CN107362769B - Composite material, preparation method and application thereof in sewage biochemical treatment - Google Patents
Composite material, preparation method and application thereof in sewage biochemical treatment Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28019—Spherical, ellipsoidal or cylindrical
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28059—Surface area, e.g. B.E.T specific surface area being less than 100 m2/g
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28064—Surface area, e.g. B.E.T specific surface area being in the range 500-1000 m2/g
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
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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
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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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 discloses a composite material, which is mainly prepared by mixing oxides containing silicon, aluminum and iron elements, has a porous lamellar microspherical structure, and has the diameter of 1-5000 microns and the specific surface area of 50-500m2(ii) in terms of/g. The invention also discloses a preparation method of the composite material, which comprises the steps of firstly preparing sodium silicate, clay and Fe2O3，Al2O3Mixing with strong acid, reaction, adding nitrogen, high-temp calcining, adding water vapor, high-temp high-pressure hydrating, drying, pulverizing and sieving. The invention also provides the application of the composite material in the biochemical treatment of sewage. The biochemical treatment with the assistance of the composite material can effectively treat high-concentration organic pollutants, quickly reduce the COD of the sewage, and effectively remove the contents of ammonia nitrogen, total nitrogen and total phosphorus; meanwhile, the composite material does not contain any environmental pollutants specified by environmental governing departments, and does not generate new environmental pollution in the using process.
Description
Technical Field
The invention mainly relates to the technical field of sewage treatment. In particular to a composite material which can be used in the sewage biochemical treatment process, a preparation method and the application thereof in the sewage biochemical treatment.
Background
The biochemical treatment of sewage, namely microbial treatment, is a general technology for removing organic matters, nitrogen, phosphorus and other nutrients in sewage from a water body by utilizing the growth and metabolism of microorganisms, and is widely applied to the treatment of domestic sewage and industrial sewage. In practical application, the technology adopts a technical scheme taking an activated sludge process as a core. The technical scheme is born before 100 years, and the principle is that nutrient components in the water body are consumed in the process of growth of microorganisms in sewage, and meanwhile, thalli spontaneously aggregate to form a bacterial colony, namely sludge, and the water body is further purified by utilizing the adsorption effect of the bacterial colony. In principle, in the treatment process of the activated sludge method, the microorganisms which play a role mainly exist in the form of bacteria mass, namely sludge, so that not only the sludge is generated, but also the sludge is an essential component of the treatment process. However, the microorganisms act in the form of a bacterial mass, which greatly limits the working efficiency thereof, because only the bacteria on the outer layer of the bacterial mass can contact the flowing water body, the bacteria inside the bacterial mass hardly act, and the larger the volume of the bacterial mass, the lower the treatment efficiency. This is why the higher the concentration of the contaminant, the lower the efficiency of the biochemical treatment of the wastewater.
In addition to the low treatment efficiency, the biochemical sludge generated by the activated sludge process is a very troublesome big problem in the sewage treatment industry. At present, no good method for treating biochemical sludge is generally adopted for treatment by means of incineration and landfill, the former consumes a large amount of energy and generates energy consumption cost, and the latter requires expensive landfill cost and transportation cost, and with the enhancement of environmental management and control, the field available for landfill is increasingly tense, and the landfill cost is continuously increased. Therefore, a great deal of scientific and technological challenges related to sludge reduction are implemented in the industry, however, the core of the activated sludge process is sludge, so that the sludge reduction in the technical principle framework cannot be successful, and the successful technical case of sludge reduction does not exist in reality. Therefore, there is a need in the art for new technologies to improve the efficiency of biochemical reactions, increase stability, and reduce the production and discharge of sludge.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a brand-new composite material with a micro-spherical structure with a porous sheet layer in a micron size, a preparation method and application thereof in sewage biochemical treatment.
The composite material is mainly prepared by mixing oxides containing silicon, aluminum and iron elements, has a porous lamellar microspherical structure, and has the diameter of 1-5000 microns and the specific surface area of 50-500m2/g。
The composite material is characterized in that the oxide containing silicon, aluminum and iron elements mainly comprises sodium silicate, aluminum oxide, iron oxide and clay.
The preparation method of the composite material comprises the following steps:
(1) mixing sodium silicate, clay, ferric oxide, aluminum oxide and acid solution uniformly, and reacting for 3-6 hours at 120-150 ℃;
(2) uniformly mixing the reaction product obtained in the step (1), introducing nitrogen at 95-100 ℃, and continuously blowing the nitrogen for 30-60 minutes;
(3) calcining the product obtained in the step (2) at 600-800 ℃ for 30-360 minutes;
(4) filling steam into the calcined product in the step (3), and hydrating at high temperature and high pressure; the high temperature and high pressure are 3-5 atmospheric pressures and 120-180 ℃;
(5) drying the hydration product in the step (4);
(6) and (4) ultrasonically crushing the dried product, and sieving the crushed product by using a screen to obtain the final required material.
Preferably, in the preparation method, in the step (1), the amount of the clay is 0.3-1.5, the amount of the iron oxide is 0.2-0.5, the amount of the aluminum oxide is 0.2-0.5, and the amount of the acid solute in the acid solution is 0.01-0.06, based on the mass of the sodium silicate being 1; the acid solution is concentrated sulfuric acid or concentrated hydrochloric acid. More preferably, in the step (1), the amount of the clay is 0.3-0.6, the amount of the iron oxide is 0.3-0.5, the amount of the aluminum oxide is 0.3-0.5, and the amount of the acid in the acid solution is 0.02-0.04, based on the mass of the sodium silicate being 1.
Preferably, the above preparation method, step (1), is carried out at 120 ℃ to 130 ℃ for 5 to 6 hours.
Preferably, in the preparation method, in the step (3), the high-temperature calcination temperature is 600-700 ℃, and the calcination time is 30-180 minutes.
Preferably, in the above preparation method, step (4), the high temperature and high pressure are at 3-4 atm and 120-140 ℃.
Preferably, in the above preparation method, step (5), the drying treatment is microwave drying.
Preferably, in the preparation method, step (6), the powder is passed through a 200-400-mesh screen after ultrasonic pulverization.
The invention also provides the application of the composite material in the biochemical treatment of sewage.
Preferably, in the application, the composite material can be directly placed in sewage or combined with aerobic bacteria or anaerobic bacteria commonly used in sewage treatment and placed in the sewage to be treated, and mechanical stirring or aeration mixing is carried out.
Preferably, the application can also be used for loading the composite material into a specific water treatment device or combining the composite material with aerobic bacteria or anaerobic bacteria commonly used in sewage treatment and loading the composite material into the specific water treatment device.
The composite material can fix microorganisms on the surface of the composite material through adsorption, and the composite material has special biocompatibility and can highly support the bacteria after being fixed to continue to grow and divide on the material, which is different from the material of the existing immobilized bacteria. Therefore, the bacteria growing on the material and the material form an organic and complete biochemical treatment unit with micron size, which can decompose the pollutants in water rapidly by biodegradation and conversion, and the organic biochemical treatment unit has obvious difference with the common activated sludge zoogloea in appearance structure and performance.
The composite material carrier supports the growth of microorganisms on the surface of the composite material carrier, the formed sewage treatment unit has extremely small volume and large specific surface area, not only can ensure that microorganism individuals in a bacterial colony are fully contacted with a water body, but also has strong adsorption effect on pollutants in water, and forms an environment with relatively rich nutrients (pollutants) on the surface of the material, thereby greatly improving the treatment efficiency of the microorganisms on the pollutants. Under the action of the material, the biochemical treatment can efficiently remove pollutants such as organic matters, ammonia nitrogen, total nitrogen, phosphorus and the like in the sewage. The strong adsorption of the material can prevent microorganisms from spontaneously forming low-activity sludge cenobium, so that the generation of sludge can be greatly reduced. Can be used for improving the efficiency of biochemical treatment of sewage and reducing sludge generated in the biochemical treatment process. Compared with the prior art, the microorganism can contact with the water body more fully under the action of the composite material, so that the biochemical treatment efficiency is greatly improved.
The composite material has negative charges with higher density, and effectively avoids the formation of bacterial sludge due to spontaneous aggregation among microorganisms through the repulsion action among the charges, thereby greatly reducing the number of ineffective microorganisms and dead microorganisms and finally realizing the great reduction of the total amount of the sludge in biochemical treatment.
The biochemical treatment with the aid of the composite material can effectively treat high-concentration organic pollutants, quickly reduce the Chemical Oxygen Demand (COD) of sewage, and effectively remove the contents of ammonia nitrogen, total nitrogen and total phosphorus. Meanwhile, the composite material does not contain environmental pollutants specified by environmental governing departments, and does not generate new environmental pollution in the using process.
Drawings
FIG. 1 is a flow diagram of the synthetic preparation of the material of the present invention;
FIG. 2 is a scanning electron micrograph of a material of the present invention;
FIG. 3 is a scanning electron micrograph of the formation of active microspheres on the material after bacterial growth;
FIG. 4 is a photograph of a water sample before, during and after treatment of domestic sewage, wherein two parallel samples are taken during treatment;
FIG. 5 is a photograph showing the effect of sludge sedimentation after treatment of domestic sewage with the above-mentioned materials compared with the effect of sludge sedimentation after treatment with a conventional activated sludge process (oxidation ditch technique), wherein the upper graph shows the effect of sludge sedimentation after treatment with a conventional activated sludge process, and the lower graph shows the effect of sludge sedimentation after treatment with the composite material of the present invention.
Detailed Description
The following examples are further illustrative of the present invention as to the technical content of the present invention, but the essence of the present invention is not limited to the following examples, and one of ordinary skill in the art can and should understand that any simple changes or substitutions based on the essence of the present invention should fall within the protection scope of the present invention.
Example 1: synthesis of materials
(1) 100 g of sodium silicate, 30 g of clay (from Wanhong mining Co., Ltd., Qingdao), 30 g of iron oxide (Fe)2O3) 30 g of alumina (Al)2O3) 10ml of concentrated hydrochloric acid (commercially available) are uniformly mixed and reacted for 6 hours in a closed manner at 120 ℃;
(2) uniformly mixing the reaction product obtained in the step (1), introducing nitrogen at 100 ℃, and continuously blowing the nitrogen for 30 minutes;
(3) calcining the product obtained in the step (2) at high temperature of 650 ℃ in air for 30 minutes;
(4) filling the calcined product in the step (3) into water vapor, and hydrating at high temperature and high pressure (3 atmospheric pressure, 120 ℃);
(5) carrying out microwave drying treatment on the hydration product in the step (4);
(6) and (4) ultrasonically crushing the product subjected to the microwave drying treatment, and screening the crushed product through a 320-mesh screen to obtain the final required material.
The material obtained from the above representative synthesis procedure had a particle size of 10 μm and a specific surface area of 195m as determined by the BET method2(ii) in terms of/g. As shown in fig. 2, the material was spherical and had a porous lamellar structure as analyzed by scanning electron microscopy imaging. The material can obtain materials with different specific surface areas by adjusting the hydration degree and the microwave drying process. The material can obtain material particles with different sizes by adjusting the ultrasonic crushing and the mesh number of the screen.
Example 2: materials supporting adherent growth of microorganisms
1g of the material is mixed and dispersed with 100ml of standard LB liquid bacterial culture medium, and then Bacillus subtilis (CGMCC No. 3755) is inoculated, wherein the standard strain is purchased from China general microbiological culture Collection center. The cells were cultured with shaking at 37 ℃ for 12 hours. The material was centrifuged and the non-adsorbed bacteria were washed off by dispersion in physiological saline. After freeze-drying, the samples were analyzed by scanning electron microscopy. As shown in FIG. 3, it can be clearly seen under a scanning electron microscope that the surface of the material is covered by the bacteria which are adhered to and grow, and a microsphere with the bacteria is formed.
Example 3: treatment of typical domestic wastewater
1g of the material is added into 100ml of domestic sewage taken from a domestic sewage plant (a domestic sewage treatment plant on the middle bank of Lishui city, Zhejiang province), and the mixture is stirred at a constant speed at room temperature, wherein the stirring speed is 100 revolutions per minute. After stirring reaction for 6 hours, detecting the indexes of main pollutants in the sewage. The main indices before and after treatment are shown in the following table:
as can be seen from the table, all indexes of the treated sewage are obviously reduced, and all the indexes of the treated sewage meet the requirements of the integrated sewage discharge standard of the people's republic of China (GB 8978-1996) by referring to relevant national environmental protection regulations.
Example 4: treatment of industrial wastewater containing high concentrations of contaminants
1g of the material was added to 100ml of production wastewater from livestock and poultry farms (pig farms) and stirred at room temperature and a stirring rate of 100 revolutions per minute. After stirring reaction for 24 hours, detecting the indexes of main pollutants in the sewage. The main indices before and after treatment are shown in the following table:
as can be seen from the table, all indexes of the treated sewage are obviously reduced, and all the indexes of the treated sewage meet the requirements of the integrated sewage discharge standard of the people's republic of China (GB 8978-1996) by referring to relevant national environmental protection regulations.
Example 5: sludge reduction experiment
10g of the material was added to 1000ml of domestic sewage from a domestic sewage plant, and stirred at room temperature at a constant speed of 100 rpm. After reacting for 6 hours at room temperature, stopping stirring, naturally settling, detecting typical pollution indexes of a supernatant, detecting the volume of the precipitate, drying the precipitate, and weighing. The sewage treated by the existing oxidation ditch technology is used as a contrast. The results are summarized in the following table:
the data in the table show that the material can reduce the sludge volume and dry weight greatly with improved treatment effect.
Claims (7)
1. A composite material is prepared by mixing oxides containing silicon, aluminum and iron elements, has a porous lamellar microspherical structure, and has a diameter of 1-5000 microns and a specific surface area of 50-500m2The oxide containing silicon, aluminum and iron elements is sodium silicate, aluminum oxide, ferric oxide and clay, the mass of the sodium silicate is 1, the clay dosage is 0.3-1.5, the ferric oxide dosage is 0.2-0.5, the aluminum oxide dosage is 0.2-0.5, and the acid dosage in the acid solution is 0.01-0.06;
the preparation method of the composite material comprises the following steps:
(1) mixing sodium silicate, clay, ferric oxide, aluminum oxide and acid solution uniformly, and reacting for 3-6 hours at 120-150 ℃;
(2) uniformly mixing the reaction product obtained in the step (1), introducing nitrogen at 95-100 ℃, and continuously blowing the nitrogen for 30-60 minutes;
(3) calcining the product obtained in the step (2) at 600-800 ℃ for 30-360 minutes;
(4) filling steam into the calcined product in the step (3), and hydrating at high temperature and high pressure; the high temperature and high pressure are 3-5 atmospheric pressures and 120-180 ℃;
(5) drying the hydration product in the step (4);
(6) and (4) ultrasonically crushing the dried product, and sieving the crushed product by using a screen to obtain the final required material.
2. A method of preparing the composite material of claim 1, comprising the steps of:
(1) mixing sodium silicate, clay, ferric oxide, aluminum oxide and acid solution uniformly, and reacting for 3-6 hours at 120-150 ℃;
(2) uniformly mixing the reaction product obtained in the step (1), introducing nitrogen at 95-100 ℃, and continuously blowing the nitrogen for 30-60 minutes;
(3) calcining the product obtained in the step (2) at 600-800 ℃ for 30-360 minutes;
(4) filling steam into the calcined product in the step (3), and hydrating at high temperature and high pressure; the high temperature and high pressure are 3-5 atmospheric pressures and 120-180 ℃;
(5) drying the hydration product in the step (4);
(6) and (4) ultrasonically crushing the dried product, and sieving the crushed product by using a screen to obtain the final required material.
3. The method according to claim 2, wherein in the step (5), the drying treatment is microwave drying.
4. The method as set forth in claim 2, wherein in the step (6), the ultrasonic pulverization is carried out through a 200-400 mesh screen.
5. Use of the composite material according to claim 1 or the composite material obtained by the preparation method according to any one of claims 2 to 4 in the biochemical treatment of wastewater.
6. The use according to claim 5, wherein the composite material is placed directly in the wastewater or is combined with aerobic bacteria or anaerobic bacteria commonly used in wastewater treatment and placed in the wastewater to be treated.
7. The use according to claim 5, wherein the composite material is loaded into a specific water treatment facility or the composite material is used in combination with aerobic bacteria or anaerobic bacteria commonly used in sewage treatment and loaded into a specific water treatment facility.
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| CN108793430B (en) * | 2018-07-03 | 2021-07-06 | 南京大学 | Treating agent for pulp paper wastewater, and preparation method and treatment process thereof |
| CN113736770B (en) * | 2021-10-14 | 2024-03-15 | 南京大学 | Particle strain, preparation method thereof and application thereof in biochemical treatment of sewage |
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