out from anolyte compartment enters neutralizer, here sulfuric acid and ammonia neutralization form subalkaline ammoniumsulphate soln, and remove impurity wherein, this solution mixes the anolyte compartment that enters electrolyzer as anode feed liquid and carries out electrolysis with the recovery mother liquor flowing out from crystallizer, obtain the electrolytic solution that contains ammonium persulphate, through thickener, send in crystallizer, through centrifugation, solid is as finished product, and Recycling Mother Solution is used.Wherein negative electrode feed composition is sulfuric acid, and anode feed consists of ammonium persulphate, ammonium sulfate, sulfuric acid.
The general production technique that chemical method is produced persulphate is: with ammonium persulphate, produce with the replacement(metathesis)reaction of its corresponding oxyhydroxide.Primitive reaction principle is as follows:
Present method is thermopositive reaction, and generates ammonia, and the persulphate generating is because heat sensitivity is large, easily decomposes and the oxygen that loses activity, and for avoiding occurring this kind of situation, temperature need remain on 40～50 ℃.Technical process as shown in Figure 1.In technique, generally add water cooler as the element of cooling, in the use procedure of water cooler, in a large amount of water of condensation of generation, will contain certain density ammonia.
In addition, the smelting wastewater of smelting industry for example, some chemical industries of ammonia-containing water producing in Catalyst Production technique etc., all can produce a large amount of ammonia-containing waters.
The treatment process of general traditional ammonia-containing water has evaporation, stripping, biological treatment etc., but these techniques all have sizable limitation, as CN99116665.5 is used method of evaporation Ammonia-Containing Wastewater Treatment, under certain vacuum tightness, in evaporating kettle, ammonia-containing water is carried out to boiling, the ammonia that boiling is produced absorbs into ammoniacal liquor by water, present method is applicable to the ammonia-containing water of general complicated component, can play the object that reclaims ammonia, but its huge energy consumption is the greatest problem of the method, and and be not suitable for the condensation ammonia-containing water in persulphate production technique; Stripping process is to utilize air or steam that ammonia is taken out of and recycled with gas form, blow-off method Ammonia-Containing Wastewater Treatment technology is very ripe, as being used single tower stripping, ZL90107237.0 processes refinery ammonia-containing water, this technique means is to processing dense ammonia-containing water, particularly under the less condition of the water yield, comparatively suitable economically, and when the water yield is large and ammonia content is lower, this processing mode is by expending a large amount of energy, less economical, and is not suitable for application; Also can be by traditional bioremediation for the ammonia-containing water of lower concentration, but because the water quality after processing becomes complicated on the contrary, cannot realize the recycling of ammonia components, cause unnecessary waste.
In sum, all there is certain drawback in traditional technological method, or energy consumption is large or less economical, maybe cannot reach the object that resource reclaims, and therefore the present invention proposes a kind of membrane concentration recovery method of Ammonia-Containing Wastewater Treatment, to overcome the defect existing in prior art.
Membrane sepn is to occur in 20 beginnings of the century, a kind of new separation technology emerging rapidly after the sixties in 20th century.Because membrane separation technique is owing to having separation, concentrated, purifying and refining function concurrently, have again efficient, energy-saving and environmental protection, molecular level filters and filtration procedure is simple, be easy to the features such as control, food, medicine, biology, environmental protection, chemical industry, metallurgy, the energy, oil, water treatment, electronics, the field such as bionical have been widely used at present, produce huge economic benefit and social benefit, become one of most important means in current separation science.At present, conventional membrane separation technique mainly contains micro-filtration, ultrafiltration, nanofiltration, reverse osmosis and gas delivery etc.
Ultra-filtration membrane can be removed macrobead molecular substance, in water treatment, be often carried out application, for example very ripe MBR technology is exactly very typically to represent at present, ultra-filtration membrane is directly immersed in biochemistry pool, utilize the stalling characteristic of film directly to make biochemical water qualified discharge later, replace the second pond in traditional biological water treatment.
Nanofiltration membrane has distincter technical characterstic, for molecular weight, be greater than 300 daltonian organic substance and divalent salts, especially as vitriol, all there is higher rejection, with respect to reverse osmosis, there is again lower working pressure, it is widely used in water technology simultaneously.Reverse osmosis is applied in the middle of desalination process mostly, and the position in water technology is particularly important, and the technical characterstic of high desalination rate makes in the water technology of some high requirement, and the position of reverse osmosis is irreplaceable.Various membrane process have different separating mechanisms, applicable to different objects and requirement.Fully realizing it separately under the prerequisite of technical characterstic, organically in conjunction with various membrane process, have more technical advantage, original intention of the present invention is exactly the ammonia-containing water that the different membrane separation technique of comprehensive utilization is processed lower concentration, reach wastewater treatment, resource reclaims, the multiple advantage object of non-secondary pollution.
Summary of the invention
Feature for lower concentration ammonia-containing water, the many deficiencies that simultaneously exist for overcoming above-mentioned traditional method, the present invention proposes a kind of technological method that utilizes membrane concentration art breading this waste water of reuse, object is ammonia and pure water to be carried out separated as far as possible and recycles respectively, reach the object that approaches zero release, and keep whole waster water process economy, effectively and reasonably.
For realizing above-mentioned technical purpose, the technical scheme that the present invention proposes is:
Utilize membrane separation technique to process a method for lower concentration ammonia-containing water, it is characterized in that, comprise the following steps:
Step 1, neutralization stage;
In ammonia-containing water, add sulphuric acid soln, regulate after the pH value of ammonia-containing water, drain into liquid storage equalizing tank, enter next processing unit;
Step 2, ultra-filtration membrane pretreatment stage;
Utilize ultra-filtration membrane hold back in waste water as macromolecular particle things such as colloid, impurity, ultra-filtration membrane is separated into dense water and penetrating fluid by the waste water after neutralization, described concentrate recirculation is to described liquid storage equalizing tank, penetrating fluid enters next stage membrane element processing unit;
Step 3, nanofiltration membrane separation stage;
Utilize nanofiltration membrane further will intake separated, the concentrate recirculation of nanofiltration membrane one side is to the water-in of nanofiltration membrane treatment unit or put into production use, and the penetrating fluid that sees through nanofiltration membrane enters next stage membrane element processing unit;
Reach certain density dense water if reuse is to persulphate production process, can complete the recycling of effective constituent ammonia;
Step 4, reverse-osmosis treated stage;
Use anti-permeable membrane to produce water to nanofiltration membrane and carry out concentration, its concentrated solution is back to the water-in of nanofiltration membrane treatment unit, and its penetrating fluid produces water and directly discharges or reclaim use.
The N-process of step 1 ammonia-containing water and sulphuric acid soln should be chosen in the line mixer of sealing or closed reactor and carry out, and to prevent separating out of ammonia, causes the secondary pollution of air.Before ultrafiltration membrane treatment unit, be provided with cartridge filter, with the normal steady running of protective membrane and system.
In above-mentioned treatment process, the present invention for the ammonia quantity of ammonia-containing water be generally no more than 5000ppm, pH value, between 9～12, is adjusted to 6～7 in neutralization stage by the pH value of ammonia-containing water.
As preferably, described sulphuric acid soln is selected the dilute sulphuric acid that massfraction is 5%～10%.
As preferably, ultra-filtration membrane membrane element is chosen as a kind of in tubular membrane, hollow-fibre membrane, rolled film, flat sheet membrane, and particularly hollow fiber ultrafiltration membrane can be selected interior pressure or External Pressure Type.Ultra-filtration membrane molecular weight cut-off MWCO may be selected to be 100K～800K, and total principle is larger, the stable membrane element of choosing flux when guaranteeing effective filter effect.
As preferably, nanofiltration membrane membrane element is elected a kind of in hollow-fibre membrane, rolled film, flat sheet membrane as, and molecular weight cut-off MWCO is controlled at 200～500.The feature of nanofiltration membrane is that it has high rejection to divalent salts, can reach the concentrated object of expection, and compare with reverse osmosis membrane, the operating pressure of nanofiltration membrane is lower, water production rate is larger, under the condition that completes same concentration rate, energy consumption is also just lower, and divalent salts rejection is 90%～99%.
In above-mentioned technique, the object of sulfuric acid neutralization stage is to make the ammonia containing in ammonia condensing water to be converted into stable ammonium radical ion, and form stable ammoniumsulphate soln waste water, its necessity is two aspects, the first, by the adjusting to waste water pH value, can make ammonia-containing water be converted into stable ammonium salt, make it form stable solution system, make ammonia be difficult for separating out from waste water, can farthest retain ammonia composition; The second, follow-up technique is membrane separation technique, especially nanofiltration part, and requiring pending feed liquid is stable salts solution, and preferably divalent salts, the so higher rejection of guarantee.
The product water of nanofiltration membrane is generally the vitriol of lower concentration, use reverse osmosis process to carry out concentrating and separating processing to it, because water inlet saltiness is lower, therefore reverse osmosis membrane can be concentrated into finite concentration by feed concentration, concentrated solution is back to after water inlet place of nanofiltration and the water inlet of nanofiltration mix and by nanofiltration, is reclaimed, make like this effective constituent reclaim completely, reverse osmosis membrane is high to the rejection of salt, the product water of penetrating fluid generally can reach the standard of reuse, like this except the cleaning of general aspects and necessary blowdown, the high yield that can substantially realize zero release and active substance containing ammonia condensing method of wastewater treatment involved in the present invention.
Beneficial effect of the present invention:
1) in sulfuric acid and technique, in line mixer or airtight container, complete, make ammonia be converted into stable ammonium salt, can prevent from separating out and cause secondary pollution, and make waste water solute system meet the technical characterstic of membrane sepn;
2) use of ultra-filtration membrane can farthest prevent the interference that feed liquid forms, and guarantees the stable of subsequent technique, and guarantees the recovery quality of effective constituent ammonia;
3) compared with RO film (reverse osmosis membrane), the feature such as it is large that NF film (nanofiltration membrane) has flux, and operating pressure is low can obtain higher concentration rate under the prerequisite of equal energy output, namely obtains more valuable reuse standard;
4) use RO film as NF film, to produce the further advanced treatment technique of water, farthest guarantee the water quality of reuse pure water, and because the water inlet of RO film is that NF produces water, so the load of RO film is extremely low, therefore can extend the work-ing life of RO film;
5) concentrated solution of reverse osmosis membrane is back to water inlet place of nanofiltration, after mixing, is reclaimed by nanofiltration membrane with the water inlet of nanofiltration again, makes like this effective constituent reclaim completely;
6) except the cleaning of general aspects and necessary blowdown, the high yield that can substantially realize zero release and active substance containing ammonia condensing method of wastewater treatment involved in the present invention.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of existing persulphate chemical method production technique;
Fig. 2 is process flow diagram of the present invention.
Embodiment
In order to illustrate technical scheme of the present invention and technical purpose, below in conjunction with the drawings and the specific embodiments, the present invention is described further.
Embodiment 1:
In Sodium Persulfate production process, condenser is discharged containing ammonia condensing waste water, ammonia content is 1250ppm, in the dilute sulphuric acid that is 5% through mass concentration in airtight line mixer and after pH value be adjusted to 6.7, after reaction, the concentration of ammoniumsulphate soln is 4780ppm, enters in ammonium sulfate liquid storage tank pending.
It is that the hollow fiber ultrafiltration membrane system of 300K is carried out pre-treatment that ammonium sulfate waste water after neutralization reaction enters molecular weight cut-off by lift pump through cartridge filter, the concentrate recirculation of ultra-filtration membrane unit is to liquid storage equalizing tank, and it is 200 rolling nanofiltration membrane that penetrating fluid enters molecular weight cut-off.The concentration rate of nanofiltration membrane unit is 5, and the ammonium sulfate dope mass concentration of reuse is 2.39%, and producing water (being penetrating fluid), to enter desalination rate be 99.2% rolling reverse osmosis system.The concentration rate of reverse osmosis membrane system is 10 times, concentrate recirculation is recycled by nano-filtration unit after mixing with former nanofiltration water inlet to nanofiltration membrane unit water inlet place, reverse osmosis produced water saltiness is 32ppm, can be used as the water purification that meets processing requirement and carries out reuse or directly discharge.
Embodiment 2:
In Sodium Persulfate production process, condenser is discharged containing ammonia condensing waste water, and ammonia content is 1800ppm, in airtight line mixer, through in 7% dilute sulphuric acid and after pH value be 6.6, ammonium sulfate concentrations is 6900ppm, enters in liquid storage equalizing tank pending.
Ammonium sulfate waste water after neutralization reaction enters through cartridge filter the rolling ultrafiltration membrane processing unit that molecular weight cut-off is 100K by lift pump, the concentrate recirculation of ultra-filtration membrane unit is to liquid storage equalizing tank, it is 300 rolling nanofiltration membrane unit that its penetrating fluid enters molecular weight cut-off, the concentration rate of described rolling nanofiltration membrane is 4, its reuse ammonium sulfate mass concentration is 2.76%, it is 99.5% rolling reverse osmosis system that product water enters desalination rate, concentrated 8 times of described reverse osmosis system, concentrate recirculation is recycled by nanofiltration after mixing with former nanofiltration water inlet to nanofiltration water inlet place, reverse osmosis produced water saltiness is 20ppm, can be used as the water purification that meets processing requirement and carry out reuse or directly discharge.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (9)
1. utilize membrane separation technique to process a method for lower concentration ammonia-containing water, it is characterized in that, comprise the following steps:
Step 1, neutralization stage;
In ammonia-containing water, add sulphuric acid soln, regulate after the pH value of ammonia-containing water, drain into liquid storage equalizing tank, enter next processing unit;
Step 2, ultra-filtration membrane pretreatment stage;
Utilize ultra-filtration membrane to hold back the partial impurities particulate matter in waste water, ultra-filtration membrane is separated into dense water and penetrating fluid by the waste water after neutralization, and described concentrate recirculation is to described liquid storage equalizing tank, and penetrating fluid enters next stage membrane element processing unit;
Step 3, nanofiltration membrane separation stage;
Utilize the nanofiltration membrane filtering separation of further intaking, the concentrate recirculation of nanofiltration membrane one side is to the water-in of nanofiltration membrane treatment unit or put into production use, and the penetrating fluid that sees through nanofiltration membrane enters next stage membrane element processing unit;
Step 4, reverse-osmosis treated stage;
Use reverse osmosis membrane to produce water to nanofiltration membrane and carry out concentration, its concentrated solution is back to the water-in of nanofiltration membrane treatment unit, and its penetrating fluid produces water and directly discharges or reclaim use.
2. a kind of method of utilizing membrane separation technique to process lower concentration ammonia-containing water according to claim 1, is characterized in that, in above-mentioned steps one, the N-process of ammonia-containing water and sulphuric acid soln carries out in the line mixer sealing or closed reactor.
3. a kind of method of utilizing membrane separation technique to process lower concentration ammonia-containing water according to claim 1, is characterized in that, is provided with cartridge filter before ultrafiltration membrane treatment unit.
4. according to a kind of method of utilizing membrane separation technique to process lower concentration ammonia-containing water described in claim 1,2 or 3, it is characterized in that, the ammonia quantity of described ammonia-containing water is no more than 5000ppm, and pH value, between 9～12, is adjusted to 6～7 in neutralization stage by the pH value of ammonia-containing water.
5. a kind of method of utilizing membrane separation technique to process lower concentration ammonia-containing water according to claim 4, is characterized in that, described sulphuric acid soln is that mass concentration is 5%～10% dilute sulphuric acid.
6. a kind of method of utilizing membrane separation technique to process lower concentration ammonia-containing water according to claim 4, is characterized in that, the membrane element of described ultra-filtration membrane is a kind of in tubular membrane, hollow-fibre membrane, rolled film, flat sheet membrane.
7. a kind of method of utilizing membrane separation technique to process lower concentration ammonia-containing water according to claim 4, is characterized in that, described ultra-filtration membrane molecular weight cut-off is 100K～800K.
8. a kind of method of utilizing membrane separation technique to process lower concentration ammonia-containing water according to claim 4, is characterized in that, the membrane element of described nanofiltration membrane is a kind of in hollow-fibre membrane, rolled film, flat sheet membrane.
9. a kind of method of utilizing membrane separation technique to process lower concentration ammonia-containing water according to claim 4, is characterized in that, the molecular weight cut-off of described nanofiltration membrane is 200～500.
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| CN104045177A (en) * | 2014-07-02 | 2014-09-17 | 清华大学 | Membrane technology integrated processing method of high-concentration acrylonitrile wastewater |
| CN107890761A (en) * | 2017-11-14 | 2018-04-10 | 合肥创想能源环境科技有限公司 | A kind of method that the industrial waste gas containing ammonia is handled using membrane separation technique |
| CN111825238A (en) * | 2020-07-07 | 2020-10-27 | 山东绿知源环保工程有限公司 | Method and device for membrane method resource treatment of dilute sulfuric acid |
| CN114044599A (en) * | 2021-10-21 | 2022-02-15 | 安徽普朗膜技术有限公司 | Processing method and processing system of seafood cleaning water |
| CN115557574A (en) * | 2022-10-20 | 2023-01-03 | 徐州水处理研究所 | Process for recycling ammonium sulfate and ammonium chloride wastewater by full membrane method |
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| CN111825238B (en) * | 2020-07-07 | 2022-05-06 | 山东绿知源环保工程有限公司 | Method and device for membrane method resource treatment of dilute sulfuric acid |
| CN114044599A (en) * | 2021-10-21 | 2022-02-15 | 安徽普朗膜技术有限公司 | Processing method and processing system of seafood cleaning water |
| CN114044599B (en) * | 2021-10-21 | 2023-12-05 | 安徽普朗膜技术有限公司 | Treatment method and treatment system for seafood cleaning water |
| CN115557574A (en) * | 2022-10-20 | 2023-01-03 | 徐州水处理研究所 | Process for recycling ammonium sulfate and ammonium chloride wastewater by full membrane method |
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Application publication date: 20140326 |