CN112264030A - Ozone catalytic treating agent for treating organic matters in wastewater and preparation method thereof - Google Patents
Ozone catalytic treating agent for treating organic matters in wastewater and preparation method thereof Download PDFInfo
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- CN112264030A CN112264030A CN202011315557.6A CN202011315557A CN112264030A CN 112264030 A CN112264030 A CN 112264030A CN 202011315557 A CN202011315557 A CN 202011315557A CN 112264030 A CN112264030 A CN 112264030A
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- diatomite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
Abstract
The invention belongs to the field of sewage treatment, and discloses an ozone catalytic treating agent for treating organic matters in wastewater, which is characterized in that: the ozone catalytic treatment agent comprises diatomite-based porous filler, and transition metal oxide and rare earth oxide loaded in the porous filler; the transition metal oxide is one of titanium oxide and nickel oxide; the rare earth oxide is lanthanum oxide or yttrium oxide. The ozone catalyst can improve the removal rate of COD in the water body, and simultaneously, also discloses a preparation method of the ozone catalytic treating agent.
Description
Technical Field
The invention belongs to the field of sewage treatment, and particularly relates to an ozone catalytic treating agent for treating organic matters in wastewater and a preparation method thereof.
Background
In various sewage treatment processes, ozone is adopted for removing organic matters in the prior art, and the ozone can generate active hydroxyl, so that the organic matters are decomposed, and the content of the organic matters in water is reduced.
CN201910280822.2 discloses a sewage treatment method by using an ozone-supported catalyst to carry out a synergistic reaction. The method comprises the following steps: (1) adding coagulant and coagulant aid into the sewage to be treated and stirring to form a water body containing micro floccules; (2) introducing high-density nano bubbles into the water body containing the micro floccules treated in the step (1), removing the micro floccules by using a mud scraper, and separating the micro floccules from the water body; (3) conveying the water body obtained by separation in the step (2) into a catalytic oxidation tower, mixing ozone and high-pressure return water of the catalytic oxidation tower by using an ejector, feeding the mixture into the catalytic oxidation tower, adding the ozone in a circulating manner, and carrying out catalytic oxidation reaction at normal temperature and normal pressure; the catalyst filled in the catalytic oxidation tower is a supported catalyst with the active component of transition metal oxide and the carrier of alumina and/or ceramsite.
But it has problems that: how to improve the removal rate of COD in the water body.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide an ozone catalytic treating agent for treating organic matters in wastewater and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
an ozone catalytic treatment agent for treating organic matters in wastewater, which comprises diatomite-based porous filler and transition metal oxide and rare earth oxide loaded in the porous filler;
the transition metal oxide is one of titanium oxide and nickel oxide;
the rare earth oxide is lanthanum oxide or yttrium oxide.
Furthermore, the diatomite-based porous filler contains 1-3 per mill of nano silver powder.
Meanwhile, the invention also provides a preparation method of the ozone catalytic treating agent, which comprises the following steps:
step 1: preparing the diatomite-based porous filler: mixing diatomite, carbon powder, adhesive and water, and performing ball milling and granulation;
step 2: the particles are sent into a high-temperature resistance furnace for calcination, and the calcination is divided into three stages: heating to 350 ℃ for 300-;
the weight proportions of the diatomite, the carbon powder and the adhesive are respectively as follows: 100: 3-5: 5-10;
and step 3: the filler particles are immersed in a solution containing transition metal salt and rare earth salt, taken out after being immersed for a period of time and sent into a high-temperature resistance furnace for secondary calcination, wherein the calcination temperature is 550-600 ℃.
Further, nano silver powder which is 1-3 per mill of the total weight of the diatomite and the adhesive is added in the step 1; the carbon powder in the step 1 is a carbon nano tube.
Further, the specific surface area of the carbon nanotube is 200-400m2/g。
Further, the diatomaceous earth is sieved to 10 μm or less and then mixed with other raw materials.
Further, the step 1 specifically comprises: mixing carbon powder and nano silver powder, then mixing the mixture with diatomite, finally adding an adhesive, adding water after all the powder is uniformly mixed, and uniformly stirring to form a paste.
Further, the method for mixing the carbon powder and the nano silver powder comprises the following steps: slowly adding the nano silver powder into the carbon powder, and stirring under the action of a magnetic stirrer.
The core of the invention is that:
(1) the transition metal oxide and the rare earth oxide are carried in the diatomite-based filler, and can activate ozone to form hydroxyl free radicals, thereby improving the decomposition efficiency of COD in wastewater.
(2) In the preparation process of the filler, the carbon powder is used as the pore-forming agent, the pore-forming rate is high, and particularly, the carbon nano-tube is used as the pore-forming agent, so that the silver nano-powder can be uniformly adsorbed around the carbon nano-tube, and after being mixed with the diatomite, the silver nano-powder can be uniformly distributed on the surface of a gap and can cooperate with the transition metal oxide and the rare earth oxide, and the decomposition efficiency of COD is further improved.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
A preparation method of an ozone catalytic treatment agent comprises the following steps:
step 1: preparing the diatomite-based porous filler: mixing diatomite, carbon powder, adhesive and water, and performing ball milling and granulation;
step 2: the particles are sent into a high-temperature resistance furnace for calcination, and the calcination is divided into three stages: heating to 350 ℃ for 2h, heating to 750 ℃ for 700 ℃ for 2h, and finally slowly cooling to normal temperature to obtain filler particles;
the weight proportions of the diatomite, the carbon powder and the adhesive are respectively as follows: 100: 4: 10; the particle size of the carbon powder can be 180 meshes.
And step 3: the filler particles are immersed in a solution containing transition metal salt and rare earth salt, are taken out after being immersed for a period of time, are dried and are sent into a high-temperature resistance furnace for secondary calcination, the calcination temperature is 550-.
In the solution in the step 3, the transition metal salt and the rare earth salt are respectively nickel nitrate and lanthanum nitrate, and the concentration is 1M.
Example 2
A preparation method of an ozone catalytic treatment agent comprises the following steps:
step 1: preparing the diatomite-based porous filler: mixing diatomite, carbon nano tubes, nano silver powder, an adhesive and water, and then carrying out ball milling and granulation;
the more specific preparation process comprises the following steps: slowly scattering nano silver powder into the carbon nano tube for mixing, stirring and dispersing by adopting a magnetic stirrer, then slowly adding the mixture into diatomite for stirring and dispersing, finally adding an adhesive, adding a proper amount of water after all solid powder is uniformly dispersed, forming the mixture into a mud shape, and feeding the mud into a ball mill for granulating.
Step 2: the particles are sent into a high-temperature resistance furnace for calcination, and the calcination is divided into three stages: heating to 350 ℃ for 2h, heating to 750 ℃ for 700 ℃ for 2h, and finally slowly cooling to normal temperature to obtain filler particles;
the weight proportions of the diatomite, the carbon nano tube and the adhesive are respectively as follows: 100: 3: 10; the weight of the nano silver powder is 2 per mill of the weight of the diatomite and the adhesive. The binder is selected to be cement.
And step 3: and (2) soaking the filler particles in a solution containing transition metal salt and rare earth salt for 12 hours, taking out, drying and sending into a high-temperature resistance furnace for secondary calcination at the calcination temperature of 550-600 ℃ for half an hour.
In the solution in the step 3, the transition metal salt and the rare earth salt are respectively nickel nitrate and lanthanum nitrate, and the concentration is 1M.
Example 3
A preparation method of an ozone catalytic treatment agent comprises the following steps:
step 1: preparing the diatomite-based porous filler: mixing diatomite, carbon nano tubes, nano silver powder, an adhesive and water, and then carrying out ball milling and granulation;
the more specific preparation process comprises the following steps: slowly scattering nano silver powder into the carbon nano tube for mixing, stirring and dispersing by adopting a magnetic stirrer, then slowly adding the mixture into diatomite for stirring and dispersing, finally adding an adhesive, adding a proper amount of water after all solid powder is uniformly dispersed, forming the mixture into a mud shape, and feeding the mud into a ball mill for granulating.
Step 2: the particles are sent into a high-temperature resistance furnace for calcination, and the calcination is divided into three stages: heating to 350 ℃ for 2h, heating to 750 ℃ for 700 ℃ for 2h, and finally slowly cooling to normal temperature to obtain filler particles;
the weight proportions of the diatomite, the carbon nano tube and the adhesive are respectively as follows: 100: 5: 5; the weight of the nano silver powder is 3 per mill of the weight of the diatomite and the adhesive. The binder is selected to be cement.
And step 3: and (2) soaking the filler particles in a solution containing transition metal salt and rare earth salt for 12 hours, taking out, drying and sending into a high-temperature resistance furnace for secondary calcination at the calcination temperature of 550-600 ℃ for half an hour.
In the solution in the step 3, the transition metal salt and the rare earth salt are respectively nickel nitrate and lanthanum nitrate, and the concentration is 1M.
Example 4
A preparation method of an ozone catalytic treatment agent comprises the following steps:
step 1: preparing the diatomite-based porous filler: mixing diatomite, carbon nano tubes, nano silver powder, an adhesive and water, and then carrying out ball milling and granulation;
the more specific preparation process comprises the following steps: slowly scattering nano silver powder into the carbon nano tube for mixing, stirring and dispersing by adopting a magnetic stirrer, then slowly adding the mixture into diatomite for stirring and dispersing, finally adding an adhesive, adding a proper amount of water after all solid powder is uniformly dispersed, forming the mixture into a mud shape, and feeding the mud into a ball mill for granulating.
Step 2: the particles are sent into a high-temperature resistance furnace for calcination, and the calcination is divided into three stages: heating to 350 ℃ for 1h, heating to 750 ℃ for 700 ℃ for 1h, and finally slowly cooling to normal temperature to obtain filler particles;
the weight proportions of the diatomite, the carbon nano tube and the adhesive are respectively as follows: 100: 4: 8; the weight of the nano silver powder is 1 per mill of the weight of the diatomite and the adhesive. The binder is selected to be cement.
And step 3: and (2) soaking the filler particles in a solution containing transition metal salt and rare earth salt for 12 hours, taking out, drying and sending into a high-temperature resistance furnace for secondary calcination at the calcination temperature of 550-600 ℃ for half an hour.
In the solution in the step 3, the transition metal salt and the rare earth salt are respectively nickel nitrate and lanthanum nitrate, and the concentration of the transition metal salt and the rare earth salt is 1.5M.
Comparative example 1
The same as example 2, except that: step 3 does not contain nickel nitrate.
Comparative example 2
The same as example 2, except that: step 3 does not contain lanthanum nitrate.
Comparative example 3
The carbon nanotube is replaced by micron-sized carbon powder, and all the powder (containing nano silver powder) is simultaneously mixed.
Test method
Preparing a glass tank with the diameter of 20cm, introducing wastewater into the bottom of the glass tank, and discharging the treated water from the top of the glass tank; filling a filler layer in the middle of the glass tank, wherein the filler is selected from the fillers of examples 1 and 2 and comparative examples 1 and 2; the ozone generator is arranged at the bottom of the glass tank, and the height of the filler is 30 cm; the grain diameter of the filler is 1-1.5 cm; the ozone generator generates micron bubbles with the flow rate of 50g/m3. The top of the glass tank is periodically deslagged, and the wastewater treatment speed is 3m3/h。
The COD content of the wastewater is 500-550 mg/L.
The test results are as follows:
| example 1 | Example 2 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| COD value in treated water | 107 | 36 | 270 | 165 | 85 |
The following conclusions can be drawn from the above tests:
1. the diatomite-based filler is adopted to load transition metal and rare earth metal, so that the oxidation activity of ozone can be improved;
2. the carbon nano tube is used as a pore forming agent, and can distribute the nano silver powder on the surface of pores, so that the treatment efficiency of the wastewater is improved.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. An ozone catalytic treatment agent for treating organic matters in wastewater, which is characterized in that: the ozone catalytic treatment agent comprises diatomite-based porous filler, and transition metal oxide and rare earth oxide loaded in the porous filler;
the transition metal oxide is one of titanium oxide and nickel oxide;
the rare earth oxide is lanthanum oxide or yttrium oxide.
2. The catalytic ozone treatment agent for organic matter treatment in wastewater according to claim 1, characterized in that: the diatomite-based porous filler contains 1-3 per mill of nano silver powder.
3. A method for producing the ozone catalytic treatment agent according to claim 1 or 2, characterized in that: the method comprises the following steps:
step 1: preparing the diatomite-based porous filler: mixing diatomite, carbon powder, adhesive and water, and performing ball milling and granulation;
step 2: the particles are sent into a high-temperature resistance furnace for calcination, and the calcination is divided into three stages: heating to 350 ℃ for 300-;
the weight proportions of the diatomite, the carbon powder and the adhesive are respectively as follows: 100: 3-5: 5-10;
and step 3: the filler particles are immersed in a solution containing transition metal salt and rare earth salt, taken out after being immersed for a period of time and sent into a high-temperature resistance furnace for secondary calcination, wherein the calcination temperature is 550-600 ℃.
4. The method of claim 3, wherein the ozone-catalyzing treatment agent is prepared by: nano silver powder which is 1-3 per mill of the total weight of the diatomite and the adhesive is also added in the step 1; the carbon powder in the step 1 is a carbon nano tube.
5. The method for producing an ozone catalytic treatment agent according to claim 4, characterized in that: the specific surface area of the carbon nano tube is 200-400m2/g。
6. The method of claim 3, wherein the ozone-catalyzing treatment agent is prepared by: the diatomite is sieved to be below 10 mu m and then is mixed with other raw materials.
7. The method for producing an ozone catalytic treatment agent according to claim 4, characterized in that: the step 1 specifically comprises the following steps: mixing carbon powder and nano silver powder, then mixing the mixture with diatomite, finally adding an adhesive, adding water after all the powder is uniformly mixed, and uniformly stirring to form a paste.
8. The method for producing an ozone catalytic treatment agent according to claim 7, characterized in that: the method for mixing the carbon powder and the nano silver powder comprises the following steps: slowly adding the nano silver powder into the carbon powder, and stirring under the action of a magnetic stirrer.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113171783A (en) * | 2021-04-21 | 2021-07-27 | 中化环境科技工程有限公司 | Microporous honeycomb ozone catalyst and preparation method and application thereof |
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| CN113171783A (en) * | 2021-04-21 | 2021-07-27 | 中化环境科技工程有限公司 | Microporous honeycomb ozone catalyst and preparation method and application thereof |
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