CN112076751A - Preparation method of diatomite-based supporter for high-efficiency oxidation high-density catalytic oxidation tower - Google Patents
Preparation method of diatomite-based supporter for high-efficiency oxidation high-density catalytic oxidation tower Download PDFInfo
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Abstract
The invention relates to the field of environmental protection, and in particular relates to a preparation method of a diatomite-based support for a high-density catalytic oxidation tower, which comprises the support and a fluidized bed reaction tank, wherein the support is an alkalization modified diatomite-based support. The preparation method of the modified diatomite comprises the following steps: adding 150 parts of the obtained carrier material 100-one into a high-speed mixer, vacuumizing, controlling the vacuum degree to be 0.085-0.098MPa, adding 1500 parts of hydrochloric acid with the mass percentage concentration of 10% -15%, controlling the temperature to be 60-80 ℃, treating for 30-60min, adding 20-28 parts of phytic acid and 3-8 parts of titanium dioxide, controlling the temperature to be 60-80 ℃, stirring and reacting for 2-5h, filtering and drying to obtain the titanium dioxide loaded modified diatomite with the phytate group.
Description
Technical Field
The invention relates to the field of environmental protection, in particular to a preparation method of a diatomite-based supporter for a high-density catalytic oxidation tower with efficient oxidation.
Background
Diatomaceous earth type carrier: is prepared by calcining natural diatomite, is pink due to containing a small amount of ferric oxide, and is called a red supporter, such as 201 type, 6201 type, C22 insulating brick, Chromsorb P and the like; if a small amount of sodium carbonate is added as a cosolvent before calcination and iron oxide forms colorless sodium ferrosilicate after calcination, the carrier is called a white support, such as type 101, type 102, Celite 545, chromosorb (AGW), Gas Chrom (APQSZ), etc.
The most remarkable characteristic of efficient oxidation is that hydroxyl radical (HO) intermediate is generated in an oxidation system in a certain mode, and takes (HO) as a main oxidant to react with organic matters, and organic radicals can be generated or organic peroxide radicals can be generated in the reaction to continue the reaction, so that the purpose of completely or partially decomposing the organic matters is achieved. CN200510026670.1 relates to a method and a system for treating high-concentration wastewater by catalytic oxidation, wherein the method comprises the following steps: the pretreated high-concentration wastewater enters a wastewater storage tank and enters a mixer through a fine filter; the stock solutions of the acid storage tank and the storage tank are respectively input into a chlorine dioxide generator to react to generate chlorine dioxide and then are prepared into chlorine dioxide aqueous solution, the chlorine dioxide aqueous solution is conveyed to a flow mixer to be mixed with high-concentration wastewater and then flows into a catalytic oxidation tower with a composite catalyst for treating wastewater by three-phase catalytic oxidation at the bottom to carry out catalytic oxidation reaction with air in the tower, the treated wastewater from the catalytic oxidation tower flows into a flow stabilizer, then enters a tubular neutralizer to neutralize the wastewater to pH7-8 and then flows into subsequent treatment equipment. The invention has the advantages of effective treatment of industrial wastewater which has high stability of organic compounds, high chroma, high salt content and difficult biodegradation, simple and convenient operation, no secondary pollution and no dregs generation.
CN200910081627.3 discloses an acrylic fiber sewage treatment process, which comprises the following steps: (1) adjusting the pH value of the acrylic fiber sewage subjected to biochemical treatment to 6.5-7.5, and filtering; (2) the filtered acrylic fiber sewage enters a circulating absorption tank and is fully mixed with the supplied chlorine dioxide; (3) the acrylic fiber sewage mixed with the chlorine dioxide enters a catalytic oxidation tower, a high-efficiency catalyst is filled in the catalytic oxidation tower, compressed air is introduced into the catalytic oxidation tower, and the acrylic fiber sewage entering the catalytic oxidation tower is subjected to oxidation reaction with the chlorine dioxide and oxygen in the compressed air under the action of the high-efficiency catalyst. Under the action of the high-efficiency catalyst, oxygen in the air is used as an oxidant to react with chlorine dioxide, so that the consumption of a liquid-phase oxidant of chlorine dioxide is reduced, the treatment cost is reduced, the treatment efficiency is improved, the reaction speed is greatly accelerated, and the retention time of sewage in the three-phase catalytic oxidation tower is shortened. The treatment process has the obvious advantages of economy and high efficiency. CN201110151561.8 discloses an organic wastewater advanced treatment system in the biopharmaceutical industry, which comprises a regulating tank, a sedimentation tank, an electric flotation device, an advanced catalytic oxidation tower, an anaerobic membrane bed-aeration biological filter and a discharge pipe which are connected in sequence; the adjusting tank comprises a submersible mixer, and the electric flotation equipment comprises an electrode group, wherein the electrode group is arranged at the bottom of the inner cavity of the tank body and comprises a base, a cathode plate and an anode plate, and a connecting screw rod, wherein the cathode plate and the anode plate are insoluble polar plates, such as titanium-coated iridium anode plates and titanium-coated ruthenium anode plates; the advanced catalytic oxidation tower is internally provided with an ozone generator and is irradiated by ultraviolet rays; the anaerobic membrane bed-biological aerated filter is provided with an anaerobic tank, an aerobic tank and an aeration system. The organic wastewater advanced treatment system integrates electrochemical treatment, filtration and biodegradation, can effectively remove organic matters and ammonia nitrogen in wastewater, has high cost performance, simple operation and no toxic effect on subsequent treatment, and can effectively avoid secondary pollution.
At present, the Fenton oxidation technology is mainly used, but the traditional Fenton method has some defects, the dosage of the ferrous salt catalyst is large, the operation cost is high, and the sludge production amount is small.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a diatomite-based support for a high-density catalytic oxidation tower, which is used for efficient oxidation.
The preparation process of diatomite-base carrier for efficient oxidation in high density catalytic oxidation tower includes one carrier and one fluidized bed reaction tank, and features the carrier being one kind of alkalization modified diatomite-base carrier.
The specific preparation scheme of the alkalization modified diatomite-based carrier is as follows:
the method comprises the following steps: putting 180 parts of modified diatomite 100-28 parts, aluminum oxide 10-28 parts, sodium silicate 12-18 parts, ammonium oxalate 0.3-0.6 part and calcium carbonate 2-6 parts into a mixing kettle, mixing and stirring for 20-30min, then adding silica sol 40-60 parts by mass of 20-30% into the mixing kettle, uniformly stirring and mixing, forming, drying at 80-120 ℃ for 1-4h to obtain a carrier embryo, putting the carrier embryo into a muffle furnace after completion, controlling the temperature to be 600-800 ℃, calcining for 60-120min, cooling to room temperature after completion, taking out and crushing into particles;
step two: adding the obtained support material into a high-speed mixer, controlling the temperature to 200-300 ℃, then vacuumizing, controlling the vacuum degree to 0.085-0.098MPa, adding 28-46 parts of sodium hydroxide solid and 2-5 parts of seleno-diacetic acid, and continuously stirring for dehydration reaction for 60-180min to obtain the alkalinized modified diatomite-based support.
The preparation method of the modified diatomite comprises the following steps:
adding 150 parts of the obtained carrier material 100-one into a high-speed mixer, vacuumizing, controlling the vacuum degree to be 0.085-0.098MPa, adding 1500 parts of hydrochloric acid with the mass percentage concentration of 10% -15%, controlling the temperature to be 60-80 ℃, treating for 30-60min, adding 20-28 parts of phytic acid and 3-8 parts of titanium dioxide, controlling the temperature to be 60-80 ℃, stirring and reacting for 2-5h, filtering and drying to obtain the modified diatomite loaded with titanium dioxide and provided with phytate groups;
the surface of the alkalinized modified diatomite-based support can form a FeOOH/titanium hydroxide layer-shaped double hydroxide composite crystal which can catalyze hydrogen peroxide catalytic oxidation.
Compared with a Fenton oxidation tower, the high-density catalytic oxidation tower with high-efficiency oxidation can reduce the addition of ferrous salt.
And part of the treated wastewater at the upper part of the oxidation tower returns to the bottom of the tower for further oxidation treatment.
The preparation method of the diatomite-based support for the high-density catalytic oxidation tower with high-efficiency oxidation, disclosed by the invention, combines the advantages of the traditional Fenton method and the fluidized bed, improves the defect of too high sludge yield of the traditional Fenton method, improves the treatment effect and reduces the chemical sludge yield by utilizing the electric field and the crystallization technology, and greatly increases the application range. Ferric iron generated by Fenton oxidation method is used for generating Fe/titanium layered double hydroxide composite crystals on the surface of an alkalization modified diatomite-based carrier in a fluidized bed reaction tank to show strong synergistic catalytic effect; the catalyst can be used as a catalyst of hydrogen peroxide to continuously catalyze the oxidation reaction of pollutants, and the FeOOH exists, so that the dosage of the ferrous salt catalyst can be greatly reduced, and the operation cost and the sludge production are further reduced.
Organic matters are chemically adsorbed on the surface of the catalyst to form surface chelates with certain nucleophilicity, then ozone or hydroxyl radicals are subjected to oxidation reaction with the surface chelates, and formed intermediate products can be further oxidized on the surface and can also be desorbed into a solution to be further oxidized.
(2) The catalyst can not only adsorb organic matters, but also directly generate oxidation-reduction reaction with ozone, and the generated oxidation state metal and hydroxyl free radicals can directly oxidize the organic matters.
(3) The catalyst catalyzes the ozone decomposition to generate an oxidant with higher activity, so that the oxidant reacts with organic molecules which are not chemically adsorbed, and the blank contrast improvement rate exceeds 20%.
Drawings
FIG. 1 is a Fourier infrared spectrum of the modified diatomaceous earth prepared in example 2:
at 464cm-1An absorption peak of silica at 1094/787cm is present in the vicinity-1An absorption peak of silica exists nearby, which indicates that the iron-containing diatomite participates in the reaction; at 1166cm-1An absorption peak of phosphorus-oxygen double bonds exists nearby, which indicates that phytic acid participates in the reaction; the absorption peak of the titanium dioxide is merged into 464cm-1The absorption peak of silica.
Detailed Description
The invention is further illustrated by the following specific examples:
a high-density catalytic oxidation tower for investigating high-efficiency oxidation aims at simulating dye wastewater (methyl orange), investigates the degradation performance of organic matters, carries out an inner-circulation high-density catalytic oxidation experiment, analyzes the content of iron element contained in a prepared support material before and after use by XRF, and determines the removal rate of the dye wastewater (methyl orange).
Example 1
The preparation process of diatomite-base carrier for efficient oxidation in high density catalytic oxidation tower includes one carrier and one fluidized bed reaction tank, and features the carrier being one kind of alkalization modified diatomite-base carrier.
The specific preparation scheme of the alkalization modified diatomite-based carrier is as follows:
the method comprises the following steps: putting 100kg of modified diatomite, 10kg of alumina, 12kg of sodium silicate, 0.3kg of ammonium oxalate and 2kg of calcium carbonate into a mixing kettle, mixing and stirring for 20min, then adding 40kg of silica sol with the mass kg of 20% into the mixing kettle, stirring and mixing uniformly, forming, then drying for 1h at 80 ℃ to obtain a carrier embryo body, putting the carrier embryo body into a muffle furnace after completion, controlling the temperature to 600 ℃, calcining for 60min, cooling to room temperature after completion, taking out and crushing into granules;
step two: and adding the obtained support material into a high-speed mixer, controlling the temperature to 200 ℃, then vacuumizing, controlling the vacuum degree to be 0.085MPa, adding 28kg of sodium hydroxide solid and 2kg of seleno-diacetic acid, and continuously stirring for dehydration reaction for 60min to obtain the alkalinized modified diatomite-based support.
The preparation method of the modified diatomite comprises the following steps:
adding 100kg of the obtained support material into a high-speed mixer, vacuumizing, controlling the vacuum degree to be 0.085MPa, adding 1000kg of hydrochloric acid with the mass percentage concentration of 10%, controlling the temperature to be 60 ℃, treating for 30min, adding 20kg of phytic acid and 3kg of titanium dioxide, controlling the temperature to be 60 ℃, stirring and reacting for 2h, filtering, and drying to obtain the titanium dioxide-loaded modified diatomite with the phytate groups;
the surface of the alkalinized modified diatomite-based support can form a Fe/titanium layered double hydroxide crystal for catalyzing hydrogen peroxide catalytic oxidation.
Compared with a Fenton oxidation tower, the high-density catalytic oxidation tower with high-efficiency oxidation can reduce the addition of ferrous salt.
The hydrogen peroxide inlet pipe and the ferrite inlet pipe are provided with flow control valves.
And part of the treated wastewater at the upper part of the oxidation tower returns to the bottom of the tower for further oxidation treatment.
In the experiment, before the experiment of the internal circulation Fenton fluidized bed, the iron content of the supporter is 8.2%, the iron content of the supporter after the experiment is 18.7%, and the decolorization rate of methyl orange is 95.8%.
Example 2
The preparation process of diatomite-base carrier for efficient oxidation in high density catalytic oxidation tower includes one carrier and one fluidized bed reaction tank, and features the carrier being one kind of alkalization modified diatomite-base carrier.
The specific preparation scheme of the alkalization modified diatomite-based carrier is as follows:
the method comprises the following steps: putting 150kg of modified diatomite, 22kg of alumina, 15kg of sodium silicate, 0.4kg of ammonium oxalate and 3kg of calcium carbonate into a mixing kettle, mixing and stirring for 25min, then adding 48kg of silica sol with the mass kg of 25% into the mixing kettle, stirring and mixing uniformly, forming, then drying for 3h at 100 ℃ to obtain a carrier embryo body, putting the carrier embryo body into a muffle furnace after the completion, controlling the temperature to 700 ℃, calcining for 90min, cooling to room temperature after the completion, taking out and crushing into granules;
step two: and adding the obtained support material into a high-speed mixer, controlling the temperature to 260 ℃, then vacuumizing, controlling the vacuum degree to be 0.09MPa, adding 41kg of sodium hydroxide solid and 3kg of seleno-diacetic acid, and continuously stirring for dehydration reaction for 150min to obtain the alkalinized modified diatomite-based support.
The preparation method of the modified diatomite comprises the following steps:
adding 140kg of the obtained support material into a high-speed mixer, vacuumizing, controlling the vacuum degree to be 0.09MPa, adding 1300kg of hydrochloric acid with the mass percentage concentration of 12%, controlling the temperature to be 66 ℃, treating for 50min, adding 23kg of phytic acid and 5kg of titanium dioxide, controlling the temperature to be 70 ℃, stirring and reacting for 3h, filtering, and drying to obtain the titanium dioxide-loaded modified diatomite with the phytate groups;
the surface of the alkalinized modified diatomite-based support can form a Fe/titanium layered double hydroxide crystal for catalyzing hydrogen peroxide catalytic oxidation.
Compared with a Fenton oxidation tower, the high-density catalytic oxidation tower with high-efficiency oxidation can reduce the addition of ferrous salt.
The hydrogen peroxide inlet pipe and the ferrite inlet pipe are provided with flow control valves.
And part of the treated wastewater at the upper part of the oxidation tower returns to the bottom of the tower for further oxidation treatment.
In the experiment, before the experiment of the internal circulation Fenton fluidized bed, the iron content of the supporter is 9.4%, the iron content of the supporter after the experiment is 20.4%, and the decolorization rate of methyl orange is 97.4%.
Example 3
The preparation process of diatomite-base carrier for efficient oxidation in high density catalytic oxidation tower includes one carrier and one fluidized bed reaction tank, and features the carrier being one kind of alkalization modified diatomite-base carrier.
The specific preparation scheme of the alkalization modified diatomite-based carrier is as follows:
the method comprises the following steps: putting 180kg of modified diatomite, 28kg of alumina, 18kg of sodium silicate, 0.6kg of ammonium oxalate and 6kg of calcium carbonate into a mixing kettle, mixing and stirring for 30min, then adding 60kg of silica sol with the mass kg of 30% into the mixing kettle, stirring and mixing uniformly, forming, then drying for 4h at 120 ℃ to obtain a carrier embryo body, putting the carrier embryo body into a muffle furnace after the completion, controlling the temperature to 800 ℃, calcining for 120min, cooling to room temperature after the completion, taking out and crushing into granules;
step two: adding the obtained support material into a high-speed mixer, controlling the temperature to 300 ℃, then vacuumizing, controlling the vacuum degree to be 0.098MPa, adding 46kg of sodium hydroxide solid and 5kg of seleno-diacetic acid, and continuously stirring for dehydration reaction for 60-180min to obtain the alkalinized modified diatomite-based support.
The preparation method of the modified diatomite comprises the following steps:
adding 150kg of the obtained support material into a high-speed mixer, vacuumizing, controlling the vacuum degree to be 0.098MPa, adding 1500kg of hydrochloric acid with the mass percentage concentration of 15%, controlling the temperature to be 80 ℃, treating for 60min, adding 28kg of phytic acid and 8kg of titanium dioxide, controlling the temperature to be 80 ℃, stirring and reacting for 5h, filtering, and drying to obtain the titanium dioxide-loaded modified diatomite with the phytate groups;
the surface of the alkalinized modified diatomite-based support can form a Fe/titanium layered double hydroxide crystal for catalyzing hydrogen peroxide catalytic oxidation.
Compared with a Fenton oxidation tower, the high-density catalytic oxidation tower with high-efficiency oxidation can reduce the addition of ferrous salt.
The hydrogen peroxide inlet pipe and the ferrite inlet pipe are provided with flow control valves.
And part of the treated wastewater at the upper part of the oxidation tower returns to the bottom of the tower for further oxidation treatment.
In the experiment, before the experiment of the internal circulation Fenton fluidized bed, the iron content of the supporter is 9.7%, the iron content of the supporter after the experiment is 21.5%, and the decolorization rate of methyl orange is 98.7%.
Comparative example 1
The specific preparation scheme of the alkalization modified diatomite-based carrier is as follows:
the method comprises the following steps: putting 100kg of diatomite, 10kg of alumina, 12kg of sodium silicate, 0.3kg of ammonium oxalate and 2kg of calcium carbonate into a mixing kettle, mixing and stirring for 20min, then adding 40kg of silica sol with the mass kg of 20% into the mixing kettle, stirring and mixing uniformly, forming, then drying for 1h at 80 ℃ to obtain a carrier embryo body, putting the carrier embryo body into a muffle furnace after completion, controlling the temperature to 600 ℃, calcining for 60min, cooling to room temperature after completion, taking out and crushing into granules;
step two: and adding the obtained support material into a high-speed mixer, controlling the temperature to 200 ℃, then vacuumizing, controlling the vacuum degree to be 0.085MPa, adding 28kg of sodium hydroxide solid and 2kg of seleno-diacetic acid, and continuously stirring for dehydration reaction for 60min to obtain the alkalinized modified diatomite-based support.
Other reaction conditions were the same as in example 1.
In the experiment, before the experiment of the internal circulation Fenton fluidized bed, the iron content of the supporter is 8.3%, the iron content of the supporter after the experiment is 9.7%, and the decolorization rate of methyl orange is 54.9%.
Comparative example 2
The specific preparation scheme of the alkalization modified diatomite-based carrier is as follows:
the method comprises the following steps: putting 100kg of modified diatomite, 10kg of alumina, 12kg of sodium silicate, 0.3kg of ammonium oxalate and 2kg of calcium carbonate into a mixing kettle, mixing and stirring for 20min, then adding 40kg of silica sol with the mass kg of 20% into the mixing kettle, stirring and mixing uniformly, forming, then drying for 1h at 80 ℃ to obtain a carrier embryo body, putting the carrier embryo body into a muffle furnace after completion, controlling the temperature to 600 ℃, calcining for 60min, cooling to room temperature after completion, taking out and crushing into granules;
step two: and adding the obtained support material into a high-speed mixer, controlling the temperature to 200 ℃, then vacuumizing, controlling the vacuum degree to be 0.085MPa, adding 28kg of sodium hydroxide solid, and continuously stirring for dehydration reaction for 60min to obtain the alkalinized modified diatomite-based support.
The preparation method of the modified diatomite comprises the following steps:
adding 100kg of the obtained support material into a high-speed mixer, vacuumizing, controlling the vacuum degree to be 0.085MPa, adding 1000kg of hydrochloric acid with the mass percentage concentration of 10%, controlling the temperature to be 60 ℃, treating for 30min, adding 20kg of phytic acid and 3kg of titanium dioxide, controlling the temperature to be 60 ℃, stirring and reacting for 2h, filtering, and drying to obtain the titanium dioxide-loaded modified diatomite with the phytate groups;
other reaction conditions were the same as in example 1.
In the experiment, before the experiment of the internal circulation Fenton fluidized bed, the iron content of the supporter is 8.2%, the iron content of the supporter after the experiment is 16.2%, and the decolorization rate of methyl orange is 84.2%.
Comparative example 3
The specific preparation scheme of the alkalization modified diatomite-based carrier is as follows:
putting 100kg of modified diatomite, 10kg of alumina, 12kg of sodium silicate, 0.3kg of ammonium oxalate and 2kg of calcium carbonate into a mixing kettle, mixing and stirring for 20min, then adding 40kg of silica sol with the mass kg of 20% into the mixing kettle, stirring and mixing uniformly, forming, then drying for 1h at 80 ℃ to obtain a carrier embryo body, putting the carrier embryo body into a muffle furnace after completion, controlling the temperature to 600 ℃, calcining for 60min, cooling to room temperature after completion, taking out and crushing into granules; thus obtaining the alkalinized modified diatomite-based supporter.
Other reaction conditions were the same as in example 1.
In the experiment, before the experiment of the internal circulation Fenton fluidized bed, the iron content of the supporter is 9.7%, the iron content of the supporter after the experiment is 15.2%, and the decolorization rate of methyl orange is 68.3%.
Claims (5)
1. The preparation process of diatomite-base carrier for efficient oxidation in high density catalytic oxidation tower includes one carrier and one fluidized bed reaction tank, and features the carrier being one kind of alkalization modified diatomite-base carrier.
2. The method for preparing a diatomite-based support for a high-efficiency oxidation high-density catalytic oxidation tower according to claim 1, wherein the method comprises the following steps: the preparation scheme of the alkalization modified diatomite-based support is as follows:
the specific preparation scheme of the alkalization modified diatomite-based carrier is as follows:
the method comprises the following steps: putting 180 parts of modified diatomite 100-28 parts, aluminum oxide 10-28 parts, sodium silicate 12-18 parts, ammonium oxalate 0.3-0.6 part and calcium carbonate 2-6 parts into a mixing kettle, mixing and stirring for 20-30min, then adding silica sol 40-60 parts by mass of 20-30% into the mixing kettle, uniformly stirring and mixing, forming, drying at 80-120 ℃ for 1-4h to obtain a carrier embryo, putting the carrier embryo into a muffle furnace after completion, controlling the temperature to be 600-800 ℃, calcining for 60-120min, cooling to room temperature after completion, taking out and crushing into particles;
step two: adding the obtained support material into a high-speed mixer, controlling the temperature to 200-300 ℃, then vacuumizing, controlling the vacuum degree to 0.085-0.098MPa, adding 28-46 parts of sodium hydroxide solid and 2-5 parts of seleno-diacetic acid, and continuously stirring for dehydration reaction for 60-180min to obtain the alkalinized modified diatomite-based support.
3. The method for preparing the diatomite-based support for the high-efficiency oxidation high-density catalytic oxidation tower according to claim 2, wherein the method comprises the following steps: the preparation method of the modified diatomite comprises the following steps:
adding 150 parts of the obtained carrier material 100-one into a high-speed mixer, vacuumizing, controlling the vacuum degree to be 0.085-0.098MPa, adding 1500 parts of hydrochloric acid with the mass percentage concentration of 10% -15%, controlling the temperature to be 60-80 ℃, treating for 30-60min, adding 20-28 parts of phytic acid and 3-8 parts of titanium dioxide, controlling the temperature to be 60-80 ℃, stirring and reacting for 2-5h, filtering and drying to obtain the titanium dioxide loaded modified diatomite with the phytate group.
4. The method for preparing a diatomite-based support for a high-efficiency oxidation high-density catalytic oxidation tower according to claim 1, wherein the method comprises the following steps: the surface of the alkalinized modified diatomite-based support can form a Fe/titanium layered double hydroxide crystal for catalyzing hydrogen peroxide catalytic oxidation.
5. The method for preparing a diatomite-based support for a high-efficiency oxidation high-density catalytic oxidation tower according to claim 1, wherein the method comprises the following steps: compared with a Fenton oxidation tower, the high-density catalytic oxidation tower with high-efficiency oxidation can reduce the addition of ferrous salt.
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| CN (1) | CN112076751A (en) |
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2020
- 2020-09-24 CN CN202011011621.1A patent/CN112076751A/en not_active Withdrawn
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Application publication date: 20201215 |
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