CN114262237B - Light microporous ceramic filter material and preparation method thereof, and ceramic particles for water treatment and filtration and preparation method thereof - Google Patents
Light microporous ceramic filter material and preparation method thereof, and ceramic particles for water treatment and filtration and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of water filtration, and particularly relates to a lightweight microporous ceramic filter material and a preparation method thereof, wherein the lightweight microporous ceramic filter material comprises the following steps: (1) ball-milling and mixing a ceramic main material, a water reducing agent, agar powder, sodium carboxymethylcellulose, aluminum dihydrogen phosphate, a pore-forming agent, an optional coloring agent and water to obtain a mixture; (2) pouring the mixture, inserting a plurality of wood sticks into the blank obtained after pouring, and then curing and demolding to obtain a formed object; (3) drying the molding object, and then sintering at 950-1050 ℃ to obtain a sintered object; (4) the sinter is cooled and then crushed. Also provides ceramic particles for water treatment and filtration and a preparation method thereof. The material disclosed by the invention is light in specific gravity, high in porosity, large in specific surface area, excellent in compressive strength and shear strength, excellent in higher filtering precision and excellent in technical performance, and has an excellent water treatment effect.
Description
Technical Field
The invention belongs to the technical field of water filtration, and particularly relates to a lightweight microporous ceramic filter material and a preparation method thereof, and ceramic particles for water treatment filtration and a preparation method thereof.
Background
In the field of water treatment filtration, most of quartz sand is used, but the surface is smooth, the interception effect is poor, and meanwhile, the specific gravity of the quartz sand reaches 2.6 g/cm for high speed cultivation, so that the energy consumption of backwashing is high.
The ceramsite is also a filtering material, has light specific gravity but has micropores in the granules, and the surface state is not ideal. The temperature for forming ceramic combination is generally 1450-1620 ℃, the sintering temperature is high, and the method is not suitable for the field of high-precision filtration of water treatment, and the high-temperature sintering is not economical due to the large quantity of the ceramic materials required in the field.
Volcanic rock can also be used as a filter material, and the volcanic rock is porous on the surface, but has a large pore size ratio, and due to the uncontrollable pore size formed naturally, although the specific gravity is lighter than that of quartz sand, generally the specific gravity is 1.6 g/cm for carrying out the cultivation, the space is reduced.
In summary, from the analysis of the comprehensive effect and market demand of the filter material, the art desires to have a formula production process method with a microporous surface, a manually controllable pore size, a light specific gravity and a low sintering temperature.
Besides the requirement of meeting the filtering function, the fish tank also can be preferably provided with optional colors, such as filtering occasions for aquarium appreciation, bottom layer sand filtration of various fish tanks and the like.
Disclosure of Invention
The invention aims to overcome the defects that the filtering performance and the backwashing performance of a filtering material in the prior art need to be further improved, and provides a light microporous ceramic filtering material, a preparation method thereof, ceramic particles for water treatment and filtration and a preparation method thereof.
In order to achieve the above object, in a first aspect, the present invention provides a method for preparing a lightweight microporous ceramic filter material, comprising the steps of:
(1) ball-milling and mixing a ceramic main material, a water reducing agent, agar powder, sodium carboxymethylcellulose, aluminum dihydrogen phosphate, a pore-forming agent, an optional coloring agent and water to obtain a mixture;
(2) pouring the mixture, inserting a plurality of wood sticks into the blank obtained after pouring, and then curing and demolding to obtain a formed object;
(3) drying the molding object, and then sintering at 950-1050 ℃ to obtain a sintered object;
(4) cooling the sinter, and then crushing;
based on the total mass of the raw materials, the agar powder is 1-2wt%, the pore-forming agent is 3-5wt%, the aluminum dihydrogen phosphate is 1-5wt%, preferably 2.5-3.5wt%, the sodium carboxymethylcellulose is 0.02-0.09wt%, the water reducing agent is 1-2wt%, the colorant is 0-6wt%, the water is 12-15wt%, and the balance is a ceramic main material.
Preferably, in the step (1), the ceramic main material comprises alumina powder and/or quartz powder with the particle size of not more than 5 μm, the water reducing agent comprises lignosulfonate, the pore-forming agent comprises wood chip powder with the particle size of not more than 20 μm, and the colorant comprises iron oxide or chromium oxide with the particle size of not more than 5 μm.
Preferably, in step (1), the ball milling and mixing manner comprises: firstly, mixing water, a water reducing agent, agar powder, a sodium carboxymethylcellulose solution and a pore-forming agent for 20-30min, and then introducing an aluminum dihydrogen phosphate solution, a ceramic main material and an optional colorant for grinding for 1.5-2 h.
Preferably, in the step (2), the maximum diameter of the stick is 10-15 mm.
Preferably, the sum of the cross-sectional areas of the plurality of wooden sticks is 10-15% of the cross-sectional area of the blank obtained after pouring.
Preferably, in the step (2), the length of the wooden stick is flush with the thickness of the formed object.
Preferably, in the step (2), the wood stick is round.
Preferably, in the step (3), the drying conditions include: the drying temperature is 120-145 ℃, and the drying time is 1.5-2 h.
Preferably, in the step (3), the sintering time is 1-1.5 h.
In a second aspect, the invention provides a lightweight microporous ceramic filter material, which comprises a ceramic main material, a water reducing agent, agar powder, sodium carboxymethylcellulose, aluminum dihydrogen phosphate and an optional colorant; the surface of the light microporous ceramic filtering material is provided with half holes with various different depths, and the light microporous ceramic filtering material meets the following requirements: specific gravity of 1.1-1.2g/cm, porosity of 40-60%, and specific surface area of 13-20m2G, the compressive strength is 5.5-5.78MPa, and the shear strength is 3.4-3.8 MPa.
Preferably, the particle size of the light microporous ceramic filter material is 0.5-5 mm.
Preferably, the lightweight microporous ceramic filter material is prepared by the preparation method of the first aspect.
In a third aspect, the present invention provides a method for preparing ceramic particles for water treatment filtration, comprising:
the light microporous ceramic filter material prepared by the preparation method of the first aspect or the light microporous ceramic filter material of the second aspect is firstly heated at the temperature of 300-400 ℃, then poured into normal-temperature alkali solution for soaking for surface activation treatment, and finally subjected to normal-temperature natural air drying treatment.
Preferably, the heating time is 0.5-1.5 h.
Preferably, the soaking time is 20-40 min.
Preferably, the mass concentration of the alkali in the alkali solution is 1-2 wt%.
Preferably, the base in the base solution comprises sodium hydroxide.
In a fourth aspect, the invention provides a ceramic particle for water treatment and filtration, which comprises a ceramic main material, a water reducing agent, agar powder, sodium carboxymethyl cellulose, aluminum dihydrogen phosphate and an optional colorant, and alkali,
and the ceramic particles for water treatment filtration satisfy: carrying out high-speed high2G, the compressive strength is 5.5-5.78MPa, and the shear strength is 3.4-3.8 MPa.
Preferably, it is prepared by the method of the third aspect.
The inventor of the invention researches and discovers that in the field of water treatment filter materials, the use strength of particles is considered in consideration of the fact that the porosity is inversely proportional to the strength of the particles, and the filter materials in the prior art generally cannot take into consideration the light specific gravity, the proper and uniform porosity and particle strength, and the economical practicability; this is because the pore distribution in the existing filter materials is not suitable, which directly affects the specific gravity, porosity and strength.
Through the technical scheme, especially aiming at specific raw materials, the method for preparing the light microporous ceramic filter material can reduce linear shrinkage in subsequent drying, promote uniform heating around and in the material, improve sintering uniformity, further improve gap uniformity, prevent a large number of gaps from being locally accumulated, improve compressive strength, avoid adverse effects of nonuniform heating on micropore distribution, avoid possibility of product cracking, promote more and more uniform high-temperature carbonization and ablation in sintering to form holes, facilitate shortening of sintering time, carry out specific crushing after cooling, enable the surface of the obtained light microporous ceramic filter material to have different uneven and different-depth half holes, and enable the external specific surface area to be far larger than the internal specific surface area, as shown in figure 2, the microporous structure can obviously improve the water filtration performance, has light specific gravity, high microporous porosity, large specific surface area, excellent compressive strength and shear strength, is used in ceramic particles for water treatment and filtration, has higher filtration precision and excellent water treatment effect. Wherein, carry out the breakage after the sinter cooling, can make the product surface have the half-hole of the different degree of depth, improve outer specific surface area, and then improve filtering quality. The raw materials can reduce the sintering temperature under the condition of only adopting proper amount of aluminum dihydrogen phosphate as a high-temperature adhesive, can save energy consumption on the basis of ensuring performance indexes such as porosity, strength and the like, and obviously reduces the manufacturing cost in large-scale production.
According to the preparation method of the ceramic particles for water treatment and filtration, provided by the invention, due to the adoption of proper heating, micropores can be expanded, surface gaps can be slightly enlarged, a surface activity accommodating space is provided for subsequent normal-temperature alkali, a part of alkali is reserved in the air-dried particles, an alkaline point is formed, and the surface potential of the particles is changed, so that the surfaces of the prepared ceramic particles for water treatment and filtration have hydrophilic and oil-repellent properties, and the ceramic particles are not only suitable for filtering water and industrial sewage, but also suitable for filtering oily sewage, are not adhered to filtered dirt, and are easy to desorb through backwashing.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is an electron micrograph of a lightweight microporous ceramic filter material according to the present invention.
Fig. 2 is a schematic view of the crushing situation of the present invention.
FIG. 3 is a schematic view of the ceramic particle filter for water treatment according to the present invention.
Fig. 4 is a schematic structural view of the insertion stick according to example 1 of the present invention.
FIG. 5 is a picture of water at each stage of water inlet-outlet-back flushing in example 1 of the present invention.
FIG. 6 is a graph showing the amount of wood flour used in example 1 as a function of the porosity of the resulting ceramic particles.
FIG. 7 is a graph of the amount of iron oxide introduced in example 1 versus the color of the resulting ceramic particles.
FIG. 8 is a graph of the amount of chromium oxide incorporated in example 1 versus the color of the resulting ceramic particles.
Description of the reference numerals
1-hole, 2-half hole, 3-stick and 4-square billet.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In the invention, the particle strength refers to compressive strength and shear strength, the compressive strength can ensure that the filter material is not crushed at the filling height, and the shear strength can ensure that the filter material is not crushed or is resistant to abrasion in the back washing friction.
Generally, compressive strength is related to porosity, with higher porosity and more pores leading to lower compressive strength and uniformity of voids.
In view of the above, in a first aspect, the present invention provides a method for preparing a lightweight microporous ceramic filter material, comprising the steps of:
(1) ball-milling and mixing a ceramic main material, a water reducing agent, agar powder, sodium carboxymethylcellulose, aluminum dihydrogen phosphate, a pore-forming agent, an optional coloring agent and water to obtain a mixture;
(2) pouring the mixture, inserting a plurality of wood rods 3 into the blank obtained after pouring, and then curing and demolding to obtain a formed object;
(3) drying the molding object, and then sintering at 950-1050 ℃ to obtain a sintered object;
(4) the sinter is cooled and then crushed.
In the step (1), by total mass of the raw materials, the agar powder accounts for 1-2wt%, the pore-forming agent accounts for 3-5wt%, the aluminum dihydrogen phosphate accounts for 1-5wt%, the sodium carboxymethylcellulose accounts for 0.02-0.09wt%, the water reducing agent accounts for 1-2wt%, the coloring agent accounts for 0-6wt%, the water accounts for 12-15wt%, and the balance is a ceramic main material.
According to the preparation method provided by the invention, the raw materials with specific compositions are treated in each step, particularly the steps (2) to (4) are matched, and the wood stick 3 is inserted, so that the sintering uniformity can be improved, the gap uniformity is further improved, a large number of gaps can be prevented from being accumulated locally, the compressive strength is good, and the product is prevented from cracking; meanwhile, the raw material system is sintered at the temperature of 950-1050 ℃, so that the combination of ceramic properties is achieved, the raw materials are fused and bonded with each other to form a whole, and the shear strength is improved; namely, the obtained light microporous ceramic filter material has high porosity, high strength and light specific gravity; after subsequent crushing, the semi-holes 2 with different depths on the surface are formed, so that the filtering performance and the filtering precision are improved.
In the present invention, the half-hole 2 refers to the incomplete holes with different sizes obtained by crushing the whole hole 1 to different degrees, and the radius or depth thereof may be uniform or non-uniform, as shown in fig. 2, including but not limited to the half-hole obtained by crushing half of the whole hole 1, for example, the half-hole obtained by crushing 1/4 of the hole 1.
In the scheme, the alumina powder and/or quartz powder are used as ceramic main materials, the water reducing agent is used for reducing the water content of the blank, the agar powder is used for keeping the blank to be shaped, the sodium carboxymethylcellulose is used for avoiding the layering of various powder materials of the blank, the aluminum dihydrogen phosphate is used as a high-temperature adhesive, the water reducing agent and water are used, the sintering temperature is low under the condition that other raw materials are not needed, and the obtained filter material has the effects of proper light specific gravity, proper distribution of a microporous structure, high strength and good water filtering performance.
Specifically, regarding the agar powder, the agar powder has the shaping effect of wet demoulding, and the collapse after demoulding is avoided, the addition amount of 1wt% of 200 x 100 x 50mm of the standard brick is better, the addition amount of 2wt% of 300 x 200 x 100mm of the standard brick is better, the standard brick is difficult to place in a large sintering device and is difficult to burn through, the agar powder is too little and does not work, and the content of the ceramic main material is influenced too much.
Regarding the pore-forming agent, the product of the invention is used for filtration, so that the porosity and the necessary strength are considered to meet the requirement of back washing mechanical scouring, the porosity is better from the viewpoint of interception filtration, the porosity is better from the viewpoint of meeting the requirement of back washing mechanical scouring strength, and the two factors are considered together, so that the pore-forming agent has the porosity of 40-60% corresponding to the final product at 3-5 wt%.
Regarding aluminum dihydrogen phosphate, aluminum dihydrogen phosphate is a high-temperature adhesive which is matched with other raw materials and melted at the temperature of 950-. In the traditional ceramic sintering, two materials are connected together after being melted in the sintering process, which is called ceramic connection, typically an alumina system and a silica system, and different proportions form different material characteristics, and the sintering porcelain forming temperature of the materials is generally more than 1650 ℃. Preferably, the amount of aluminium dihydrogen phosphate is 1 to 3.5 wt.%, for example 1 wt.%, 1.5 wt.%, 2 wt.%, 3 wt.%, 3.5 wt.% and any value between adjacent values, more preferably 2.5 to 3.5 wt.%. Under this preferred scheme, more do benefit to and make the compressive strength and the shear strength who improves the product, improved the tolerance level of back flush, and have specific surface area and porosity and filter fineness concurrently, the back flush energy consumption is lower, and multiple performance index and economic nature are more excellent.
The proper addition amount of the sodium carboxymethyl cellulose can avoid layering in the formula system of the invention, the effect is limited when the addition amount is too small, and the sodium carboxymethyl cellulose is easy to collapse when the addition amount is too large for shaping and demoulding.
As for the water reducing agent, the formula system of the invention adopts water as a dispersing agent, the grinding is carried out in a ball mill, and according to the analysis of the requirement of casting and forming after grinding, the smaller the water amount is, the better the water amount is, so as to improve the quality of the finished product, particularly the compactness, but the too small water amount causes the grinding difficulty, the research proves that the adding of 1-2wt% of the water reducing agent can reduce the water adding amount by 5-10wt% in proportion, the normal grinding is still kept, the effect is not obvious when the adding amount is too small, the effect of adding the water reducing agent excessively is limited, and the optimal value is 1-2wt%, such as any value of 1wt%, 1.5wt%, 1.8wt% and 2wt% and any value between adjacent values from the economical and practical angles.
The color of the finished product obtained by the invention is white when no colorant is added, and on the basis, if a proper colorant is added, the finished product can be a colored product. The skilled person can select a colorant according to colour requirements, preferably the colorant comprises iron oxide or chromium oxide having a particle size of no more than 5 μm. It is to be understood that "iron oxide or chromium oxide having a particle size of not more than 5 μm" means iron oxide having a particle size of not more than 5 μm or chromium oxide having a particle size of not more than 5 μm. Wherein, proper amount of ferric oxide can be added to obtain red color, and proper amount of chromium oxide can be added to obtain green color.
Preferably, the sodium carboxymethyl cellulose is introduced in the form of a solution, the solid content of which is 2-3 wt%; the aluminum dihydrogen phosphate is introduced in the form of a solution, and the solid content of the aluminum dihydrogen phosphate is 25-35 wt%.
Preferably, in the step (1), the ceramic main material comprises alumina powder and/or quartz powder with the particle size not greater than 5 μm. It is to be understood that "alumina powder and/or quartz powder having a particle size of not more than 5 μm" means alumina powder having a particle size of not more than 5 μm and/or quartz powder having a particle size of not more than 5 μm. Preferably, the alumina powder can be industrial alumina powder, wherein the content of alumina is more than or equal to 99%. Preferably, the quartz content in the quartz powder is more than or equal to 99%.
The skilled in the art can select the types of the water reducing agent and the pore-forming agent according to the requirements.
Preferably, the water reducing agent comprises lignosulfonate. The lignosulfonate may be a commercially available product or may be prepared by a conventional method.
Preferably, the pore-forming agent comprises wood dust with a particle size of not more than 20 μm.
According to the present invention, preferably, in step (1), the ball milling and mixing manner includes: firstly, mixing water, a water reducing agent, agar powder, a sodium carboxymethylcellulose solution and a pore-forming agent for preferably 20-30min, and then introducing an aluminum dihydrogen phosphate solution, a ceramic main material and an optional colorant for grinding for preferably 1.5-2 h.
Preferably, in step (2), a person skilled in the art can select a material and a shape of the forming mold according to requirements, for example, a carbon steel mold tool filled with a lining stainless steel plate is used for forming, the carbon steel mold tool is generally brick-shaped, the thickness of the carbon steel is 2-3mm, the smooth stainless steel plate is used as a lining, the thickness of the smooth stainless steel plate is 0.5mm, and machine oil can be smeared before pouring to facilitate demolding. It will be appreciated that the shape of the blank is adapted to the casting mould.
Preferably, in the step (2), the maximum diameter of the stick 3 is 10-15 mm. It will be appreciated that when the wooden stick 3 is in a regular pattern, such as a circle, the maximum diameter of the wooden stick 3 is the diameter of the circular wooden stick 3.
Preferably, the sum of the cross-sectional areas of the several sticks 3 is 10-15% of the cross-sectional area of the blank obtained after casting. Under this preferred scheme, more do benefit to and promote follow-up stoving and sintering even, more do benefit to the comprehensive effect of promoting micropore distribution and product intensity.
It is understood that the blank obtained after casting refers to the blank after casting and before inserting the wood stick 3.
Preferably, in the step (2), the length of the wooden stick 3 is flush with the thickness of the formed object. The thickness of the formed object is the thickness of the formed object in the direction perpendicular to the surface of the pouring opening.
The shape of the stick 3 can be chosen by the person skilled in the art according to the sintering uniformity and economy. Preferably, in the step (2), the wooden stick 3 is circular.
Preferably, in the step (3), the drying conditions include: the drying temperature is 120-145 ℃, and the drying time is 1.5-2 h.
In the present invention, the sintering is performed in a positive pressure oxidizing atmosphere.
Preferably, in the step (3), the sintering time is 1-1.5 h.
Preferably, the sintering mode is a step-by-step temperature-rise sintering, and specifically includes: heating to 500 ℃ at the rate of 90-110 ℃/h, heating to 500-1000 ℃ at the rate of 160 ℃/h at 140-1.2 h, and cooling at the rate of 210 ℃/h at 190-210 ℃ after heat preservation for 0.8-1.2 h. Under this preferred scheme, slow programming rate more is favorable to making the adobe inside and outside to be heated evenly, and in the gradual intensification process, wood rod 3 carbonizes the ablation gradually and forms the hole, makes the product that makes like this heat simultaneously all around and inside to more be favorable to promoting suitable micropore distribution, promotion intensity, avoid the possibility of fracture simultaneously.
The cooling manner in step (4) can be selected by those skilled in the art according to the requirement, and the present invention is not limited thereto.
The crushing in the step (4) of the invention enables the particle size of the single particles to be 0.5-5 mm. In the present invention, the particle size of the single particle refers to the equivalent particle size of the single particle. It is understood that the particle size of each of the crushed grains satisfies the above range. The average particle diameter can also be obtained based on the particle diameter of each crushed particle.
According to the invention, as shown in the leftmost side of the figure 2, the sintered object in the step (4) is sintered and cooled, the pore diameters of the gaps in the material are uniformly distributed, and after the sintered object is crushed, the crushed sintered object is cracked along the black line in the middle figure of the figure 2, so that the light microporous ceramic filter material with uneven pore diameter distribution as shown in the rightmost side of the figure 2 is formed, the surface of the light microporous ceramic filter material mainly comprises half-pores 2 with various different depths, the whole pores 1 are arranged in the light microporous ceramic filter material, the outer specific surface area is far larger than the inner specific surface area, uneven-surface particles are formed, the half-pores 2 with various different depths are more beneficial to filtration, the whole pores 1 in the light microporous ceramic filter material do not contribute to the filtration effect basically, only play a role in reducing the specific gravity, and the material has excellent water filtration performance due to the special pore distribution.
In the invention, the internal specific surface area of the product before crushing is far larger than the external specific surface area because the inside is fully distributed with gaps, and the external specific surface area of the crushed particles is far larger than the internal specific surface area because the particles are very small, the internal gaps are gradually converted into the external gaps and are converted into the uneven surface, and the specific surface area of the product is tens of times of that of the internal gaps.
The crushed particles obtained by crushing the invention are a plurality of, and are piled together to form a filter layer during water flow filtration, as shown in figure 3, for example, the height is more than 3 m. During filtering, the rugged surface forms a bent and curved flow channel, when water flow shown by arrows in figure 3 passes through the flow channels, the flow velocity in each horizontal section is microscopically different, the flow velocity is changed due to the width change of the flow channel, impurities in the water are pushed to continuously move transversely by the change, the flow velocity at the center of the flow channel is high, the surface flow velocity of the rugged half-hole 2 is close to zero, large impurities are directly intercepted, namely mechanical obstruction, the medium impurities are organically retained on the inner surface of the half-hole 2, namely adsorption, the internal specific surface area of the adsorbed impurities is further increased, and the smaller impurities can be adsorbed, and in the same way, the filtration is called as slag filtration residue; thereby making the filtering performance excellent.
In a second aspect, the invention provides a lightweight microporous ceramic filter material, which comprises a ceramic main material, a water reducing agent, agar powder, sodium carboxymethylcellulose, aluminum dihydrogen phosphate and an optional colorant; the light microporous ceramic filter materialHas half-holes 2 of various different depths, and the lightweight microporous ceramic filter material satisfies: performing high-density nucleic acid amplification at a specific gravity of 1.1-1.2g/cm, porosity of 40-60%, and specific surface area of 13-20m2G, the compressive strength is 5.5-5.78MPa, and the shear strength is 3.4-3.8 MPa.
Wherein, the specific gravity is light, the backwashing energy consumption is reduced, the porosity is high, the scale capacity is improved, the specific surface area is large, the adsorption capacity is improved, the compression strength provides guarantee for the height of the filter layer, and the shearing strength is high, so that the damage is reduced by backwashing. The light microporous ceramic filter material has the advantages of light specific gravity, high dirt capacity, large specific surface area, high compressive strength and high shear strength, so that the filter performance is excellent.
The surface of the light microporous ceramic filter material is provided with half holes with various different depths, uneven bent flow channels are formed on the surface, the filtering performance is excellent, the flow velocity of water flow shown by arrows in figure 3 is microscopically different in each horizontal section when the water flow passes through the flow channels during filtering, the flow velocity is changed due to the change of the width of the flow channels, impurities in water are pushed to continuously move transversely by the change, the flow velocity at the center of the flow channels is high, the flow velocity on the surfaces of the uneven half holes is close to zero, large impurities are directly intercepted and called mechanical blockage, the medium impurities are organically retained on the inner surfaces of the half holes and called adsorption, the adsorption impurities further increase the inner specific surface area, and the smaller impurities can be adsorbed, and the rest is called slag filtration. The invention can also prepare white or yellow or green or red colored products by introducing the colorant, and is suitable for the field of ornamental filtration.
Preferably, the particle size of the light microporous ceramic filter material is 0.5-5 mm. It will be appreciated that in an actual filter vessel, the filter media may be filled to a range of sizes including all sizes in the range of 0.5-5mm, or a range of sizes, such as 1-3 mm, depending on the water treatment specifications.
In some embodiments, the lightweight microporous ceramic filter material is prepared by the preparation method of the first aspect. The content of each component in the light microporous ceramic filter material corresponds to the respective addition amount.
The light microporous ceramic filter material provided by the invention has high filtering precision. On one hand, the filtration precision is improved, and on the other hand, the material is required to reach proper high porosity and strength, because only enough gaps exist, the surface of the final material particle can be uneven as much as possible, and more opportunities for contact adsorption with water flow are created, and the material disclosed by the invention has proper high porosity and strength; on the other hand, in connection with the material particles, the smaller the particles, the higher the bulk density, the higher the filtration accuracy, and the particles of the present invention are generally in the range of 0.5 to 5mm in diameter, so that the filtration accuracy of the material of the present invention can be brought to the ultrafiltration accuracy range, for example, 0.1 μm. The skilled person can also choose the height of the stack of material particles on the basis of this, the higher the filter layer stack the higher the filtration accuracy.
In a third aspect, the present invention provides a method for preparing ceramic particles for water treatment filtration, comprising: the light microporous ceramic filter material prepared by the preparation method of the first aspect or the light microporous ceramic filter material of the second aspect is firstly heated at the temperature of 300-400 ℃, then poured into normal-temperature alkali solution for soaking for surface activation treatment, and finally subjected to normal-temperature natural air drying treatment.
In the process of pouring the normal-temperature alkali solution, alkali rapidly and more enters the expanded micropores of the heated light microporous ceramic filter material, then normal-temperature natural air drying treatment is carried out to ensure that most of the alkali entering the micropores is remained in the micropores, the normal-temperature natural air drying enables the gaps to be reduced and locked in the material, so that the surface potential of the ceramic particles moves to negative potential, the negative potential is repelled, the oil-repellent characteristic is macroscopically played, namely the oil-repellent characteristic is not easy to form substantial adhesion with oil stains in sewage, and the oil-repellent characteristic is easy to desorb through backwashing; if the solution is directly poured into the normal-temperature alkali solution without being heated at the temperature of 300-400 ℃, more alkali is left on the surface of the material, and the small pores are difficult to contain enough alkali and change the potential. However, the oil content of general sewage is negative potential, and the material particles without activation treatment are neutral potential, so that the effect of changing potential is difficult to achieve.
The heated material is preferably poured into the normal-temperature alkali solution quickly.
Preferably, the heating time is 0.5-1.5 h.
Preferably, the soaking time is 20-40 min.
The temperature of the soaking can be selected by a person skilled in the art according to requirements, and can be normal temperature, or can be heated to a certain temperature, as long as alkali can better enter the heated and expanded micropores.
Preferably, the mass concentration of the alkali in the alkali solution is 1-2 wt%.
In the preferable scheme, the higher the alkali concentration is, the better the potential changing effect is, but the higher the economic cost is, and the process parameters of the invention can not only achieve that the ceramic particles and the oil stains do not form substantial adhesion in the sewage treatment process, but also give consideration to the economy.
The kind of base can be selected by those skilled in the art according to the need. Preferably, the alkali in the alkali solution comprises sodium hydroxide and potassium hydroxide.
In a fourth aspect, the present invention provides a ceramic particle for water treatment filtration, which comprises a ceramic main material, a water reducing agent, agar powder, sodium carboxymethyl cellulose, aluminum dihydrogen phosphate, an optional colorant, and an alkali, wherein the ceramic particle for water treatment filtration satisfies the following requirements: carrying out high-speed high2G, the compressive strength is 5.5-5.78MPa, and the shear strength is 3.4-3.8 MPa.
Wherein 0.1 μm in filtration precision is the ultrafiltration precision range. The product of the invention has high filtration precision and is adjustable, and the specific adjustment mode can be realized by controlling the porosity and adjusting the height of the filter layer, the particle size, the working pressure, the flow rate and other technical measures.
The content of alkali in the ceramic particles is a trace amount and can be adjusted according to the addition amount.
The amount added during the preparation can be selected by the person skilled in the art according to the content of the base and other factors, which can be determined, for example, according to technical requirements and taking into account cost factors.
Preferably, it is prepared by the method of the third aspect. The content of each component contained in the ceramic particles for water treatment and filtration corresponds to the respective addition amount.
The grain diameter, the pore distribution and the strength of the ceramic particles for water treatment and filtration are basically the same as the corresponding performances of the light microporous ceramic filter material. Before and after the heating, surface activation treatment and normal-temperature natural air drying treatment, the change of the potential of the material is greatly influenced, and the material pore distribution and the strength change are not large.
The ceramic particles for water treatment and filtration can be suitable for water treatment in various scenes, including filtration treatment of alkaline wastewater, acidic wastewater, aquarium bottom filter layers and the like, and are particularly suitable for water supply treatment and advanced sewage treatment. Wherein, the advanced sewage treatment is to arrange a filter device on a terminal device of the sewage treatment process, and the filter device is filled with the ceramic particles.
The filtering precision of the ceramic particles can be adjusted, and the ceramic particles can be realized by adjusting the technical measures of the height of a filtering layer, the size of the particle size, the working pressure, the flow velocity and the like.
The invention is further illustrated by the following detailed examples.
Example 1
The raw materials comprise the following components in percentage by mass: 2% of agar powder, 3% of sawdust powder, 3% of aluminum dihydrogen phosphate solution, 1.5% of sodium carboxymethyl cellulose solution, 1% of water reducing agent, 15% of water and the balance of quartz powder. The particle size of the quartz powder is less than 5 micrometers, the content of the quartz powder is more than or equal to 99%, the particle size of the wood dust powder is less than 20 micrometers, the solid content of the aluminum dihydrogen phosphate solution is 30%, the solid content of the sodium carboxymethylcellulose solution is 2%, and the water reducing agent is a lignosulfonate commercial product.
Firstly, mixing water, a water reducing agent, agar powder, a sodium carboxymethylcellulose solution and wood dust powder for 25min, then introducing an aluminum dihydrogen phosphate solution and quartz powder for grinding for 1.5h, and pouring and molding after grinding.
The grinding tool for casting molding is a square brick type and is made of a carbon steel and stainless steel composite steel plate, the thickness of carbon steel is 2-3mm, the smooth stainless steel plate is used as an inner lining, the thickness of the carbon steel is 0.5mm, engine oil is smeared before casting to facilitate demoulding, a plurality of round wood sticks 3 prepared in advance are uniformly inserted into a square billet 4 after casting, as shown in figure 4, the length of the grinding tool is equal to the depth (namely the thickness) of the grinding tool, and the diameter of the grinding tool is 12 mm. The sum of the cross-sectional areas of the wood rods 3 is 12% of the cross-sectional area of the blank obtained after pouring.
After curing and demoulding, the mixture is dried for 1.5 hours at the temperature of 135 ℃.
Sintering for 1 hour at 950 ℃, and gradually carbonizing and ablating the round wood rod 3 to form holes in the gradual heating process, so that the obtained microporous brick product is simultaneously heated around and inside, the sintering uniformity is improved, the uniformity and the strength of the holes are improved, and the possibility of cracking caused by nonuniform heating is avoided.
Cooling the product, and crushing the cooled microporous brick to form particles with the particle size of 0.5-5 mm. Thus obtaining the light microporous ceramic filter material with a certain porosity, wherein the porosity is 40%. The granules obtained from the above formulation were white.
Then heating the particles at 350 ℃ for 1h to expand micropores of the particles, then quickly pouring the particles into a sodium hydroxide solution with the concentration of 2wt% in a normal temperature state for soaking for 30 minutes, and finally carrying out normal-temperature natural air drying treatment. The treated ceramic particles for water treatment and filtration have the characteristics of hydrophilicity and oil repellency, and the application range of the product is expanded.
The electron microscope picture of the ceramic particles for water treatment filtration is shown in figure 1, and satisfies the following conditions: average particle diameter of 3mm, filtration precision of 1 μm, specific gravity of 1.2g/cm, porosity of 40%, and specific surface area of 15m2(iv) g, compressive strength of 5.6MPa, shear strength of 3.6 MPa.
Example 2
The process is carried out as in example 1, except that the amount of wood flour is different, specifically 4% and 5% are added, the other components and their amounts are the same as in example 1, and the quartz flour is made up to 100%.
The porosity of the resulting ceramic particles is shown in fig. 6.
At 4% of wood flourIn the powder dosage scheme, the ceramic particles meet the following requirements: average particle diameter of 3mm, filtration precision of 1 μm, specific gravity of 1.15g/cm, porosity of 50%, and specific surface area of 22m2(iv)/g, compressive strength of 5MPa, shear strength of 3.5 MPa.
In the 5% wood dust dosage scheme, the ceramic particles meet the following requirements: grain diameter of 3mm, filtration precision of 1 μm, specific gravity of 1.1g/cm, porosity of 60%, and specific surface area of 24m2(iv) g, compressive strength of 4.5MPa, shear strength of 3 MPa.
Example 3
The procedure is followed as in example 1, except that the colorants iron oxide (commercial iron oxide powder with a particle size < 5 μm) or chromium oxide are also introduced, as shown in FIGS. 7 and 8, respectively, the other components and their amounts are the same as in example 1, and the quartz powder makes up to 100%.
The obtained ceramic particles are products with the colors shown in figure 7 or figure 8, and other performance parameters are unchanged.
Example 4
The procedure of example 1 was followed except that aluminum dihydrogen phosphate was increased to 5% by weight, the other components and the amounts thereof were the same as in example 1, and the quartz powder made up to 100%.
The ceramic particles satisfy: porosity of 20%, average particle diameter of 3mm, filtration precision of 2 μm, specific gravity of 1.3g/cm, and specific surface area of 12m2(iv) g, compressive strength of 6MPa, shear strength of 3.5 MPa.
As can be seen by comparison, in this example, when the aluminum dihydrogen phosphate is increased to 5wt%, although the compressive strength is increased and the shear strength is similar to that of example 1, and the durability of the backwashing is improved, the specific surface area and the porosity are reduced, so that the filtration precision is reduced during the water treatment process, and the specific gravity is increased, which means that greater backwashing energy consumption is required, so that example 4 is not better than example 1 in consideration of multiple performance indexes and economy.
Comparative example 1
The procedure of example 1 was followed except that the wooden stick 3 was not inserted but directly cured and molded after casting.
In the comparative example, the time from sintering to porcelain formation is prolonged by 0.5h compared with that in example 1, the energy consumption is increased, the sintered blank has irregular cracks, and the pores are not uniformly distributed from outside to inside along the cracks, so that the porosity of the crushed particles is not uniform, the compressive strength and the shear strength are not uniform, the particles with low strength can be further broken into powder, and the normal filtration is influenced.
Comparative example 2
The procedure of example 1 was followed except that the temperature of heating before the activation of the granules was lowered to 150 ℃ and a normal temperature sodium hydroxide solution was added thereto and the granules were soaked for 30 minutes, and the same procedure as in example 1 was repeated.
The oil-repellent effect of the final pellets was reduced by 50% in the treatment of oily sewage as compared with example 1, which indicates that the activation effect is reduced by a low heating temperature.
Comparative example 3
The procedure was followed as in example 1, except that the amount of aluminum dihydrogen phosphate was reduced to 1% by weight, the other components and the amounts thereof were the same as in example 1, and the quartz powder made up to 100%.
The ceramic particles satisfy: porosity of 65%, average particle diameter of 3mm, filtration precision of 1 μm, specific gravity of 1.1g/cm, and specific surface area of 22m2(g), the compressive strength is 4.5MPa, and the shear strength is 2.8 MPa.
By comparison it can be seen that: in the comparative example, when the content of aluminum dihydrogen phosphate is reduced to 1wt%, although the cost can be reduced and the porosity and the specific surface area can be improved as compared with example 1, the compressive strength and the shear strength are both reduced, and the anti-washing tolerance is reduced by analyzing from the water treatment use angle, and the filter material particles are easy to further break into powder, so that the filtering value is lost, and the practicability is poor.
Test example 1
Taking the ceramic particles obtained in the above example 1 as an example, a sewage advanced treatment test was performed. The advanced sewage treatment is that the terminal equipment of the sewage treatment process is provided with filtering equipment, and the filtering equipment is filled with ceramic particles. The water outlet index of the ultrafiltration membrane can achieve the same water production effect of the ultrafiltration membrane. The results of the test indexes of example 1 are specifically shown in table 1 below, and the graphs of the influent water, the filtered effluent water, and the backwash water of the filtering apparatus of example 1 are shown in fig. 5.
TABLE 1
| Index (I) | Inflow (mg/L) | Water outlet (mg/L) | Average removal rate over a year% |
| COD | 27.71 | 19.62 | 29.20 |
| SS | 8.1 | 1.67 | 79.38 |
| Ammonia nitrogen | 1.17 | 0.54 | 53.85 |
| Total nitrogen | 7.28 | 5.79 | 20.47 |
| Total phosphorus | 0.13 | 0.078 | 40.0 |
| Turbidity of water | 8 NTU | 0.35 NTU | 95.6 |
Note: the water inlet refers to sewage before entering the filtering equipment filled with ceramic particles; the effluent is water filtered by a filter device filled with ceramic particles; the average removal rate over one year means an average value of removal rates per filtration in one year of filtration by the filtration apparatus, the removal rate = (water inlet value-water outlet value of corresponding item)/water inlet value.
As can be seen from fig. 5 and table 1, the ceramic particles of example 1 of the present invention have good filtration effect, and can achieve the same water production filtration effect as the ultrafiltration membrane; the ceramic particles obtained in the example 1 are filled in a microfiltration tank, the designed flow rate is 100 cubes per hour, the flow rate can reach 100 cubes after each backwashing, and the flow rate is not attenuated after 6 years, which shows that the backwashing performance is good.
The ceramic particles of other embodiments have a filtering function similar to that of embodiment 1, and can also have an ornamental function, and are suitable for an aquarium or a fish tank as a bottom filtering layer.
Test example 2
Taking the ceramic particles prepared in example 1 as an example, the ceramic particles were compared with the conventional ultrafiltration membrane process, and the results are shown in table 2 below. Wherein, the microfiltration process of the filter material filled with the ceramic particles comprises the following steps: the method comprises the steps of inflow water, biochemistry, precipitation, ceramic particle filtration and water discharge. The traditional ultrafiltration membrane process comprises the following steps: the method comprises the steps of inflow water, biochemistry, precipitation, membrane pretreatment, ultrafiltration membrane and water discharge.
TABLE 2
| Contrasting content | Ultrafiltration membrane process | Ceramic particle microfiltration | Remarks for note |
| Equipment factory building | Need to make sure that | Does not need to use | / |
| Heating plant | Need to make sure that | Does not need to use | The micro-filtration tank and the pipeline adopt heat preservation and heat tracing band |
| Filtration before membrane | Need to make sure that | Does not need to use | General ultrafiltration requires prefiltration |
| Yielding water SS | 1—2mg/L | 1—5mg/L | The microfiltration can adjust the precision to achieve the best cost performance |
| Accuracy of water discharge | Is not adjustable | Is adjustable | Can be adjusted to reduce the operating cost |
| Chemical cleaning | Need to make sure that | Does not need to use | / |
| Off-line cleaning | Need to make sure that | Does not need to use | / |
| Flow attenuation | 10-15%/year | Does not attenuate | Can maintain the designed flow |
| Filter material replacement | About 5 years | Effective life of 20 years | Pre-installation of 5 years natural loss |
| Used in the open air | Generally do not suggest | Can be used for | / |
| Influent SS | ≤10mg/L | ≤20mg/L | The microfiltration time can be higher |
As can be seen from the above table 2, compared with the conventional ultrafiltration membrane process, the ceramic particles of the present invention do not require a specific plant or a plant for heating when being filtered, have wide applicability, and can be used in any scene requiring water filtration; the pre-membrane filtration is not needed, the sewage can be directly filtered, and the filtering range is wide; and the effluent SS and the precision can be adjusted, the flow can be recovered after backwashing, the flow is not attenuated, and the service life is long. The surface of the ultrafiltration membrane is filtered, and the surface of the ultrafiltration membrane is easy to block because the ultrafiltration membrane is intercepted by a thin membrane, while the surface of the ceramic particle microfiltration membrane is intercepted by micropores (including half pores) on the surface, and the filtered layer is up to 3 meters and has more dirt containing space than the ultrafiltration membrane, and the filtered layer can be dispersed during backwashing, so the ultrafiltration membrane is not easy to block and can be applied for a long time.
The ceramic particles of the present invention have wide application in the field of water treatment and filtration, and can be filled into a closed steel tank, called a micro-filtration tank, and can be used for filtering and reusing circulating water, oily sewage, slag flushing wastewater of steel plants, oilfield reinjection water and various cleaning solutions in the industrial field, and can be filled into an open filter tank, called a micro-filter tank, and can be used for treating sewage in large-flow water plants and cities and towns.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (17)
1. The preparation method of the lightweight microporous ceramic filter material is characterized by comprising the following steps:
(1) ball-milling and mixing a ceramic main material, a water reducing agent, agar powder, sodium carboxymethylcellulose, aluminum dihydrogen phosphate, a pore-forming agent and water to obtain a mixture;
(2) pouring the mixture, inserting a plurality of wood sticks into the blank obtained after pouring, and then curing and demolding to obtain a formed object; the sum of the cross sectional areas of the plurality of wood rods is 10-15% of the cross sectional area of the blank obtained after pouring;
(3) drying the molding object, and then sintering at 950-1050 ℃ to obtain a sintered object;
(4) cooling the sinter, and then crushing;
based on the total mass of the raw materials, the agar powder accounts for 1-2wt%, the pore-forming agent accounts for 3-5wt%, the aluminum dihydrogen phosphate accounts for 1.5-5wt%, the sodium carboxymethylcellulose accounts for 0.02-0.09wt%, the water reducing agent accounts for 1-2wt%, the water accounts for 12-15wt%, and the balance is a ceramic main material.
2. The method according to claim 1, wherein the aluminum dihydrogen phosphate is used in an amount of 1.5 to 3.5 wt%.
3. The method according to claim 1, wherein in the step (1), a coloring agent is further added, and the coloring agent is used in an amount of 0 to 6wt% based on the total mass of the raw materials, and the coloring agent comprises iron oxide or chromium oxide having a particle size of not more than 5 μm.
4. The production method according to claim 1, wherein, in the step (1),
the ceramic main material comprises alumina powder and/or quartz powder with the particle size not more than 5 mu m, the water reducing agent comprises lignosulfonate, and the pore-forming agent comprises wood chip powder with the particle size not more than 20 mu m;
and/or, the ball milling and mixing mode comprises the following steps: firstly, mixing water, a water reducing agent, agar powder, a sodium carboxymethylcellulose solution and a pore-forming agent for 20-30min, and then introducing an aluminum dihydrogen phosphate solution and a ceramic main material for grinding for 1.5-2 h.
5. The preparation method according to claim 4, wherein in the step (1), the ball milling and mixing manner comprises: firstly, mixing water, a water reducing agent, agar powder, a sodium carboxymethylcellulose solution and a pore-forming agent for 20-30min, and then introducing an aluminum dihydrogen phosphate solution, a ceramic main material and a colorant for grinding for 1.5-2 h.
6. The production method according to claim 1, wherein in the step (2),
the maximum diameter of the wooden stick is 10-15 mm;
and/or the length of the wooden stick is flush with the thickness of the molded object;
and/or the wood stick is round.
7. The production method according to claim 1, wherein, in the step (3),
the drying conditions include: the drying temperature is 120-145 ℃, and the drying time is 1.5-2 h;
and/or the sintering time is 1-1.5 h.
8. A light microporous ceramic filter material is characterized by comprising a ceramic main material, a water reducing agent, agar powder, sodium carboxymethylcellulose and aluminum dihydrogen phosphate;
the surface of the light microporous ceramic filtering material is provided with half holes with various different depths, and the light microporous ceramic filtering material meets the following requirements: performing high-density nucleic acid amplification at a specific gravity of 1.1-1.2g/cm, porosity of 40-60%, and specific surface area of 13-20m2G, the compressive strength is 5.5-5.78MPa, and the shear strength is 3.4-3.8 MPa.
9. The lightweight microporous ceramic filter material of claim 8, further comprising a colorant.
10. The lightweight microporous ceramic filter material of claim 8, wherein the lightweight microporous ceramic filter material has a particle size of 0.5 to 5 mm.
11. The lightweight microporous ceramic filter material according to any one of claims 8 to 10, prepared by the preparation method according to any one of claims 1 to 7.
12. A method for preparing ceramic particles for water treatment and filtration is characterized by comprising the following steps:
the light microporous ceramic filter material prepared by the preparation method of any one of claims 1 to 7 or the light microporous ceramic filter material of any one of claims 8 to 10 is heated at the temperature of 300-400 ℃, then is poured into a normal-temperature alkali solution for soaking and surface activation treatment, and finally is naturally air-dried at the normal temperature.
13. The production method according to claim 12,
the heating time is 0.5-1.5 h;
and/or the soaking time is 20-40 min.
14. The production method according to claim 12,
the mass concentration of alkali in the alkali solution is 1-2 wt%;
and/or, the base in the base solution comprises sodium hydroxide.
15. The ceramic particles for water treatment and filtration are characterized by comprising a ceramic main material, a water reducing agent, agar powder, sodium carboxymethylcellulose, aluminum dihydrogen phosphate and alkali,
and the ceramic particles for water treatment filtration satisfy: carrying out high-speed high2G, the compressive strength is 5.5-5.78MPa, and the shear strength is 3.4-3.8 MPa.
16. The ceramic particles for water treatment filtration according to claim 15, further comprising a colorant.
17. The ceramic particles for water treatment filtration according to claim 15, which are prepared by the method of any one of claims 12 to 14.
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