CN115477387A - Anoxic pond enhanced denitrification suspended filler and preparation method thereof - Google Patents
Anoxic pond enhanced denitrification suspended filler and preparation method thereof Download PDFInfo
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- CN115477387A CN115477387A CN202211067363.8A CN202211067363A CN115477387A CN 115477387 A CN115477387 A CN 115477387A CN 202211067363 A CN202211067363 A CN 202211067363A CN 115477387 A CN115477387 A CN 115477387A
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- 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
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention relates to an anoxic pond enhanced denitrification suspended filler and a preparation method thereof, wherein the filler is an active biological filler and comprises the following raw material components in parts by weight: 100 parts of polyethylene; 5-10 parts of sulfur-beta-cyclodextrin inclusion compound; 5-10 parts of molecular sieve activation powder; 3-8 parts of auxiliary materials; the raw materials are subjected to mixing, granulation and extrusion molding to obtain the filler with a plurality of cavities inside. By using alkali modified 4A molecular sieve activation powder, sulfur-beta-cyclodextrin inclusion compound and metal powder, the filler has the performance of quickly enriching anaerobic ammonium oxidation bacteria and nitrobacteria, and is particularly suitable for enhanced nitrogen removal of an anoxic tank; a sulfur-beta-cyclodextrin inclusion compound is introduced, hydrophilic groups on the surface of polyethylene are increased, microorganism adhesion is promoted, a nutrient matrix is provided for the microorganisms, and the film hanging time is reduced; stearic acid and polyethylene wax are added to provide necessary support for ensuring the physical property, the processing property and the like of the filler. The filler disclosed by the invention is simple and efficient to process, flexible in configuration selection, strong in environmental adaptability and has great economic and environmental protection values.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to an anoxic tank enhanced denitrification suspended filler and a preparation method thereof.
Background
The nitrogen-containing substances in the sewage can cause serious eutrophication and water body oxygen deficiency, generate toxicity to aquatic organisms, and inhibit the effect of chlorine sterilization and disinfection, so that the reduction of the nitrogen content in the sewage becomes necessary. Biological sewage treatment methods have been widely used in the fields of municipal sewage, industrial wastewater, and the like, due to their high efficiency and economic feasibility. The existing denitrification process for sewage treatment is mainly based on three-phase reactions of ammoniation, nitrification and denitrification, namely: the organic nitrogen in the water body is firstly converted into ammonia Nitrogen (NH) under the action of ammoniation bacteria 4 + ) I.e. an ammoniation stage; then a nitrification stage is carried out, ammonia nitrogen is converted into NO by nitrosobacteria and nitrobacteria under the aerobic condition 2 ﹣ Or NO 3 ﹣ (ii) a The final denitrification stage is to convert nitrite nitrogen and nitrate nitrogen into nitrogen (N) by denitrifying bacteria under anoxic condition 2 )。
In recent years, the anaerobic ammonia oxidation process breaks through the basic theoretical concept in the traditional biological denitrification process, autotrophic anaerobic ammonia-oxidizing bacteria take ammonia as an electron donor and nitrite as an electron acceptor under anaerobic conditions to oxidize the ammonia into nitrogen, so that the anaerobic ammonia-oxidizing bacteria have the advantages of saving aeration, needing no organic carbon source, being small in residual sludge amount and the like, and the anaerobic ammonia oxidation effect is found in an oxygen-deficient (anaerobic) pond of a town sewage treatment plant in recent years, so that the anaerobic ammonia-oxidizing bacteria have the condition of generating anaerobic ammonia oxidation under the condition of the ammonia nitrogen concentration of Chi Zhongdi in the anaerobic (anaerobic) oxygen of the sewage treatment plant.
The consumption of an external carbon source is reduced, the ammonia nitrogen removal rate is improved, and the anaerobic ammonia oxidation of the anoxic tank is promoted to become one of the methods for strengthening denitrification. However, the sludge in the anoxic tank does not have the function of enriching the anammox bacteria, and the traditional suspension carrier does not promote the growth and reproduction of the anammox bacteria, so that the anammox generation degree is low and the denitrification capability is poor.
The development and development of biological carriers, which are places on which microorganisms live, are important links for the development of a fixed bed or moving bed biofilm reaction process. However, most of the bio-carriers produced in China directly process and mold high molecular materials, so the produced bio-carriers have the defects of low film formation speed, poor biological affinity, easy falling of the bio-films, low ammonia nitrogen removal efficiency and the like. The patent CN103420490B provides a surface electrophilic biological carrier which can improve the biological affinity of the surface of the carrier, has high removal efficiency on organic matters and ammonia nitrogen, and is simple and convenient in production method, wherein the biological carrier takes polyethylene or polypropylene as a polymer base material and also comprises an electrophilic functional material; the electrophilic functional material is provided with positive electricity, so that the surface of the biological carrier is provided with positive charges with different degrees, the electrophilic functional material has good biological affinity with microorganisms with negative electricity, the membrane hanging period is shortened, the microorganisms are not easy to fall off, and the microbial biomass on the surface of the biological carrier is large; can provide a good growth environment for autotrophic nitrifying bacteria and heterotrophic denitrifying bacteria in water. Although the biological carrier improves electrophilicity and is beneficial to microorganism attachment, the biological carrier does not relate to the promotion effect on the growth and reproduction of the anammox bacteria, so that the anammox technology is not suitable for the biological carrier, and the denitrification capability is limited.
Based on this, how to make the biological carrier have the rapid enrichment performance of the anammox bacteria, and simultaneously improve the comprehensive performances such as hydrophilicity, suspension stability and the like of the biological carrier so as to realize better denitrification effect of the anoxic tank becomes a technical problem to be solved in the field.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide an anoxic pond enhanced denitrification suspended filler and a preparation method thereof. Through designing and improving the traditional suspended biological carrier, the anaerobic ammonium oxidation bacteria carrier has the rapid enrichment performance of anaerobic ammonium oxidation bacteria, and has better comprehensive performances such as hydrophilicity, suspension stability and the like, so as to realize better denitrification effect of an anoxic tank.
Specifically, the invention provides an anoxic pond enhanced denitrification suspended filler, which is an active biological filler and comprises the following raw material components in parts by weight:
100 portions of polyethylene
5-10 parts of sulfur-beta-cyclodextrin inclusion compound
5-10 parts of molecular sieve activation powder
3-8 parts of auxiliary materials;
the particle sizes of the molecular sieve activation powder, the sulfur-beta-cyclodextrin inclusion compound and the auxiliary materials are all less than 200 meshes;
the raw material components are subjected to melt extrusion molding to obtain the filler with a plurality of cavities inside.
Preferably, the polyethylene is a high density polyethylene. The use of polyethylene, particularly high density polyethylene, provides the filler of the present invention with good mechanical and processing properties, as well as a relatively low density, which facilitates the formation of a stable suspended filler. The high-density polyethylene is preferably high-density polyethylene pure raw material, and reclaimed materials can be properly added on the basis of reducing the cost, but the weight of the reclaimed materials is not more than 5 percent of the total weight of the high-density polyethylene.
Furthermore, the auxiliary materials comprise stearic acid, polyethylene wax and metal powder, wherein the metal powder is one or more of ferroferric oxide powder, iron oxide powder, reduced iron powder and manganese carbonate powder.
Stearic acid improves the transition from the hydrophilicity to the hydrophobicity of the clathrate compound master batch, and improves the affinity between the clathrate compound master batch and polyethylene, and the using amount of the stearic acid is preferably 1 to 3 parts by weight.
The polyethylene wax has good compatibility with polyethylene, plays a role of a cosolvent and a lubricant in polyethylene processing, can improve the processing performances such as melt flowability, demolding performance and the like, and improves the comprehensive high performances such as wear resistance, stability and the like of the filler, and the dosage of the polyethylene wax is preferably 1 to 3 parts by weight.
The metal powder is preferably used in an amount of 1 to 3 parts by weight. The metal ions have different promoting effects on anaerobic ammonia oxidation, fe 2+ Can be used as a coenzyme factor of Fe-S protein and hemoprotein to participate in the electron transfer process of anaerobic ammonium oxidation bacteria and promote NH 4+ -N to N 2 Is rotatedAnd can promote metabolism of anammox bacteria. Mn 2+ Is an activator of enzyme, and can promote metabolism of anammox bacteria by increasing enzyme activity. Fe 3+ As an electron acceptor in the anaerobic ammonia oxidation metabolism, the enrichment of anaerobic ammonia oxidation bacteria can be promoted. When the filler is loaded with the metal ions, the metabolism of the anaerobic ammonium oxidation bacteria can be obviously promoted, the enzyme activity of the anaerobic ammonium oxidation bacteria is improved, and the denitrification effect is improved.
Further, the sulfur-beta-cyclodextrin inclusion compound is prepared by the following method:
1) Adding 1.5-3 times of water into beta-cyclodextrin, mixing, and grinding to obtain a mixture;
2) Adding carbon disulfide organic solvent dissolved with sulfur powder into the mixture, fully grinding the mixture into paste, and drying the paste at 35-45 ℃;
3) Cleaning redundant sulfur powder with carbon disulfide, and drying again;
4) Crushing the mixture by a jet mill to obtain the sulfur-beta-cyclodextrin inclusion compound.
Preferably, the sulfur powder used in the preparation of the sulfur- β -cyclodextrin inclusion compound is a sulfur powder having a purity of 99% or more. The difference with the prior art is that in the filler of the invention, the function of sulfur does not only provide sulfur autotrophic denitrification, but nitrate nitrogen is reduced into nitrite nitrogen under the action of sulfur autotrophic denitrifying bacteria in the initial stage, so as to promote the generation and enrichment of anammox bacteria, and the anammox bacteria convert nitrite nitrogen and ammonia nitrogen into nitrogen. At the initial stage of biofilm formation, the biofilm formation speed of anaerobic ammonia oxidizing bacteria is improved through the promotion effect of sulfur autotrophic denitrification, so that the denitrification process is more efficient.
The sulfur-beta-cyclodextrin inclusion compound and high-density polyethylene are preferably prepared into master batch in advance, the master batch has excellent hydrophilic performance, can improve the overall hydrophilicity of products, and provides conditions for the effects of enhancing the microorganism attachment capacity of a suspended carrier, shortening the film forming time and the like.
More preferably, the sulfur-beta-cyclodextrin inclusion compound and part of the high-density polyethylene are melted, mixed and crushed to obtain the sulfur-beta-cyclodextrin inclusion compound polyethylene master batch, and the specific method comprises the following steps:
adding 30-40 parts of polyethylene into a plasticator, and melting at 175 +/-3 ℃; then adding 5-10 parts of sulfur-beta-cyclodextrin inclusion compound, mixing for 6-8 minutes, slicing and crushing into micron-sized particle master batch.
The content and the use mode of the sulfur-beta-cyclodextrin inclusion compound are selected, so that on one hand, enough hydrophilicity is provided for polyethylene products; on the other hand, the sulfur powder included in the sulfur powder can be attached to and utilized by sulfur autotrophic denitrifying bacteria.
Particularly advantageously, the surface roughness of the filler is improved and microorganisms are easy to attach in the process of consuming components such as cyclodextrin, sulfur powder and the like.
Further, the molecular sieve activation powder is 4A molecular sieve activation powder, particularly preferably alkali-modified 4A molecular sieve activation powder, and is prepared by the following method:
1) Soaking 4A molecular sieve activated powder in distilled water, performing ultrasonic treatment for 1-3h, filtering, and drying at 100-110 ℃;
2) Soaking the dried 4A molecular sieve activated powder in a NaOH solution with the concentration of 1-2mol/L, heating to 70-90 ℃, and treating for 5-8h;
3) Acting under 500-700W microwave power for 1-3min, and filtering;
4) Repeatedly washing the molecular sieve activated powder with distilled water, and drying at 100-110 ℃ after the filtrate is neutral; and crushing into the alkali modified 4A molecular sieve activation powder.
The molecular sieve activating powder can increase the ammonia nitrogen adsorption performance of the filler, and the content of the molecular sieve activating powder is 5-10 parts by weight, preferably 8-10 parts by weight. When the content is too low, the total amount of adsorbed ammonia nitrogen is too low, which is not beneficial to realizing high-efficiency denitrification, and when the content is too high, the product becomes brittle and the loss factor is increased. After the molecular sieve activating powder is treated by the method, the purity of the molecular sieve activating powder is improved, and the adsorption efficiency is obviously improved.
The active biological suspended filler is generally in a cylindrical structure, a plurality of cavities are arranged in the active biological suspended filler, the active biological suspended filler is preferably cylindrical, the diameter is 10-50mm, the height is 2-15mm, the wall thickness is 0.33-0.55mm, the effective specific surface area can be freely designed according to different internal structural designs, and the optimal specific surface area is more than 1000m 2 /m 3 More preferably greater than 1200m 2 /m 3 . The filler can be designed to be provided with a plurality of radiating fins outwards along the radial direction of the filler and connected to the inner wall of the cylinder, and the inside of the cylinder further comprises a plurality of reinforcing ribs connected with adjacent radiating fins. Further, the outer wall of the cylinder has a plurality of outwardly extending protrusions. The above designs are merely examples and are not intended to be exhaustive or limiting of the present invention, and in practice, depending on the mold and process conditions, a variety of structures and designs having a large effective specific surface area may be used in the filler configuration of the present invention.
In addition, in order to further improve the effective specific surface area and further improve the denitrification efficiency, a proper amount of foaming agent is added in the melt extrusion molding process, the filler with a foaming porous structure is obtained simultaneously in the extrusion molding process, the effective specific surface area of the filler can be improved by at least 20% compared with the filler with the same macroscopic configuration, and the macroscopic structure and the microscopic structure are combined, so that the effective specific surface area of the suspended filler can be easily obtained to be larger than 1200m on the basis of free design 2 /m 3 Preferably greater than 1400m 2 /m 3 The effective specific surface area of (a). Therefore, the invention can effectively improve and design the effective specific surface area of the required filler according to requirements by combining the macroscopic cavity structure design and the microscopic porous structure design, so that the suspension filler can adapt to various application environments.
The denitrification efficiency of the filler is not only influenced by the effective specific surface area, but also is very relevant to the surface activity of the filler. In order to further increase the surface activity of the active biological suspension filler, the filler product is preferably additionally subjected to a surface treatment, for example, a plasma treatment, a corona treatment, a glow discharge treatment, or a sputtering treatment. Plasma treatment and corona treatment are preferred, and a sufficient amount of polar groups can be introduced to the surface of the filler.
As a method and an apparatus for performing the plasma treatment, there are included: a device of a high-frequency induction type, a capacitive coupling type electrode type, a corona discharge electrode-plasma spray type, a parallel flat plate type, a remote plasma type, an atmospheric pressure plasma type, an ICP type high-density plasma type is used. The energy of the generated electrons is controlled to be 1-10eV, and the treatment time is 1-30 minutes, preferably 2-10 minutes. The filler is preferably subjected to plasma treatment in an atmosphere containing at least 1 kind selected from the group consisting of argon, helium and oxygen, in combination with introduction of the polar group species and treatment effectiveness.
Corona treatment, discharge voltage control at 9500V/m 2 -18000V/m 2 。
After the surface treatment, a large number of active groups are loaded on the surface of the filler, so that the attachment of microorganisms is easy.
Aiming at the suspended filler, the invention correspondingly provides a preparation method of the anoxic pond enhanced denitrification suspended filler, which comprises the following steps:
s1: mixing: adding 30-40 parts of polyethylene into a plasticator, and melting at 175 +/-3 ℃; adding 5-10 parts of sulfur-beta-cyclodextrin inclusion compound, mixing for 6-8 minutes, slicing and crushing into a micron-sized particle master batch;
s2: material blending: mixing the master batch, the rest polyethylene, the molecular sieve activated powder and the auxiliary materials by a high-speed mixer to obtain a mixture;
s3: and (3) granulation: extruding and granulating the mixture through a screw extruder;
s4: and (3) extrusion molding: and (4) melting and extruding the granules obtained in the step (S3) through a screw extruder, cooling and shaping, cutting and collecting.
The raw materials of the invention are formed by mixing, granulating and extruding through a screw extruder. On one hand, the sulfur-beta-cyclodextrin inclusion compound is favorably and fully fused with polyethylene, and the hydrophilicity of the master batch is improved; the stearic acid serving as the auxiliary material is favorable for improving the dispersion uniformity of the master batch containing the sulfur-beta-cyclodextrin inclusion compound in the filler and improving the affinity between the hydrophilic master batch and the hydrophobic polyethylene.
Preferably, in step S2, the rotational speed of the high-speed stirrer is 200-400rpm, and the temperature is 100-120 ℃. In step S4, the temperature of the melting cylinder of the screw extruder is 150-170 ℃.
Further, in step S4, the screw extruder adopts five sections of independent temperature control: the first section is 145-155 ℃, the second section is 160-170 ℃, the third section is 165-175 ℃, the fourth section is 160-170 ℃, and the fifth section is 155-165 ℃; and immediately performing water cooling setting after extrusion. The segmented temperature control mode of 'two ends are low and the middle is high' is adopted, so that the materials are fully melted and mixed in the front section, and are cooled and extruded in the rear section, the extrusion swelling deformation is prevented, and the preparation method is more favorable for preparing products with fine and stable structures.
On the other hand, in order to prepare the filler with a foamed porous structure, it is preferable that in the step S4, the pellets obtained in the step S3 are fed into the screw extruder together with a blowing agent in an amount of 0.1 to 1%, preferably 0.2 to 0.4% by weight based on the polyethylene. The blowing agent may be selected from those commonly used in the art, which meet the melt extrusion conditions, such as azodicarbonamide (ADCA), sodium bicarbonate, and the like; the dosage of the foaming agent is strictly controlled according to the use environment of the filler, effective surface pores are difficult to form due to too low dosage, and the foaming and pore-forming effect cannot be achieved; too high a quantity may damage the overall structure, reduce the mechanical properties, be unfavorable for the long-term stable use of the filler.
The suspended filler can effectively promote the growth and reproduction of anammox bacteria, has excellent biological activity, and is particularly suitable for enhanced denitrification in an anoxic pond. In addition, based on the excellent structural design and material components of the suspended filler, the suspended filler can also be used for purification treatment of other water bodies, and has wide application and great value.
The invention has the advantages that:
1) The anoxic pond enhanced denitrification suspended filler has better synergistic effect and practical effect on material composition and proportion:
first, polyethylene, particularly high density polyethylene (density of 0.940-0.960 g/cm) 3 ) The high-density polyethylene is a base material, provides basic conditions for the suspension property of the filler, has excellent comprehensive performance, and can meet the requirements of various aspects such as production, use, transportation and the like of the filler; in addition, the sulfur-beta-cyclodextrin inclusion compound is added into the filler, so that the defect of poor hydrophilicity of the high-density polyethylene base material can be overcome, the hydrophilicity of the filler is improved from the material component, and the film forming speed is favorably improvedThe rate is increased.
Secondly, alkali modified 4A molecular sieve activated powder is used, so that the ammonia nitrogen adsorption performance of the filler is improved. Adding sulfur-beta-cyclodextrin inclusion compound, reducing the nitrate nitrogen into nitrite nitrogen under the action of sulfur autotrophic denitrifying bacteria, and converting the nitrite nitrogen and ammonia nitrogen into nitrogen by anaerobic ammonium oxidation bacteria. The biofilm formation speed of the anaerobic ammonia oxidizing bacteria is improved by the promoting effect of sulfur autotrophic denitrification at the initial biofilm formation. Meanwhile, by adding the metal powder, the filler is loaded with metal ions, so that the metabolism of the anaerobic ammonia oxidizing bacteria can be promoted, the enzyme activity of the anaerobic ammonia oxidizing bacteria can be improved, and the denitrification effect can be improved.
On the other hand, because the functional components are added into the base material, in order to ensure the processing performance and the quality of a formed product of the filler, the polyethylene wax serving as an auxiliary material is preferably added to adjust the compatibility among the components, improve the processing performance and be beneficial to increasing the comprehensive performances such as the wear resistance, the stability and the like of the filler.
2) The invention adopts mixing, granulation and extrusion molding of a screw extruder, and effectively realizes the modification of the sulfur-beta-cyclodextrin inclusion compound on polyethylene so as to improve the hydrophilicity of the filler; in addition, the foaming agent is added to obtain the foaming porous filler, and the effective specific surface area of the filler is improved and regulated by combining the macroscopic cavity structure design and the microscopic porous structure design, so that the suspension filler disclosed by the invention can adapt to various application environments.
3) The active biological suspended filler provided by the invention has the advantages of good enrichment effect of anaerobic ammonium oxidation bacteria, high denitrification efficiency, stable structure, simple preparation method of the filler, low cost, good environmental adaptability, long service cycle and wide application prospect.
Drawings
FIG. 1 shows a schematic structural view of a cross-section of a packing according to a first group of embodiments of the present invention;
FIG. 2 shows a schematic structural view of a cross section of a packing according to a second group of embodiments of the present invention;
fig. 3 shows a schematic structural view of a cross section of a packing according to a third group of embodiments of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below.
The anoxic tank enhanced denitrification suspended filler is an active biological filler and comprises the following raw material components in parts by weight:
100 portions of polyethylene
5-10 parts of sulfur-beta-cyclodextrin inclusion compound
5-10 parts of molecular sieve activation powder
3-8 parts of auxiliary materials;
the particle sizes of the molecular sieve activation powder, the sulfur-beta-cyclodextrin inclusion compound and the auxiliary materials are all less than 200 meshes;
the raw material components are subjected to melt extrusion molding to obtain the filler with a plurality of cavities inside.
In order to prepare the enhanced denitrification suspended filler for the anoxic pond, the invention adopts the following preparation method, which specifically comprises the following steps:
step one, preparing alkali modified 4A molecular sieve activated powder:
1) Soaking 4A molecular sieve activated powder in distilled water, performing ultrasonic treatment for 1-3h, filtering, and drying at 100-110 ℃;
2) Soaking the dried 4A molecular sieve activated powder in a NaOH solution with the concentration of 1-2mol/L, heating to 70-90 ℃, and treating for 5-8h;
3) Acting under 500-700W microwave power for 1-3min, and filtering;
4) Repeatedly washing the molecular sieve activated powder with distilled water, and drying at 100-110 ℃ after the filtrate is neutral; and crushing the mixture into the alkali modified 4A molecular sieve activation powder, wherein the particle size of the activation powder is less than 200 meshes.
Step two, preparing the sulfur-beta-cyclodextrin inclusion compound:
1) Adding 1.5-3 times of water into beta-cyclodextrin, mixing, and grinding to obtain a mixture;
2) Adding carbon disulfide organic solvent dissolved with sulfur powder into the mixture, fully grinding the mixture into paste, and drying the paste at 35-45 ℃; the purity of the sulfur powder is more than 99 percent;
3) Cleaning redundant sulfur powder with carbon disulfide, and drying again;
4) Crushing the mixture by a jet mill to obtain the sulfur-beta-cyclodextrin inclusion compound.
Step three, mixing, granulating and extrusion molding:
s1: mixing: adding 30-40 parts of polyethylene into a plasticator, and melting at 175 +/-3 ℃; adding 5-10 parts of sulfur-beta-cyclodextrin inclusion compound, mixing for 6-8 minutes, slicing and crushing into a micron-sized particle master batch;
s2: material blending: mixing the master batch, the rest polyethylene, the molecular sieve activated powder and the auxiliary materials by a high-speed mixer to obtain a mixture; preferably, the particle sizes of the molecular sieve activation powder, the sulfur-beta-cyclodextrin inclusion compound and the auxiliary materials are all smaller than 200 meshes; the auxiliary materials preferably comprise 1-3 parts of stearic acid, 1-3 parts of polyethylene wax and 1-3 parts of metal powder, wherein the metal powder is one or more of ferroferric oxide powder, iron oxide powder, reduced iron powder and manganese carbonate powder; the rotating speed of the high-speed stirrer is 200-400rpm, and the temperature is 100-120 ℃;
s3: and (3) granulation: extruding and granulating the mixture through a screw extruder; the temperature of a material cylinder of the screw extruder is 150-170 ℃;
s4: and (3) extrusion molding: and (4) melting and extruding the granules obtained in the step (S3) through a screw extruder, cooling and shaping, cutting and collecting. Preferably, the screw extruder adopts five sections for independent temperature control: the temperature of the first section is 145-155 ℃, the temperature of the second section is 160-170 ℃, the temperature of the third section is 165-185 ℃, the temperature of the fourth section is 160-170 ℃, and the temperature of the fifth section is 155-165 ℃; and immediately performing water cooling setting after extrusion.
By the method, the oxygen tank enhanced denitrification suspended filler with a plurality of cavities inside is prepared.
When the foamed cellular filler is to be prepared, the above step S4 is: and (3) extrusion molding: and (4) adding the granules obtained in the step (S3) and the foaming agent into an extruder, melting, extruding by using a screw extruder, cooling and shaping, cutting and collecting. Wherein the foaming agent can be selected from foaming agents commonly used in the art, such as azodicarbonamide (ADCA), sodium bicarbonate, etc., and is used in an amount of 0.1-1% by weight of the polyethylene.
By the method, the prepared suspended filler has effective specific surface area which is higher than that of the same macroscopic configurationAt least 20% higher than the total weight of the filler (B), and can easily obtain a filler with a thickness of more than 1200m 2 /m 3 Preferably greater than 1400m 2 /m 3 The effective specific surface area of (a).
In order to more clearly illustrate the objects, technical solutions and technical effects of the present invention, the present invention will be further described in detail with reference to the following examples, comparative examples and the accompanying drawings.
The examples of the invention are mainly divided into three groups of embodiments for comparison:
a first set of embodiments, examples 1-2, comparative example 1, macrostructures, see figure 1;
a second set of embodiments, examples 3-4, comparative example 2, macrostructures see figure 2;
a third set of embodiments, examples 5-7, the macrostructures of which are shown in figure 3;
it should be noted that the cross-sectional structural schematic diagrams of the product of the present invention are only shown in fig. 1-3, and do not limit the specific structure of the product of the present invention, the filler of the present invention has various configurations, for example, the cross-sectional shape can be selected from circular, square, polygonal, etc., and the specific configuration and the corresponding effective specific surface area can be designed and controlled according to the application environment and requirements.
Example 1
The enhanced denitrification suspended filler for the anoxic tank comprises the following raw material components in parts by weight:
100 portions of high-density polyethylene
5 parts of sulfur-beta-cyclodextrin inclusion compound
10 portions of alkali modified 4A molecular sieve activated powder
Stearic acid 1 part
2 parts of manganese carbonate powder
And 2 parts of polyethylene wax.
The preparation method integrally comprises the following steps:
step one, preparing alkali modified 4A molecular sieve activated powder:
1) Soaking 4A molecular sieve activated powder in distilled water, performing ultrasonic treatment for 1h, filtering, and drying at 105 ℃;
2) Soaking the dried 4A molecular sieve activated powder in a NaOH solution with the concentration of 1.5mol/L, heating the solution at the temperature of 80 ℃, and treating the solution for 6 hours;
3) Acting for 2min under 600W microwave power, and filtering;
4) Repeatedly washing the molecular sieve activated powder with distilled water, and drying at 105 ℃ after the filtrate is neutral; and crushing the mixture into the alkali modified 4A molecular sieve activation powder, wherein the particle size of the activation powder is less than 200 meshes.
Step two, preparing the sulfur-beta-cyclodextrin inclusion compound:
1) Adding 2 times of water into beta-cyclodextrin, mixing, and grinding uniformly to obtain a mixture;
2) Adding a carbon disulfide organic solvent dissolved with sulfur powder into the mixture, fully grinding the mixture into paste, and drying the paste at 40 ℃; the purity of the sulfur powder is more than 99 percent;
3) Cleaning redundant sulfur powder with carbon disulfide, and drying again;
4) Crushing the mixture by a jet mill to obtain the sulfur-beta-cyclodextrin inclusion compound.
Step three, mixing, granulating and extrusion molding:
s1: mixing: adding 30 parts of high-density polyethylene into a plasticator, and melting at 175 +/-3 ℃; adding 5 parts of sulfur-beta-cyclodextrin inclusion compound, mixing for 6 minutes, discharging and crushing into a micron-sized particle master batch;
s2: material blending: mixing the master batch, the rest 70 parts of high-density polyethylene, molecular sieve activation powder, stearic acid, manganese carbonate powder and polyethylene wax by a high-speed mixer to obtain a mixture; the particle sizes of the molecular sieve activation powder, the sulfur-beta-cyclodextrin inclusion compound and the auxiliary materials are all less than 200 meshes; the rotating speed of the high-speed stirrer is 300rpm, and the temperature is 100-120 ℃;
s3: and (3) granulation: extruding and granulating the mixture through a screw extruder; the temperature of a material cylinder of the screw extruder is 150-170 ℃;
s4: and (3) extrusion molding: and (4) melting and extruding the granules obtained in the step (S3) through a screw extruder, wherein the screw extruder adopts five sections to independently control the temperature: the first section is 150 ℃, the second section is 165 ℃, the third section is 175 ℃, the fourth section is 165 ℃ and the fifth section is 160 ℃; and (5) immediately performing water cooling setting after extrusion, and collecting cut materials.
By the above method, the filler having a plurality of cavities inside according to the first group of embodiments of the present invention is prepared, and the effective specific surface area thereof is about 450m 2 /m 3 See fig. 1.
Example 2
This example is the same as the filler composition of example 1, with the main difference that the foaming agent is added during extrusion molding in the preparation process to obtain a foamed cellular filler, comprising the following steps:
s1: mixing: adding 30 parts of high-density polyethylene into a plasticator, and melting at 175 +/-3 ℃; adding 5 parts of sulfur-beta-cyclodextrin inclusion compound, mixing for 6 minutes, discharging and crushing into a micron-sized particle master batch;
s2: material blending: mixing the master batch, the rest 70 parts of high-density polyethylene, molecular sieve activation powder, stearic acid, manganese carbonate powder and polyethylene wax by a high-speed mixer to obtain a mixture; the particle sizes of the molecular sieve activation powder, the sulfur-beta-cyclodextrin inclusion compound and the auxiliary materials are all less than 200 meshes; the rotating speed of the high-speed stirrer is 300rpm, and the temperature is 100-120 ℃;
s3: and (3) granulation: extruding and granulating the mixture through a screw extruder; the temperature of a charging barrel of the screw extruder is 150-170 ℃;
s4: and (3) extrusion molding: adding the granules obtained in the step S3 and 0.25 weight part of azodicarbonamide (ADCA) into a screw extruder, and carrying out melt extrusion, wherein the screw extruder is provided with a five-way heating device and is used for independently controlling the temperature of a charging barrel in a partition manner, and the partition temperature is as follows: 150 ℃,165 ℃,175 ℃,165 ℃, and 160 ℃. Immediately after extrusion, the material was water-cooled and cut into a desired length.
Through the method, the foaming porous filler with a plurality of cavities inside is prepared, and the effective specific surface area of the foaming porous filler is about 600m 2 /m 3 。
Example 3
This example is identical to example 1 in terms of filler composition and preparation method, and the main difference is that the extrusion molding die is different, and the filler having a plurality of cavities inside, according to the second group of embodiments of the present invention, is prepared, and the effective specific surface area of the filler is about 800m 2 /m 3 See fig. 2.
Example 4
This example is the same as example 3 in terms of filler composition, with the main difference that in the preparation method, the foaming agent is added during extrusion molding to obtain the foamed cellular filler, comprising the following steps:
s1: mixing: adding 30 parts of high-density polyethylene into a plasticator, and melting at 175 +/-3 ℃; adding 5 parts of sulfur-beta-cyclodextrin inclusion compound, mixing for 6 minutes, discharging and crushing into a micron-sized particle master batch;
s2: material blending: mixing the master batch, the rest 70 parts of high-density polyethylene, molecular sieve activation powder, stearic acid, manganese carbonate powder and polyethylene wax by a high-speed mixer to obtain a mixture; the particle sizes of the molecular sieve activation powder, the sulfur-beta-cyclodextrin inclusion compound and the auxiliary materials are all less than 200 meshes; the rotating speed of the high-speed stirrer is 300rpm, and the temperature is 100-120 ℃;
s3: and (3) granulation: extruding and granulating the mixture through a screw extruder; the temperature of a charging barrel of the screw extruder is 150-170 ℃;
s4: and (3) extrusion molding: adding the granules obtained in the step S3 and 0.25 part by weight of azodicarbonamide (ADCA) into a screw extruder together, and carrying out melt extrusion, wherein the screw extruder is provided with a five-way heating device and is used for independently controlling the temperature of a charging barrel in a partition mode, and the partition temperature is as follows: 150 ℃,165 ℃,175 ℃,165 ℃, and 160 ℃. Immediately after extrusion, the material was water-cooled and cut into a desired length.
Through the method, the foaming porous filler with a plurality of cavities inside is prepared, and the effective specific surface area of the foaming porous filler is about 1000m 2 /m 3 。
Example 5
The anoxic pond enhanced denitrification suspended filler comprises the following raw material components in parts by weight:
100 portions of high-density polyethylene
10 portions of sulfur-beta-cyclodextrin inclusion compound
5 parts of alkali modified 4A molecular sieve activated powder
Stearic acid 1 part
Ferroferric oxide 2 parts
And 2 parts of polyethylene wax.
The preparation method integrally comprises the following steps:
step one, preparing alkali modified 4A molecular sieve activated powder:
1) Soaking 4A molecular sieve activated powder in distilled water, performing ultrasonic treatment for 1h, filtering, and drying at 105 ℃;
2) Soaking the dried 4A molecular sieve activated powder in a NaOH solution with the concentration of 1.5mol/L, heating the solution at the temperature of 80 ℃, and treating the solution for 6 hours;
3) Acting for 2min under 600W microwave power, and filtering;
4) Repeatedly washing the molecular sieve activated powder with distilled water, and drying at 105 ℃ after the filtrate is neutral; and crushing the mixture into the alkali modified 4A molecular sieve activated powder, wherein the particle size of the alkali modified 4A molecular sieve activated powder is less than 200 meshes.
Step two, preparing the sulfur-beta-cyclodextrin inclusion compound:
1) Adding 2 times of water into beta-cyclodextrin, mixing, and grinding uniformly to obtain a mixture;
2) Adding a carbon disulfide organic solvent dissolved with sulfur powder into the mixture, fully grinding the mixture into paste, and drying the paste at 40 ℃; the purity of the sulfur powder is more than 99 percent;
3) Cleaning redundant sulfur powder with carbon disulfide, and drying again;
4) Crushing the mixture by a jet mill to obtain the sulfur-beta-cyclodextrin inclusion compound.
Step three, mixing, granulating and extrusion molding:
s1: mixing: adding 40 parts of high-density polyethylene into a plasticator, and melting at 175 +/-3 ℃; then adding 10 parts of sulfur-beta-cyclodextrin inclusion compound, mixing for 8 minutes, feeding and crushing into a micron-sized particle master batch;
s2: material blending: mixing the master batch, the rest 60 parts of high-density polyethylene, molecular sieve activating powder, stearic acid, ferroferric oxide and polyethylene wax by a high-speed mixer to obtain a mixture; the particle sizes of the molecular sieve activation powder, the sulfur-beta-cyclodextrin inclusion compound and the auxiliary materials are all less than 200 meshes; the rotating speed of the high-speed stirrer is 300rpm, and the temperature is 100-120 ℃;
s3: and (3) granulation: extruding and granulating the mixture through a screw extruder; the temperature of a material cylinder of the screw extruder is 150-170 ℃;
s4: and (3) extrusion molding: and (4) melting and extruding the granules obtained in the step (S3) through a screw extruder, wherein the screw extruder adopts five sections to independently control the temperature: the first section is 150 ℃, the second section is 165 ℃, the third section is 175 ℃, the fourth section is 165 ℃ and the fifth section is 160 ℃; and (5) immediately performing water cooling setting after extrusion, and collecting cut materials.
By the above method, a packing having a plurality of cavities inside according to the third group of embodiments of the present invention, which had a size of about 1200m, was prepared 2 /m 3 Effective specific surface area, see fig. 3.
Example 6
This example is the same as example 5 in terms of filler composition, with the main difference that the foaming agent is added during extrusion molding in the preparation process to obtain a foamed cellular filler, comprising the following steps:
s1: mixing: adding 40 parts of high-density polyethylene into a plasticator, and melting at 175 +/-3 ℃; adding 10 parts of sulfur-beta-cyclodextrin inclusion compound, mixing for 8 minutes, blanking and crushing into a micron-sized particle master batch;
s2: material blending: mixing the master batch, the rest 60 parts of high-density polyethylene, molecular sieve activating powder, stearic acid, ferroferric oxide and polyethylene wax by a high-speed mixer to obtain a mixture; the particle sizes of the molecular sieve activation powder, the sulfur-beta-cyclodextrin inclusion compound and the auxiliary materials are all less than 200 meshes; the rotating speed of the high-speed stirrer is 300rpm, and the temperature is 100-120 ℃;
s3: and (3) granulation: extruding and granulating the mixture through a screw extruder; the temperature of a material cylinder of the screw extruder is 150-170 ℃;
s4: and (3) extrusion molding: adding the granules obtained in the step S3 and 0.25 part by weight of azodicarbonamide (ADCA) into a screw extruder together, and carrying out melt extrusion, wherein the screw extruder is provided with a five-way heating device and is used for independently controlling the temperature of a charging barrel in a partition mode, and the partition temperature is as follows: 150 ℃,165 ℃,175 ℃,165 ℃, and 160 ℃. Immediately after extrusion, the material was water-cooled and cut into a desired length.
By the above method, theThe foamed porous suspension packing of the invention having a plurality of cavities inside is prepared, having a thickness of more than 1400m 2 /m 3 Effective specific surface area.
Example 7
This example is the same as the filler composition and preparation method of example 6, except that the filler was subjected to plasma surface treatment, the energy of generated electrons was controlled at 8eV in an oxygen atmosphere, and the treatment time was 5 minutes.
Comparative example 1
Unmodified polyethylene fillers of the same type as in examples 1-2, see FIG. 1, having an effective specific surface area of about 450m 2 /m 3 。
Comparative example 2
Unmodified polyethylene fillers of the same type as in examples 3 to 4, see FIG. 2, having an effective specific surface area of about 800m 2 /m 3 。
Test results and analysis
And (3) testing the nitration activity:
the fillers of examples 1-2, comparative examples 1, examples 3-4, comparative examples 2 and examples 5-7 with the same specification and model are respectively filmed under the condition of low temperature (about 13 ℃), the filling rate of the fillers is 50%, DO is kept to be controlled to be 2-5 mg/L, the initial ammonia nitrogen concentration is 50mg/L, and the nitration activity test result after 20d is shown in Table 1.
And (3) testing the enrichment performance of the anaerobic ammonium oxidation bacteria:
the fillers of examples 1-2 and comparative example 1, examples 3-4 and comparative example 2, and examples 5-7 with the same specification and model are put into an anoxic tank to operate under the condition of AOO pilot test for treating domestic sewage, and the anaerobic ammonium oxidation bacteria in the fillers are detected after 6 months, and the results are shown in Table 1.
TABLE 1 test results of inventive and comparative examples
Through comparative experiments, in the same group of the first group of embodiments and the second group of embodiments, compared with the corresponding common filler with the same specification and model, the suspended filler of the example has obvious advantages in the aspects of nitrification activity and enrichment effect of anaerobic ammonia oxidizing bacteria. The nitration activity of the filler of the same group of examples is more than 3 times of that of the common filler of the comparative example; the filler is more obvious in the aspects of producing and enriching the anaerobic ammonium oxidation bacteria, the common filler of the comparative example has almost no producing and enriching capacity, and the suspended filler of the invention has better biological activity, which is mainly benefited by the selection of the components and the mixture ratio of the filler of the invention. The alkali modified 4A molecular sieve activated powder is used, so that the ammonia nitrogen adsorption performance of the filler is improved; the sulfur powder included by the sulfur-beta-cyclodextrin inclusion compound reduces nitrate nitrogen into nitrite nitrogen under the action of sulfur autotrophic denitrifying bacteria, and the anaerobic ammonia oxidizing bacteria convert the nitrite nitrogen and ammonia nitrogen into nitrogen. The biofilm formation speed of the anaerobic ammonia oxidizing bacteria is improved by the promoting effect of sulfur autotrophic denitrification at the initial biofilm formation. Meanwhile, the metal ions loaded on the filler can promote the metabolism of the anaerobic ammonium oxidation bacteria and improve the enzyme activity of the anaerobic ammonium oxidation bacteria, thereby improving the denitrification effect.
In addition to the combination of the high denitrification components, the high-density polyethylene is adopted as a base material, and the sulfur-beta-cyclodextrin inclusion compound and the polyethylene wax are added into the filler, so that necessary auxiliary support is provided for the filler in the aspects of physical properties, hydrophilicity, processability and the like, and the full and efficient exertion of the denitrification effect is ensured.
Compared with the first group of embodiments and the second group of embodiments, namely from fig. 1 to fig. 2, with the change of the filler configurations of examples 1 and 3 or examples 2 and 4, the effective specific surface area of the corresponding filler is increased, the nitrification activity greatly influenced by the effective specific surface area shows obvious increase, the proportion of the anammox bacteria is kept at a higher level, and the enrichment effect of the anammox bacteria is better; in the same group, the effective specific surface areas of the fillers of the embodiments 2 and 4 with the internal cavities and the foaming porous structures, and the nitrification activity and the enrichment effect of the anaerobic ammonium oxidation bacteria are better than those of the corresponding embodiments 1 and 3, so that the denitrification effect is improved by adopting the mode of foaming by the foaming agent to improve the effective specific surface areas of the fillers.
The examples 5 to 7 of the third group of embodiments significantly increase the effective specific surface area through configuration adjustment, but the nitrification activity and the enrichment effect of anammox bacteria are only slightly improved compared with the examples of the second group of embodiments, mainly because the amount of the alkali-modified 4A molecular sieve activation powder in the components is relatively less, that is, the amount of the ammonia nitrogen adsorbent is less. Therefore, according to the actual application requirement, the proper component content is selected, and the high-efficiency filler configuration is matched, so that the comprehensive mode of obtaining the high denitrification effect is realized.
In addition, in example 7, surface treatment of the filler is added on the basis of example 6, the surface treatment can enhance the surface activity of the filler, and the fast film forming speed of the filler can be observed in the initial stage of the test, but the effect on the overall nitrification activity and the enrichment effect of the anaerobic ammonium oxidation bacteria are not obvious, and the test result is similar to that of example 6.
In conclusion, the active biological suspended filler provided by the invention has rapid enrichment performance of anammox bacteria, excellent comprehensive performances such as suspension and hydrophilicity, can stably realize a better denitrification effect of an anoxic tank, is simple and efficient to process, flexible in configuration selection, strong in environmental adaptability, convenient to popularize and apply, and has great economic value and environmental protection value.
The foregoing describes preferred embodiments of the present invention, and is intended to provide a clear and concise description of the spirit and scope of the invention, and not to limit the same, but to include all modifications, substitutions, and alterations falling within the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The anoxic pond enhanced denitrification suspended filler is characterized in that the suspended filler is an active biological filler and comprises the following raw material components in parts by weight:
the particle sizes of the molecular sieve activation powder, the sulfur-beta-cyclodextrin inclusion compound and the auxiliary materials are all less than 200 meshes;
the raw material components are subjected to melt extrusion molding to obtain the filler with a plurality of cavities inside.
2. The filler according to claim 1, wherein the polyethylene is a high density polyethylene.
3. The filler of claim 1, wherein the auxiliary material comprises stearic acid, polyethylene wax and metal powder, and the metal powder is at least one of ferroferric oxide powder, iron oxide powder, reduced iron powder and manganese carbonate powder.
4. The filler according to any one of claims 1 to 3, wherein the sulphur- β -cyclodextrin inclusion compound is prepared by:
1) Adding 1.5-3 times of water into beta-cyclodextrin, mixing, and grinding to obtain a mixture;
2) Adding carbon disulfide organic solvent dissolved with sulfur powder into the mixture, fully grinding the mixture into paste, and drying the paste at 35-45 ℃;
3) Cleaning redundant sulfur powder with carbon disulfide, and drying again;
4) Crushing the mixture by a jet mill to obtain the sulfur-beta-cyclodextrin inclusion compound.
5. The filler according to claim 4, wherein the molecular sieve activated powder is an alkali-modified 4A molecular sieve activated powder, and is prepared by the following method:
1) Soaking 4A molecular sieve activated powder in distilled water, performing ultrasonic treatment for 1-3h, filtering, and drying at 100-110 deg.C;
2) Soaking the dried 4A molecular sieve activated powder in a NaOH solution with the concentration of 1-2mol/L, heating to 70-90 ℃, and treating for 5-8h;
3) Acting under 500-700W microwave power for 1-3min, and filtering;
4) Repeatedly washing the molecular sieve activated powder with distilled water, and drying at 100-110 ℃ after the filtrate is neutral; and crushing into the alkali modified 4A molecular sieve activation powder.
6. The filler according to claim 5, wherein the filler is a foamed porous filler having an effective specific surface area of more than 1000m 2 /m 3 。
7. The filler according to claim 5 or 6, characterized in that it is surface-treated, including plasma treatment or corona treatment.
8. The preparation method of the anoxic pond enhanced denitrification suspended filler according to any one of claims 1 to 7, characterized by comprising the following steps:
s1: mixing: adding 30-40 parts of polyethylene into a plasticator, and melting at 175 +/-3 ℃; adding 5-10 parts of sulfur-beta-cyclodextrin inclusion compound, mixing for 6-8 minutes, slicing and crushing into a micron-sized particle master batch;
s2: material blending: mixing the master batch, the rest polyethylene, the molecular sieve activated powder and the auxiliary materials by a high-speed mixer to obtain a mixture;
s3: and (3) granulation: extruding and granulating the mixture through a screw extruder;
s4: and (3) extrusion molding: and (4) melting and extruding the granules obtained in the step (S3) through a screw extruder, cooling and shaping, cutting and collecting.
9. The method of claim 8, wherein in step S4, the screw extruder employs five sections for independent temperature control: the temperature of the first section is 145-155 ℃, the temperature of the second section is 160-170 ℃, the temperature of the third section is 165-185 ℃, the temperature of the fourth section is 160-170 ℃, and the temperature of the fifth section is 155-165 ℃; and immediately performing water cooling setting after extrusion.
10. The method according to claim 8 or 9, wherein in step S4, the pellets obtained in step S3 are fed into the screw extruder together with a blowing agent in an amount of 0.1 to 1% by weight based on the polyethylene.
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| CN202211067363.8A CN115477387B (en) | 2022-09-01 | 2022-09-01 | Reinforced denitrification suspension filler for anoxic tank and preparation method thereof |
| PCT/CN2022/131553 WO2024045346A1 (en) | 2022-09-01 | 2022-11-11 | Suspended filler for enhanced denitrification in anoxic tank and preparation method therefor |
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