CN114262104B - Method for removing trace pollutants in tap water by combining catalytic oxidation and membrane treatment technology - Google Patents
Method for removing trace pollutants in tap water by combining catalytic oxidation and membrane treatment technology Download PDFInfo
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Abstract
The invention discloses a method for removing trace pollutants in tap water by a catalytic oxidation combined membrane treatment technology, and belongs to the technical field of water treatment. The invention solves the problem of low removal rate of inorganic micromolecular pollutants by the existing catalytic oxidation technology. The invention adopts the catalytic oxidation combined membrane treatment process, and particularly adopts the catalytic ceramic membrane-nanofiltration-reverse osmosis combined membrane treatment system to enhance the treatment effect of catalytic oxidation on trace pollutants in tap water, thereby realizing the efficient removal of the trace pollutants in the tap water. The method provided by the invention has the advantages of high ozone generation rate, high ozone content in water and high removal rate of trace pollutants in tap water. The catalytic oxidation combined membrane treatment technology is used for treating tap water containing trace pollutants, and can also obtain good effects.
Description
Technical Field
The invention relates to a method for removing trace pollutants in tap water by combining catalytic oxidation and membrane treatment technologies, and belongs to the technical field of water treatment.
Background
The prior tap water plant adopts an ozone oxidation technology to treat source water so as to remove organic matter pollution in the water, but the ozone oxidation technology used in the prior water plant has low efficiency, low ozone concentration in the water, short residence time and low efficiency of removing trace organic matter pollution. Although increasing the amount of ozone added can increase the efficiency of removing trace organic matters, increasing the amount of ozone added can increase the generation of disinfection byproducts (such as bromates, brominated organic matters, iodinated organic matters, etc.). In addition, the existing water plants mostly adopt a single membrane to treat micromolecular pollutants in filtered water, the removal rate of micro-pollutants for ozone degradation is low, and the water quality of effluent of the water plants is seriously affected.
In order to overcome the defects of the traditional ozone oxidation technology treatment method, the catalytic oxidation technology is applied to remove trace organic matters in water. However, in practical applications, although catalytic oxidation can promote the removal of refractory organic matters in water by ozone, some disinfection byproducts are also produced, resulting in the production of small molecular organic pollutants (such as haloacetic acid and trihaloethane). And the removal rate of inorganic micromolecular pollutants by the traditional catalytic oxidation technology is still very low. Therefore, new catalytic oxidation techniques are needed in the prior art to improve the removal of trace organics from water.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method for removing trace pollutants in tap water by combining catalytic oxidation and membrane treatment technologies.
The technical scheme of the invention is as follows:
a method for removing trace pollutants in tap water by combining catalytic oxidation and membrane treatment technology comprises the following steps: tap water is filtered by sand filtration, activated carbon and PP cotton in sequence, then filtered by a catalytic ceramic membrane, enters a sealed water tank, is subjected to electrocatalytic combined ozone catalytic oxidation treatment, and effluent is filtered by a nanofiltration membrane and a reverse osmosis membrane respectively after being filtered by nano activated carbon, and is mixed with effluent of the nanofiltration membrane and effluent of the reverse osmosis membrane according to the proportion of 1 (2-4), and finally enters a water storage tank after being disinfected by ultraviolet light.
Further limited, the electrocatalytic combined ozone catalytic oxidation treatment process is to adopt a nano bubble generator to carry out ozone catalytic oxidation on tap water for 3-5 min.
Further limiting, the removal rate of the electrocatalytic combined ozone catalytic oxidation to the trace organic pollutants in the tap water is 99.90-99.98%.
Further limited, the removal rate of trace organic matters in tap water by electrocatalytic combined ozone catalytic oxidation is 99.90-99.99%.
The sealed water tank is characterized by further comprising at least one pair of electrodes, a direct current power supply and an ozone generator, wherein the direct current power supply is connected with the electrodes and supplies power to the electrodes.
Further defined, the electrode comprises an anode and a cathode, wherein the anode material is a multi-metal Ti composite oxide, and the cathode material is a Pt/Ti composite material.
Further defined, tap water includes surface water and groundwater.
Further defined, the metal in the multi-metal Ti composite oxide comprises one or more of aluminum, copper, tin, antimony, nickel, magnesium, titanium, iron, iridium, chromium, yttrium, platinum, gold and silver mixed in any proportion.
Further defined, the oxide in the multi-metal Ti composite oxide comprises one or more of titanium oxide, aluminum oxide, yttrium oxide, chromium oxide, iridium oxide, nickel oxide, selenium oxide, manganese oxide, antimony oxide, tin oxide and nickel oxide mixed in any proportion.
Further defined, the preparation method of the multi-metal Ti composite oxide comprises the following steps:
(1) Cutting and preprocessing the Ti plate;
(2) Adopting a surface etching technology to process the pretreated Ti plate;
(3) Under the vacuum condition, uniformly plating the mixture slurry of the metal and the metal oxide on the Ti plate in a thermal spraying mode, and spraying 4 layers each time;
(4) After finishing one-time spraying, performing thermal sintering;
(5) And (3) repeating the step (3) and the step (4) to obtain the multi-metal Ti composite oxide anode material.
Further defined, the surface etching technique in step (2) is acid etching.
Still further defined, the mixture slurry of metal and metal oxide is configured under vacuum conditions, and the mixture slurry of metal and metal oxide is composed of a multi-metal Ti composite oxide, a nano-conductive ceramic powder, and an organic additive.
Further limited, the sintering is a two-step sintering method, specifically, the sample is heated to 1530 ℃ for 15s, then cooled to 1425 ℃ rapidly, and the temperature is kept for 6min.
Further defined, the preparation method of the Pt/Ti composite material comprises the following steps:
(1) for Pt/Ti/SiO 2 Pretreating the Si negative film;
(2) mixing metal and metal oxide to prepare a metal/metal oxide metal target by adopting a melt casting method or a powder metallurgy method;
(3) pre-sputtering Ti under the vacuum condition and inert gas Ar atmosphere, wherein the current density is 10mA/cm 2 The pre-sputtering time is 5min;
(4) introducing oxygen, wherein the volume ratio of oxygen to argon is 5:30, spraying 2 layers by using a direct-current magnetron sputtering method and taking a high-purity Ti metal target as a sputtering source;
(5) under vacuum condition, using direct current magnetron sputtering to spray 2 layers by taking a metal/metal oxide metal target as a sputtering source;
(6) and (5) repeating the step (4) and the step (5) to obtain the Pt/Ti composite cathode material.
Further defined, the current density in step (4) and step (5) is 20mA/cm, respectively 2 And 35mA/cm 2 。。
The invention has the beneficial effects that:
(1) The invention adopts the catalytic oxidation combined membrane treatment process, and particularly adopts the catalytic ceramic membrane-nanofiltration-reverse osmosis combined membrane treatment system to enhance the treatment effect of catalytic oxidation on trace pollutants in tap water, thereby realizing the efficient removal of the trace pollutants in the tap water.
(2) The invention couples membrane filtration, electrochemical oxidation and ozone oxidation, thereby fundamentally solving the problems that the ozone oxidation effect is poor, most of nondegradable organic pollutants can not be degraded almost, and the reaction rate is low due to diffusion mass transfer limitation of ozone oxidation. The invention utilizes the diffusion mass transfer effect of electrons on the surface and inside of the electrode to improve the utilization rate and the reaction efficiency of electrons.
(3) The invention uses titanium as a base material and plates a layer of multi-metal and metal oxide on the surface as anode materials, and the multi-metal and metal oxide has good electrocatalytic activity and conductivity due to existence of the multi-metal and metal oxide, and the metal and metal oxide are plated on the surface of the base material in a slurry spraying mode, so that the formed multi-metal Ti composite oxide is of a uniform porous structure, the effective catalytic surface area is increased, and the addition of the metal and the metal oxide improves the catalytic activity of the coating and enhances the degradation capability on organic matters. In addition, the metal and the metal oxide can lead the coating to generate better binding force with the titanium, exert stronger electrocatalytic effect, and have long service life and good corrosion resistance.
(4) The invention adopts a direct current magnetron alternative sputtering method to prepare the Pt/Ti composite material as the cathode material, the surface of the electrode prepared by the method presents a uniform porous structure, the average residual stress is relatively less in change, and the surface is more uniform. The carried metal and metal oxide nano particles reduce agglomeration, not only improve specific surface area and surface activity, but also prevent bubbles from entering the inner surface of the electrode, avoid passivation of the titanium substrate, and ensure good stability and service life of the titanium substrate.
Drawings
FIG. 1 is a process flow diagram of the catalytic oxidation combined membrane treatment technique of the invention for removing trace contaminants in tap water;
fig. 2 is a graph showing the ozone concentration change curves of example 1 and comparative example 1.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials, reagents, methods and apparatus used, without any particular description, are those conventional in the art and are commercially available to those skilled in the art.
Example 1:
the preparation method of the multi-metal Ti composite oxide as the anode material comprises the following specific preparation processes:
(1) Firstly cutting a Ti plate into a required size, and then preprocessing the Ti plate, wherein the preprocessing is surface cleaning processing comprising metal layer surface oil removal and oxidation film removal.
(2) The pretreated Ti plate is treated by adopting a surface etching technology, specifically, a mixed solution of hydrofluoric acid and nitric acid with the volume ratio of 1:3 is used for 1min.
(3) The preparation process of the mixture slurry of the metal and the metal oxide comprises the following steps: using acetone as solvent, adding metal Ti, multi-metal composite oxide (0.05% Al, 0.05% Sn, 0.90% Sb, 0.5% Ni, 0.5% Fe, 0.3% Ir, 0.2% Y, 1.0% Pt, 2.0% Ti oxide, 1.0% Y oxide, 1.0% Cr oxide, 1.0% Ir oxide, 1.0% Ni oxide, 1.0% Sb oxide, 1.0% Sn oxide, 1.0% Ni oxide), ti 3 SiC 2 Mixing 85%, 12.5% and 2.5% of nano conductive ceramic powder according to mass fraction, and uniformly obtaining slurry in an organic solvent by ultrasonic; under vacuum condition, the mixture slurry of metal and metal oxide is uniformly plated on the Ti plate by a thermal spraying mode, 4 layers are sprayed each time, wherein the spraying pressure is 1.5Pa.
(4) After the primary spraying is finished, two-step sintering is carried out, and the specific operation process is as follows:
removing a small amount of gas in the sample by using 200A pulse current, controlling the heating rate to be 100 ℃/min, heating the sample to 1530 ℃ for 15 seconds, and then rapidly cooling to 1425 ℃ and preserving heat for 6min.
(5) And (3) repeating the step (3) and the step (4), and spraying 20 layers in total to obtain the multi-metal Ti composite oxide with the thickness of 15 mu m as the anode material.
Example 2:
the preparation method of the Pt/Ti composite material as the cathode material comprises the following specific preparation processes:
(1) For Pt/Ti/SiO 2 Pretreating the Si negative film, wherein the pretreatment is surface cleaning;
(2) The metal and the metal oxide are mixed by adopting a powder metallurgy method to prepare a metal/metal oxide metal target, wherein the metal/metal oxide metal target is composed of Pt, ti, a metal composite material (0.06% of titanium, 0.10% of chromium, 0.03% of yttrium, 1.2% of aluminum oxide, 1.50% of chromium oxide, 1.20% of platinum oxide, 0.5% of nickel oxide, 0.08% of zinc oxide, 0.5% of selenium oxide, 1.10% of titanium oxide, 1.10% of manganese oxide, 0.08% of antimony oxide, 0.5% of tin oxide, 0.02% of yttrium oxide and 0.03% of nickel oxide) according to the proportion of 12%, 80% and 8%;
(3) pre-sputtering Ti under the vacuum condition and inert gas Ar atmosphere, wherein the current density is 10mA/cm 2 The pre-sputtering time is 5min;
(4) introducing oxygen, wherein the volume ratio of oxygen to argon is 5:30, spraying 2 layers by using a direct-current magnetron sputtering method and taking a high-purity Ti metal target as a sputtering source; the specific technological parameters are as follows: the current density was 20mA/cm 2 The time is 1min, and the magnetic field intensity control parameter is 2000A/m;
(5) under vacuum condition, using direct current magnetron sputtering to spray 2 layers by taking a metal/metal oxide metal target as a sputtering source; the specific technological parameters are as follows: the current density was 35mA/cm 2 The time is 2min, and the magnetic field strength control parameter is 3500A/m;
(6) repeating the step (4) and the step (5) for 5 times to obtain the Pt/Ti thin film composite material with the thickness of 40 mu m as a cathode material.
Example 3:
the method for removing trace pollutants in tap water by adopting a catalytic oxidation combined membrane treatment technology comprises the following specific operation steps:
as shown in fig. 1, tap water is filtered by sand filtration, activated carbon and PP cotton in sequence, filtered by a catalytic ceramic membrane, enters a sealed water tank, is subjected to electrocatalytic combined ozone catalytic oxidation treatment for 4min, and effluent is filtered by a nanofiltration membrane and a reverse osmosis membrane respectively after being filtered by nano activated carbon, and is mixed with the effluent of the nanofiltration membrane and the effluent of the reverse osmosis membrane according to a ratio of 1:3, and finally enters a water tank after being disinfected by ultraviolet light.
The sealed water tank contains a pair of electrodes, the anode is the multi-metal Ti composite oxide prepared in the embodiment 1, the cathode is the Pt/Ti composite material prepared in the embodiment 2, the ozone gas flow is 35g/h, the concentration of the ozone gas in water is 0.7mg/L, and the output voltage of the direct current power supply is 220V.
Example 4:
this embodiment differs from embodiment 3 in that: tap water is not filtered by sand filtration, activated carbon and PP cotton, is not filtered by nano activated carbon, nanofiltration membrane and reverse osmosis filtration membrane, is only subjected to catalytic ceramic membrane and electrocatalytic combined ozone catalytic oxidation treatment, and the rest of operation processes and parameter settings are the same as those of example 3.
Example 5:
this embodiment differs from embodiment 3 in that: tap water was not filtered through sand, activated carbon and PP cotton, and the rest of the procedure and parameter settings were the same as in example 3.
Comparative example 1:
this comparative example differs from example 3 in that: the dc power was turned off and tap water was subjected to conventional ozone treatment, and the rest of the operation and parameter settings were the same as in example 3.
Effect example:
(1) The concentration of ozone in the sealed water tanks of example 3 and comparative example 1 was measured, and as shown in fig. 2, it can be seen from fig. 2 that the ozone catalytic oxidation technique provided in example 3 increased the concentration of ozone in water.
And according to the comparison of the water quality of the inlet water (tap water) and the outlet water (water storage tank), the removal rate of trace organic matters of the tap water treated in the mode of the embodiment 3 is 99.90-99.98%, and the removal rate of trace organic matters is 99.90-99.99%.
(2) The effluent of example 4 and comparative example 1 was tested for trace amounts of organic contaminants (including nitro compounds, alkanes, alkenes, organic acids, ketones, lipids, benzenes, halogenated hydrocarbons, amines, polycyclic aromatic hydrocarbons and heterocyclic compounds) and the results are shown in table 1 below:
| ketones (I) | Alkanes | Olefines | Organic acid | Nitro compounds | |
| Example 4 (mg/L) | 0.00001 | 0.00002 | 0.00001 | 0.00003 | 0.00004 |
| Comparative example 1 (mg/L) | 0.00006 | 0.00008 | 0.00007 | 0.00012 | 0.00012 |
| Lipid | Benzene compounds | Halogenated hydrocarbons | Amines | Polycyclic aromatic hydrocarbon and heterocyclic compound | |
| Example 4 (mg/L) | 0.00002 | 0.00002 | 0.00002 | 0.00002 | 0.00001 |
| Comparative example 1 (mg/L) | 0.00007 | 0.00008 | 0.00007 | 0.00005 | 0.00005 |
From the above table, the ozone catalytic oxidation technique provided in example 4 significantly reduced the concentration of trace organic contaminants in water.
(3) The effluent of example 5 and comparative example 1 was tested for trace organic contaminants (including carbonates, chlorides, sub-chlorides, bromates, nitrates, sulfides and fluorides) and the results are shown in table 2 below:
| nitro compounds | Alkanes | Olefines | Organic acid | Ketones (I) | |
| Example 5 (mg/L) | <0.00001 | <0.00001 | <0.00001 | <0.00001 | <0.00001 |
| Comparative example 1 (mg/L) | 0.00005 | 0.00002 | 0.00001 | 0.00004 | 0.00002 |
| Lipid | Benzene compounds | Halogenated hydrocarbons | Amines | Polycyclic aromatic hydrocarbon and heterocyclic compound | |
| Example 5 (mg/L) | <0.00001 | <0.00001 | <0.00001 | <0.00001 | <0.00001 |
| Comparative example 1 (mg/L) | 0.00003 | 0.00002 | 0.00002 | 0.00001 | 0.00001 |
From the above table, the ozone catalytic oxidation technique provided in example 5 significantly reduced the concentration of trace organic contaminants in water.
(4) The trace inorganic contaminants (carbonate, chloride, sub-chloride, bromate, nitrate, sulfide and fluoride) of the effluent of example 4 and comparative example 1 were detected and the results are shown in table 3 below:
| carbonate salt | Chlorides (CPS) | Sub-chlorides | Bromate salt | Nitrate salts | Sulfides | Fluoride compounds | |
| Example 4 (mg/L) | 0.00002 | 0.00004 | 0.00001 | 0.00006 | 0.00007 | 0.00005 | 0.00006 |
| Comparative example 1 (mg/L) | 0.00008 | 0.00008 | 0.00010 | 0.00011 | 0.00020 | 0.00009 | 0.00008 |
From the above table, the ozone catalytic oxidation technique provided in example 4 significantly reduced the concentration of trace inorganic contaminants in water.
(5) Trace inorganic contaminants (including calcium carbonate, magnesium carbonate, copper sulfate, chloride and nitrate) of the effluent of example 5 and comparative example 1 were detected, and the results are shown in table 4 below:
| carbonate salt | Chlorides (CPS) | Sub-chlorides | Bromate salt | Nitrate salts | Sulfides | Fluoride compounds | |
| Example 5 (mg/L) | <0.00001 | <0.00001 | <0.00001 | <0.00001 | 0.00002 | <0.00001 | <0.00001 |
| Comparative example 1 (mg/L) | 0.00002 | 0.00003 | 0.00005 | 0.00004 | 0.00010 | 0.00002 | 0.00002 |
From the above table, the ozone catalytic oxidation technique provided in example 5 significantly reduced the concentration of trace inorganic contaminants in water.
The above description is merely a preferred embodiment of the present invention, and since the person skilled in the art can make appropriate changes and modifications to the above-described embodiment, the present invention is not limited to the above-described embodiment, and some modifications and changes of the present invention should fall within the scope of the claims of the present invention.
Claims (5)
1. A method for removing trace pollutants in tap water by combining catalytic oxidation and membrane treatment technology is characterized by comprising the following steps: tap water is filtered by sand filtration, activated carbon and PP cotton in sequence, then filtered by a catalytic ceramic membrane, enters a sealed water tank after filtration, is subjected to electrocatalytic combined ozone catalytic oxidation treatment, and effluent is filtered by a nanofiltration membrane and a reverse osmosis membrane after being filtered by nano activated carbon, and is mixed with effluent of the nanofiltration membrane and effluent of the reverse osmosis membrane according to a proportion of 1 (2-4), and finally enters a water storage tank after being disinfected by ultraviolet light;
the sealed water tank at least comprises a pair of electrodes, a direct current power supply and an ozone generator, wherein the direct current power supply is connected with the electrodes to supply power for the electrodes;
the electrode comprises an anode and a cathode, wherein the anode material is a multi-metal Ti composite oxide, and the cathode material is a Pt/Ti composite material;
the preparation method of the multi-metal Ti composite oxide comprises the following steps:
(1) Cutting and preprocessing the Ti plate;
(2) Adopting a surface etching technology to process the pretreated Ti plate;
(3) Under the vacuum condition, uniformly plating the mixture slurry of the metal and the metal oxide on the Ti plate in a thermal spraying mode, and spraying 4 layers each time;
(4) After finishing one-time spraying, performing thermal sintering;
(5) Repeating the step (3) and the step (4) to obtain a multi-metal Ti composite oxide anode material;
the preparation method of the Pt/Ti composite material comprises the following steps:
(1) for Pt/Ti/SiO 2 Pretreating the Si negative film;
(2) mixing metal and metal oxide to prepare a metal/metal oxide metal target by adopting a melt casting method or a powder metallurgy method;
(3) pre-sputtering Ti under the vacuum condition and inert gas Ar atmosphere, wherein the current density is 10mA/cm 2 The pre-sputtering time is 5min;
(4) introducing oxygen, wherein the volume ratio of oxygen to argon is 5:30, spraying 2 layers by using a direct-current magnetron sputtering method and taking a high-purity Ti metal target as a sputtering source;
(5) under vacuum condition, using direct current magnetron sputtering to spray 2 layers by taking a metal/metal oxide metal target as a sputtering source;
(6) repeating the step (4) and the step (5) to obtain a Pt/Ti composite cathode material;
the metal in the multi-metal Ti composite oxide comprises one or more than two of aluminum, copper, tin, antimony, nickel, magnesium, titanium, iron, iridium, chromium, yttrium, platinum, gold and silver which are mixed according to any proportion, and the oxide in the multi-metal Ti composite oxide comprises one or more than two of titanium oxide, aluminum oxide, yttrium oxide, chromium oxide, iridium oxide, nickel oxide, selenium oxide, manganese oxide, antimony oxide, tin oxide and nickel oxide which are mixed according to any proportion.
2. The method for removing trace contaminants from tap water by combining catalytic oxidation and membrane treatment according to claim 1, wherein said surface etching technique in step (2) is acid etching.
3. The method for removing trace contaminants from tap water by combining catalytic oxidation with membrane treatment according to claim 1, wherein said metal and metal oxide mixture slurry is configured under vacuum conditions and consists of a multi-metal Ti composite oxide, a nano conductive ceramic powder and an organic additive.
4. The method for removing trace pollutants in tap water by combining catalytic oxidation and membrane treatment technology according to claim 1, wherein the thermal sintering is a two-step sintering method, specifically, the temperature is raised to 1530 ℃ for 15s, and then the temperature is lowered to 1425 ℃ for 6min.
5. A catalytic oxidation combined membrane treatment process according to claim 1The method for treating trace pollutants in the incoming water is characterized in that the current density in the step (4) and the step (5) is 20mA/cm respectively 2 And 35mA/cm 2 。
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