CN109569315B - Preparation and application method of inorganic ceramic membrane for treating oily wastewater - Google Patents
Preparation and application method of inorganic ceramic membrane for treating oily wastewater Download PDFInfo
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Abstract
The invention discloses a preparation method of an inorganic ceramic membrane for treating oily wastewater, which comprises the following operation steps: (1) uniformly mixing deionized water and absolute ethyl alcohol to obtain a solvent, adding aluminum isopropoxide, uniformly stirring, continuing to use a hydrochloric acid solution, refluxing and stirring, and aging at room temperature to obtain an alumina sol; (2) dissolving cerium chloride and dysprosium chloride in water, mixing and stirring uniformly, continuously adding ammonia water and ammonium bicarbonate, heating the mixture, and carrying out heat preservation treatment to obtain rare earth sol; (3) and coating the sol on the cleaned microporous ceramic substrate for three times, drying, and roasting at high temperature to obtain the inorganic ceramic membrane. The inorganic ceramic membrane prepared by the invention has the advantages of large specific surface area, large pore volume, small pore diameter and obvious filtering effect, and is particularly suitable for treating oily wastewater in the mechanical field.
Description
Technical Field
The invention belongs to the technical field of ceramic membrane preparation and application, and particularly relates to a preparation method and a use method of an inorganic ceramic membrane for treating oily wastewater.
Background
Earlier membrane materials developed in the technical field of membranes are organic membranes which have the advantages of good toughness, easiness in processing and forming, simple preparation process, low price and the like, so that the application of the organic membrane is rapidly expanded to various fields. With the continuous development of membrane technology and the continuous improvement of the requirements of people on membrane materials, the defects of poor thermal stability, easy corrosion, short service life, difficult cleaning and the like of organic membranes are continuously exposed, so that the application of the organic membranes is limited. Therefore, inorganic materials such as ceramics, metals, glasses, and inorganic polymers have been the focus of research and development of membrane materials in recent three decades.
There are many methods for preparing inorganic ceramic films, such as solid particle sintering, thin film deposition, anodic oxidation, hydrothermal method, sol-gel method, etc. The sol-gel method is widely applied to the fields of electronics, composite materials, biology, ceramics, optics, electromagnetism, thermology, environmental treatment and the like due to the advantages of low reaction temperature, simple process, easy control of the process and the like. It is a new method in the wet chemical method for preparing materials. The method uses liquid chemical reagent or dissolves powder in solvent as raw material, and mixes the raw material uniformly under liquid phase; forming a stable transparent sol system after hydrolysis and polycondensation; the sol is aged, dried and sintered to prepare the required material, and the process is shown as the attached figure 1.
The sol-gel preparation technique has many advantages, mainly as follows: the process is simple, the equipment is cheap, the gel or powder with large specific surface area can be obtained, compared with a melting method or a chemical vapor deposition method, the heat treatment temperature is lower, and the strength and the toughness of the material are higher; the chemical uniformity of a multicomponent system is improved, which is very important for controlling the physical and chemical properties of the material; the reaction process is easy to control, and the microstructure of the gel can be regulated and controlled; the material prepared by the method has uniform components and high product purity; compared with other film preparation processes, the sol-gel process does not need vacuum conditions and too high temperature, and can carry out film coating on a substrate with large area or any shape; the method has the advantages of wide doping range of the prepared material, accurate stoichiometry and easy modification.
Lubricating oil used in the machining process, emulsified oil used for cooling and transmission, oily wastewater generated by cleaning parts, oily wastewater caused by equipment leakage, and wastewater discharged by flushing containers, equipment, the ground and the like in a machining workshop are main sources of the oily wastewater in the machining process. In the machining process, cutting efficiency can be obviously improved by using cutting (grinding) fluid, the precision of a workpiece is improved, the surface roughness of the workpiece is reduced, the corrosion of a cutter is reduced, the service life of the cutter is prolonged, the optimal economic effect is achieved, the friction between the cutter and the workpiece and between the cutter and chips is reduced, and heat generated by material deformation in a cutting area is taken away in time. Because the emulsion has the characteristics of certain lubricating effect, cooling effect, cleaning effect, antirust effect, health and safety benefits for workers and the like, the emulsion becomes the most widely used cutting fluid in production in recent years. During the machining and cleaning processes, the emulsion is polluted by bacteria, microorganisms, high temperature, mechanical impurities and the like to generate a large amount of emulsion waste liquid. Finally, the emulsion is exhausted as emulsion waste liquid after being failed, the main component of the emulsion is surfactant, and the surfactant is combined with the mechanical oil highly dispersed in water to form the emulsion oil with stable property, so that the treatment difficulty is high, the improper treatment can cause serious pollution.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method and a use method of an inorganic ceramic membrane for treating oily wastewater.
The invention is realized by the following technical scheme.
A preparation method of an inorganic ceramic membrane for treating oily wastewater comprises the following operation steps:
(1) uniformly mixing deionized water and absolute ethyl alcohol, heating to 88-92 ℃ to prepare a solvent, adding 8-12% by weight of aluminum isopropoxide into the solvent, uniformly stirring, continuously adding 1mol/L hydrochloric acid solution with the concentration of 2-4% by weight of the solvent, carrying out reflux stirring treatment for 5-8 hours, and carrying out aging treatment for 50-60 hours at room temperature to prepare alumina sol;
(2) dissolving 38-44 parts of cerium chloride and 13-19 parts of dysprosium chloride in 220 parts of 180-part water by weight, mixing and stirring uniformly, continuously adding 55-60 parts of ammonia water and 10-20 parts of ammonium bicarbonate, heating the mixture to 70-75 ℃, and carrying out heat preservation treatment for 2-3 hours to obtain rare earth sol;
(3) and putting the cleaned microporous ceramic substrate into alumina sol, standing for 40-50min, vertically lifting the microporous ceramic substrate upwards, drying, putting the microporous ceramic substrate into rare earth sol, standing for 2-3 h, vertically lifting upwards, drying, putting the microporous ceramic substrate into the alumina sol again, standing for 120min, vertically lifting upwards, drying, and roasting at high temperature to obtain the inorganic ceramic membrane.
Further, in the step (1), the volume ratio of the deionized water to the absolute ethyl alcohol is 2-4: 1.
Further, in the step (1), the average particle size of aluminum isopropoxide is 150-200 mesh.
Further, in the step (2), the mass fraction of the ammonia water is 27-32%, and the purity of the ammonium bicarbonate is 99%.
Further, in the step (3), the microporous ceramic substrate has a membrane tube outer diameter of 30mm, a channel inner diameter of 4.0mm, and a tube length of 500mm, and is made of alumina, silica, cordierite, zirconia, titania, or a mixture thereof.
Further, in the step (3), the vertical upward pulling rate is 4 to 6 mm/s.
Further, in the step (3), the drying temperature is 110-120 ℃, and the drying time is 2-3 hours.
Further, the temperature of the high-temperature roasting treatment is 850-900 ℃, and the treatment time is 2-3 hours.
The invention also provides a using method of the inorganic ceramic membrane for treating the oily wastewater, which comprises the following operation steps:
(1) oil-containing wastewater is filtered and pretreated by an oil separation tank and a paper bag;
(2) discharging the pretreated wastewater into a raw material tank, heating the wastewater to 57-60 ℃, and carrying out heat preservation and stirring treatment for 100-fold and 120 min;
(3) and pumping the wastewater in the raw material tank into the inorganic ceramic membrane component by a circulating pump, and controlling the pressure after the circulating pump to be 0.26-0.32 MPa.
According to the technical scheme, the beneficial effects of the invention are as follows:
the preparation method of the inorganic ceramic membrane for treating the oily wastewater, provided by the invention, has the advantages of simple operation, low cost, time and labor saving, the time consumption is 1-2 months in the prior art, and the prepared inorganic ceramic membrane has a large specific surface area which can reach 340m2About/g, large pore volume, small pore diameter and obvious filtering effect, and is particularly suitable for treating oily wastewater in the mechanical field. According to the invention, a cerium oxide and dysprosium oxide film layer is prepared in two layers of aluminum oxide inorganic ceramic films, so that the contact angle of organic waste on the surface of the ceramic film can be effectively increased, and the retention effect of the ceramic film on the organic waste is further improved; according to the use method of the inorganic ceramic membrane for treating the oily wastewater, provided by the invention, after the pretreatment of filtering through the oil separation tank and the paper bag, the content of macromolecular impurities in the wastewater can be effectively reduced, the filtering pressure of the inorganic ceramic membrane is relieved, meanwhile, the temperature of the wastewater is raised, and the interception effect of the inorganic ceramic membrane on organic substances in the wastewater can be further improved.
Drawings
Fig. 1 is a process flow for preparing an inorganic ceramic membrane in the prior art.
FIG. 2 is a schematic view showing the structure of a partitioned oil pool in example 5.
Fig. 3 is a schematic structural view of a paper bag filter device in example 5.
Fig. 4 is a schematic perspective view of the inorganic ceramic membrane module of example 5.
Fig. 5 is a top view of the inorganic ceramic membrane module of example 5.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
A preparation method of an inorganic ceramic membrane for treating oily wastewater comprises the following operation steps:
(1) uniformly mixing deionized water and absolute ethyl alcohol, heating to 88 ℃ to obtain a solvent, adding 8 wt% of aluminum isopropoxide into the solvent, uniformly stirring, continuously adding a hydrochloric acid solution with the concentration of 1mol/L, the mass percent of the solvent being 2%, refluxing, stirring and treating for 5 hours, and aging at room temperature for 50 hours to obtain alumina sol;
(2) dissolving 38 parts by weight of cerium chloride and 13 parts by weight of dysprosium chloride in 180 parts by weight of water, mixing and stirring uniformly, continuously adding 55 parts by weight of ammonia water and 10 parts by weight of ammonium bicarbonate, heating the mixture to 70 ℃, and carrying out heat preservation treatment for 2 hours to obtain rare earth sol;
(3) putting the cleaned microporous ceramic substrate into alumina sol, standing for 40min, vertically lifting the microporous ceramic substrate upwards, drying, putting into rare earth sol, standing for 2 h, vertically lifting upwards, drying, putting into alumina sol again, standing for 100min, vertically lifting upwards, drying, and roasting at high temperature to obtain the inorganic ceramic membrane.
Further, in the step (1), the volume ratio of the deionized water to the absolute ethyl alcohol is 2: 1.
Further, in the step (1), the average particle size of aluminum isopropoxide is 150 mesh.
Further, in the step (2), the mass fraction of the ammonia water is 27%, and the purity of the ammonium bicarbonate is 99%.
Furthermore, in the step (3), the microporous ceramic substrate has a membrane tube with an outer diameter of phi 30mm, a channel inner diameter of phi 4.0mm, a tube length of 500mm, and is made of alumina.
Further, in the above step (3), the vertical pull-up rate was 4 mm/s.
Further, in the step (3), the temperature of the drying treatment was 110 ℃ and the time of the drying treatment was 2 hours.
Further, the temperature of the high-temperature calcination treatment was 850 ℃ and the treatment time was 2 hours.
Example 2
A preparation method of an inorganic ceramic membrane for treating oily wastewater comprises the following operation steps:
(1) uniformly mixing deionized water and absolute ethyl alcohol, heating to 90 ℃ to obtain a solvent, adding 10 wt% of aluminum isopropoxide into the solvent, uniformly stirring, continuously adding a hydrochloric acid solution with the concentration of 1mol/L and the mass of the solvent being 3%, refluxing, stirring and treating for 7 hours, and aging at room temperature for 55 hours to obtain alumina sol;
(2) dissolving 40 parts by weight of cerium chloride and 16 parts by weight of dysprosium chloride in 200 parts by weight of water, mixing and stirring uniformly, continuously adding 58 parts by weight of ammonia water and 15 parts by weight of ammonium bicarbonate, heating the mixture to 73 ℃, and carrying out heat preservation treatment for 2.5 hours to obtain rare earth sol;
(3) and putting the cleaned microporous ceramic substrate into alumina sol, standing for 45min, vertically lifting the microporous ceramic substrate upwards, drying, putting the microporous ceramic substrate into rare earth sol, standing for 2.5 h, vertically lifting upwards, drying, putting the microporous ceramic substrate into the alumina sol again, standing for 110min, vertically lifting upwards, drying, and roasting at high temperature to obtain the inorganic ceramic membrane.
Further, in the step (1), the volume ratio of the deionized water to the absolute ethyl alcohol is 3: 1.
Further, in the step (1), the average particle size of aluminum isopropoxide is 180 mesh.
Further, in the step (2), the mass fraction of the ammonia water is 30%, and the purity of the ammonium bicarbonate is 99%.
Furthermore, in the step (3), the microporous ceramic substrate has a membrane tube with an outer diameter of phi 30mm, a channel inner diameter of phi 4.0mm, a tube length of 500mm, and is made of silicon oxide.
Further, in the above step (3), the vertical pull-up rate was 5 mm/s.
Further, in the step (3), the temperature of the drying treatment was 115 ℃ and the time of the drying treatment was 2.5 hours.
Further, the temperature of the high-temperature calcination treatment was 880 ℃ and the treatment time was 2.5 hours.
Example 3
A preparation method of an inorganic ceramic membrane for treating oily wastewater comprises the following operation steps:
(1) uniformly mixing deionized water and absolute ethyl alcohol, heating to 91 ℃ to obtain a solvent, adding 11% of aluminum isopropoxide by weight into the solvent, uniformly stirring, continuously adding a hydrochloric acid solution with the concentration of 1mol/L and the mass of the solvent being 3%, refluxing, stirring and treating for 7 hours, and aging at room temperature for 58 hours to obtain alumina sol;
(2) dissolving 42 parts by weight of cerium chloride and 18 parts by weight of dysprosium chloride in 210 parts by weight of water, mixing and stirring uniformly, continuously adding 58 parts by weight of ammonia water and 18 parts by weight of ammonium bicarbonate, heating the mixture to 74 ℃, and carrying out heat preservation treatment for 2.8 hours to obtain rare earth sol;
(3) and putting the cleaned microporous ceramic substrate into alumina sol, standing for 48min, vertically lifting the microporous ceramic substrate upwards, drying, putting the microporous ceramic substrate into rare earth sol, standing for 2.5 h, vertically lifting upwards, drying, putting the microporous ceramic substrate into the alumina sol again, standing for 110min, vertically lifting upwards, drying, and roasting at high temperature to obtain the inorganic ceramic membrane.
Further, in the step (1), the volume ratio of the deionized water to the absolute ethyl alcohol is 3: 1.
Further, in the step (1), the average particle size of aluminum isopropoxide is 200 mesh.
Further, in the step (2), the mass fraction of the ammonia water is 31%, and the purity of the ammonium bicarbonate is 99%.
Furthermore, in the step (3), the microporous ceramic substrate has a membrane tube outer diameter of 30mm, a channel inner diameter of 4.0mm, a tube length of 500mm, and is made of cordierite.
Further, in the above step (3), the vertical pull-up rate was 6 mm/s.
Further, in the step (3), the temperature of the drying treatment was 118 ℃ and the time of the drying treatment was 2.8 hours.
Further, the temperature of the high-temperature calcination treatment was 880 ℃ and the treatment time was 2.5 hours.
Example 4
A preparation method of an inorganic ceramic membrane for treating oily wastewater comprises the following operation steps:
(1) uniformly mixing deionized water and absolute ethyl alcohol, heating to 92 ℃ to obtain a solvent, adding 12 wt% of aluminum isopropoxide into the solvent, uniformly stirring, continuously adding a hydrochloric acid solution with the concentration of 1mol/L, the mass percent of the solvent being 4% of that of the solvent, refluxing, stirring and treating for 8 hours, and aging at room temperature for 60 hours to obtain alumina sol;
(2) dissolving 44 parts by weight of cerium chloride and 19 parts by weight of dysprosium chloride in 220 parts by weight of water, mixing and stirring uniformly, continuously adding 60 parts by weight of ammonia water and 20 parts by weight of ammonium bicarbonate, heating the mixture to 75 ℃, and carrying out heat preservation treatment for 3 hours to obtain rare earth sol;
(3) putting the cleaned microporous ceramic substrate into alumina sol, standing for 50min, vertically lifting the microporous ceramic substrate upwards, drying, putting into rare earth sol, standing for 3 h, vertically lifting upwards, drying, putting into alumina sol again, standing for 120min, vertically lifting upwards, drying, and roasting at high temperature to obtain the inorganic ceramic membrane.
Further, in the step (1), the volume ratio of the deionized water to the absolute ethyl alcohol is 4: 1.
Further, in the step (1), the average particle size of aluminum isopropoxide is 200 mesh.
Further, in the step (2), the mass fraction of the ammonia water is 32%, and the purity of the ammonium bicarbonate is 99%.
Furthermore, in the step (3), the microporous ceramic substrate has a membrane tube with an outer diameter of phi 30mm, a channel inner diameter of phi 4.0mm, and a tube length of 500mm, and is made of a mixture of alumina and zirconia.
Further, in the above step (3), the vertical pull-up rate was 6 mm/s.
Further, in the step (3), the temperature of the drying treatment was 120 ℃ and the time of the drying treatment was 3 hours.
Further, the temperature of the high-temperature calcination treatment was 900 ℃ and the treatment time was 3 hours.
The inorganic ceramic films were prepared by the methods of the examples, and then the properties thereof were tested, the test results are shown in table 1:
table 1 inorganic ceramic film performance test results
| Item | Most probable pore radius, nm | Average pore radius, nm | Specific surface area, m2/g | Pore volume, cm3/g |
| Example 1 | 1.02 | 2.14 | 339.32 | 0.293 |
| Example 2 | 1.02 | 2.12 | 340.58 | 0.299 |
| Example 3 | 1.01 | 2.11 | 342.25 | 0.302 |
| Example 4 | 1.00 | 2.10 | 344.31 | 0.306 |
Example 5
The use method of the inorganic ceramic membrane for treating the oily wastewater comprises the following operation steps:
(1) oil-containing wastewater is subjected to filtering pretreatment by an oil separation tank and a paper bag, wherein the oil separation tank is a horizontal flow type oil separation tank and consists of a water distribution tank 1, a water inlet pipe 2, a water inlet valve plate 3, a manual oil scraping plate 4, an oil collecting tank 5, a water outlet valve plate 6, a water outlet tank 7 and a water outlet pipe 8, and the structure of the horizontal flow type oil separation tank is shown in the attached figure 2; the paper bag filtering device consists of a tank body 9 at the lower part and paper tape filtering cloth 10 arranged at the upper part of the tank body, the periphery of the paper tape filtering cloth is tightly fixed at the periphery of the tank body by weights to form a filtering body capable of bearing certain weight and pressure, as shown in figure 3;
(2) discharging the pretreated wastewater into a raw material tank, heating the wastewater to 57-60 ℃, and carrying out heat preservation and stirring treatment for 100-fold and 120 min;
(3) the method comprises the following steps of pumping wastewater in a raw material tank into an inorganic ceramic membrane component by a circulating pump, controlling the pressure after the circulating pump to be 0.26-0.32MPa, wherein the inorganic ceramic membrane component consists of a ceramic membrane component mounting column 21, a standby circulating pipe 22, a ceramic membrane component outer shell 23, a ceramic membrane component baffle bolt 24, a ceramic membrane component baffle 25, a circulating hole 26 and an inorganic ceramic membrane 27, the structure of the inorganic ceramic membrane component is shown in the attached drawings 4 and 5, and the water quality before and after the inorganic ceramic membrane provided by the invention is treated is shown in a table 2:
TABLE 2 Water quality before and after treatment of wastewater by inorganic ceramic Membrane Process
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art should understand that they can make various changes, modifications, additions and substitutions within the spirit and scope of the present invention.
Claims (8)
1. The preparation method of the inorganic ceramic membrane for treating the oily wastewater is characterized by comprising the following operation steps of:
(1) uniformly mixing deionized water and absolute ethyl alcohol, heating to 88-92 ℃ to prepare a solvent, adding 8-12% by weight of aluminum isopropoxide into the solvent, uniformly stirring, continuously adding 1mol/L hydrochloric acid solution with the concentration of 2-4% by weight of the solvent, carrying out reflux stirring treatment for 5-8 hours, and carrying out aging treatment for 50-60 hours at room temperature to prepare alumina sol;
(2) dissolving 38-44 parts of cerium chloride and 13-19 parts of dysprosium chloride in 220 parts of water of 180-fold proportion by weight, mixing and stirring uniformly, continuously adding 55-60 parts of ammonia water and 10-20 parts of ammonium bicarbonate, heating the mixture to 70-75 ℃, and carrying out heat preservation treatment for 2-3 hours to obtain rare earth sol;
(3) and putting the cleaned microporous ceramic substrate into alumina sol, standing for 40-50min, vertically lifting the microporous ceramic substrate upwards, drying, putting the microporous ceramic substrate into rare earth sol, standing for 2-3 h, vertically lifting upwards, drying, putting the microporous ceramic substrate into the alumina sol again, standing for 120min, vertically lifting upwards, drying, and roasting at high temperature to obtain the inorganic ceramic membrane.
2. The method for preparing an inorganic ceramic membrane for treating oily wastewater according to claim 1, wherein in the step (1), the volume ratio of the deionized water to the absolute ethyl alcohol is 2-4: 1.
3. The method as claimed in claim 1, wherein the average particle size of the aluminum isopropoxide in step (1) is 150-200 mesh.
4. The method according to claim 1, wherein in the step (2), the mass fraction of the ammonia water is 27-32%, and the purity of the ammonium bicarbonate is 99%.
5. The method according to claim 1, wherein in the step (3), the microporous ceramic substrate has a membrane tube diameter of 30mm, a channel inner diameter of 4.0mm, and a tube length of 500mm, and is made of alumina, silica, cordierite, zirconia, titania, or a mixture thereof.
6. The method for producing an inorganic ceramic membrane for treating oily wastewater as claimed in claim 1, wherein in the step (3), the vertical upward pulling rate is 4 to 6 mm/s.
7. The method as claimed in claim 1, wherein the drying temperature in step (3) is 110-120 ℃, and the drying time is 2-3 hours.
8. The method as claimed in claim 1, wherein the high temperature calcination treatment is performed at 850-900 ℃ for 2-3 hours.
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| ES2466571B1 (en) * | 2014-03-12 | 2015-03-16 | Likuid Nanotek, S.L. | Ceramic filtration membrane |
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| CN102614782A (en) * | 2012-04-12 | 2012-08-01 | 上海海事大学 | Ceramic filter film of rare-earth modified attapulgite with nano coating and preparation method thereof |
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