CN114516750B - Nano-micro porous ceramic based on oil-containing waste residue recycling and preparation method and application thereof - Google Patents
Nano-micro porous ceramic based on oil-containing waste residue recycling and preparation method and application thereof Download PDFInfo
- Publication number
- CN114516750B CN114516750B CN202210416871.6A CN202210416871A CN114516750B CN 114516750 B CN114516750 B CN 114516750B CN 202210416871 A CN202210416871 A CN 202210416871A CN 114516750 B CN114516750 B CN 114516750B
- Authority
- CN
- China
- Prior art keywords
- micro porous
- nano
- oil
- porous ceramic
- containing waste
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62665—Flame, plasma or melting treatment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/08—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
- C04B38/085—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances of micro- or nanosize
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/443—Nitrates or nitrites
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/448—Sulphates or sulphites
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
A nano-micro porous ceramic based on oil-containing waste residue recycling and a preparation method and application thereof belong to the field of waste recycling and environmental protection and treatment. The nano-micro porous ceramic is: the method comprises the steps of taking oil-containing waste residues and magnetic particle components as basic raw materials, preparing magnetic nano-micro porous particles by a thermal plasma transient high-temperature sintering process, taking the magnetic nano-micro porous particles as main components, preparing a ceramic green body by a slurry method, and finally sintering at high temperature to obtain the magnetic nano-micro porous ceramic. The invention simultaneously realizes the purpose of treating wastes by wastes and comprehensively recycling and treating wastes, can effectively relieve the environmental pressure and ecological pollution caused by long-term stacking of the oily waste residues in China, and can develop the oily waste residues into wastewater purification treatment products with high added values, thereby realizing the real change of wastes into valuables.
Description
Technical Field
The invention belongs to the technical field of ceramics, relates to a preparation method and application of nano-micro porous ceramics, and particularly relates to a preparation method and application of nano-micro porous ceramics based on oil-containing waste residue recycling.
Background
A large amount of oil-containing waste residues are generated in oil exploitation. According to statistics, the oil-containing waste residue yield of China at the present stage is up to 40 ten thousand tons/year, and the oil-containing waste residue has the characteristics of high production speed and high yield, and becomes a pollutant seriously harming the ecological environment and the human health. Oily waste residues are classified as oily waste in the national catalog of hazardous wastes, and the national clean production promotion law requires harmless treatment of the oily waste residues. But the oily waste residue is complex in component and mainly comprises components such as solid minerals, water, petroleum, polymers, inorganic salts and the like, wherein the petroleum component accounts for about 3-15%, the solid minerals account for more than 80%, and quartz, kaolinite, mica, corundum, dolomite, pyrite and the like are used as main components. The harmless treatment technology of the oily waste residues comprises various modes such as solidification landfill, thermal desorption, chemical hot washing, incineration, biological treatment and the like, and currently, solidification landfill and incineration treatment methods are widely adopted; the oil-containing waste residue resource is mainly used for building material filler production, deep profile control and oil displacement increase in oil fields and the like. Can simultaneously give consideration to harmless treatment and resource recycling, and has the shortage of treatment technology with economic competitiveness.
There are some reports on the technology of harmless and recycling treatment of oil-containing waste residues. For example, based research on oil-containing waste residues is carried out by professor goeh, and preparation and performance analysis of low-density petroleum propping agent are carried out by taking the oil-containing waste residues as main raw materials, so that a new way for resource utilization is explored.
CN201610172350.5 discloses a method for treating oily waste residues by microorganisms, which is characterized by utilizing a prefabricated microbial reaction bed, wherein the reaction bed combines the advantages of a soil cultivation method, a composting method, a prefabricated bed method and a bioreactor method in the microbial remediation technology. The method can improve the microbial activity and the degradation efficiency, shorten the degradation time, and more rapidly degrade the oily pollutants in the waste residues, and solves the problems of poor microbial adaptability, low microbial activity, low treatment efficiency, incomplete treatment effect and the like in the prior microbial technology for treating the oily waste residues. However, the method cannot effectively utilize oil phase components in the oil-containing waste residue, is greatly influenced by temperature and humidity, and has large difficulty in large-scale application.
CN201710223019.6 discloses a method for recovering oil-containing waste residues, which is characterized in that octanol and the oil-containing waste residues are used for preparing and stirring mixed liquid, then the mixed liquid is put into a reaction kettle for stirring, so that the octanol dissolves oil phase in the waste residues, then the waste residues are filtered, solid phase is dried, and the mixed solution is dealcoholized. The invention can recover the oil phase in the waste residue and realize the reutilization of the crude oil.
CN201822112060.9 discloses a innocent treatment system of oiliness water waste residue, this innocent treatment system of its characterized in that includes waste residue feed unit and coking device, the discharge gate of waste residue feed unit all communicates with coking device's bottom feed inlet and top feed inlet, and it has utilized the abundant waste heat of coking device in a large amount of big steam blowing stage, handles oiliness waste residue, through set up spray set in coking device's top and bottom, spouts the waste residue into, has improved coking device's waste residue treatment volume by a wide margin, and simultaneously, the top spray set who adds has played the effect of washing, prevents when the waste residue is handled, and steam brings the solid into the risk of oil gas pipeline and contact cooling tower. The method only realizes the harmlessness of the waste residue containing oil and water, and cannot realize the resource utilization of useful components.
Disclosure of Invention
One of the purposes of the invention is to provide a nano-micro porous ceramic based on oil-containing waste residue resource, wherein the nano-micro porous ceramic is prepared from the following components in parts by weight: the method comprises the steps of taking oil-containing waste residues and magnetic particle components as basic raw materials, preparing magnetic nano-micro porous particles by a thermal plasma transient high-temperature sintering process, taking the magnetic nano-micro porous particles as main components, preparing a ceramic green body by a slurry method, and finally sintering at high temperature to obtain the magnetic nano-micro porous ceramic.
Furthermore, the inside of the nano-micro porous ceramic has a porous structure, and the pore size of the nano-micro porous ceramic is 0.1-20.0 mu m.
Furthermore, the magnetic particles in the nano-micro porous ceramic have an association effect with the polar end of the surfactant in the oily wastewater, so that the demulsification effect of emulsion droplets in the wastewater can be obviously improved.
Furthermore, the pressure-bearing strength of the nano-micro porous ceramic is greater than 10Mpa, the mechanical strength is high, and the nano-micro porous ceramic is not easy to damage.
The invention also aims to provide a preparation method of the nano-micro porous ceramic, which comprises the following steps:
(1) mixing the oil-containing waste residue, bauxite and a pore-forming agent, drying and crushing to obtain a mixture;
(2) dispersing the mixture obtained in the step (1) into a ferrous salt solution, soaking to enable the mixture to fully adsorb ferrous ions, then filtering, and drying a filter cake to obtain a sintering precursor;
(3) sintering the sintering precursor obtained in the step (2) by adopting thermal plasma transient high temperature to obtain magnetic nano-micro porous particles;
(4) dispersing the magnetic nano-micro porous particles obtained in the step (4) with calcium hydroxide and sodium silicate in water to prepare slurry, putting the slurry into a centrifugal die for centrifugation to obtain a preliminarily molded ceramic green body, and drying the ceramic green body;
(5) and sintering the dried ceramic green body in a high-temperature furnace to obtain the nano-micro porous ceramic.
The magnetic nano-micro porous ceramic is prepared by taking oil-containing waste residues as raw materials, fully utilizing oil phase components in the oil-containing waste residues and other additives to realize pore forming, modifying the oil-containing waste residues by utilizing magnetic particles, preparing the magnetic nano-micro porous particles by a thermal plasma transient high-temperature sintering process, further taking the magnetic nano-micro porous particles as main raw materials, preparing ceramic green bodies by utilizing a slurry method, and preparing the magnetic nano-micro porous ceramic by high-temperature sintering.
Further, the pore-forming agent in the step (1) is one or more of ammonium sulfate, ammonium chloride and ammonium nitrate, and the crushed mixture is below 500 meshes; the composition of the mixture is as follows: by weight, 30-40% of oil-containing waste residue, 55-68% of bauxite and 2-5% of pore-forming agent.
Further, in the step (2), the ferrous salt is one or more of ferrous sulfate, ferrous gluconate, ferrous nitrate and ferrous chloride, and the mass concentration of the ferrous salt solution is 2-20%; the weight ratio of the mixture to the ferrous salt solution is as follows: 20-50% of powder and 50-80% of magnetic ferrous solution.
Furthermore, in the step (3), the sintering temperature is 800-2200 ℃, and the sintering time is 5-120 s.
Further, the slurry in the step (4) comprises the following components: by weight, the magnetic nano-micro porous particles are 15-35%, the calcium hydroxide is 3-12%, the sodium silicate is 3-10%, and the water is 43-79%.
Furthermore, in the step (5), the sintering temperature is 1000-1400 ℃, and the sintering time is 2-24 h.
The invention also aims to provide the application of the nano-micro porous ceramic, which is used for purifying oily wastewater in oil fields, factories and mines or daily chemical industry.
The invention has the greatest advantage of simultaneously realizing the purposes of treating wastes with processes of wastes against one another and comprehensively recycling and treating wastes. The invention not only can effectively relieve the environmental pressure and ecological pollution caused by long-term stacking of the oily waste residues in China, but also can develop the oily waste residues into a waste water purification treatment product with high added value, thereby realizing the real change of waste into valuable and opening up a new direction of high-end utilization for harmless treatment and resource utilization of the oily waste residues.
The invention has the following beneficial technical effects:
1. the invention uses the solid waste oil-containing waste residue as the raw material to prepare the magnetic porous ceramic, reduces the using amount of minerals such as high-quality bauxite, effectively utilizes the chemical components of the oil-containing waste residue, and realizes the resource utilization of dangerous solid waste.
2. The magnetic modified porous ceramic prepared by the invention has a porous structure in the interior, the pore size is 0.1-20.0 mu m, the demulsification effect of emulsion droplets in wastewater can be obviously improved by association between the magnetic particles in the magnetic modified porous ceramic and the polar end of a surfactant in oily wastewater, the magnetic modified porous ceramic has the advantages of excellent floating oil and dispersed oil filtering effects and excellent emulsified oil filtering effect of the magnetic particles, the COD removal rate is higher than 95% and the turbidity removal rate is higher than 97% after oilfield wastewater treatment. Chemical agents are not needed in the treatment process, the effect of completely removing the waste liquor after treatment is almost achieved, and the national emission standard is met. Compared with the prior porous ceramic for treating the oily wastewater, the invention not only simplifies the process flow of the oily wastewater treatment, but also avoids secondary pollution caused by using chemical agents.
3. The magnetic modified porous ceramic prepared by the invention has the advantages of pressure-bearing strength of more than 10Mpa, high mechanical strength, difficult damage and long service life.
Drawings
FIG. 1 is an SEM photograph of the magnetic nanoporous ceramic obtained in example 1.
Detailed Description
The technical scheme of the invention is clearly and completely described below by combining the attached drawings of the specification. It is to be understood that the described embodiments are merely exemplary of some, and not necessarily all, embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments of the present invention, belong to the protection scope of the present invention.
Example 1
(1) Mechanically mixing oil-containing waste residue of Hongkong oil field, bauxite (Zhengzhou Yanxia refractory Co., Ltd.) and ammonium nitrate at 30%, 68% and 2% respectively, drying at 105 deg.C for 2 hr, pulverizing the above particles to particle size below 500 mesh in a pulverizer, and mixing.
(2) And dispersing the uniformly mixed powder into 3kg of ferrous sulfate solution with the mass fraction of 2%, soaking for 24h for sufficient adsorption, then filtering, and drying the filtered solid mixture at 100 ℃ for 3h to obtain a sintering precursor.
(3) And (3) performing transient high-temperature sintering on the precursor by using a thermal plasma device (produced by Process engineering research institute of Chinese academy of sciences) with the power of 100KW, wherein the sintering flame temperature is 2200 ℃, the sintering time is 5s, and magnetic nano-micro porous particles with the particle size of 200 mu m and the internal pore size of 0.1-5.0 mu m are prepared.
(4) The prepared magnetic nano-micro porous particles, calcium hydroxide, sodium silicate and water are prepared into slurry, wherein the mass fractions of the four components are 35%, 12%, 10% and 33%, and the total mass fraction is 13 kg. And putting the slurry into a centrifugal mold, centrifuging to obtain a preliminarily molded ceramic green body, putting the ceramic green body into an oven, drying for 6 hours at 55 ℃, and then drying for 5 hours at 100 ℃.
(5) And (3) putting the ceramic green body formed by primary sintering into a high-temperature furnace, and sintering for 24 hours at 1000 ℃ to obtain the magnetic nano-micro porous ceramic.
Example 2
(1) Mechanically mixing oil-containing waste residue of North China oil field, bauxite (Zhengzhou Yanxia refractory Co., Ltd.) and ammonium chloride at mass percentages of 40%, 55% and 5%, respectively, 3kg in total, drying at 100 deg.C for 6h, pulverizing the above particles to particle size below 500 mesh in a pulverizer, and mixing well.
(2) And dispersing the uniformly mixed powder into 3kg of ferrous gluconate solution with the mass fraction of 20%, soaking for 1h for sufficient adsorption, then filtering, and drying the filtered solid mixture at 105 ℃ for 1h to obtain a sintering precursor.
(3) And (3) performing transient high-temperature sintering on the precursor by using thermal plasma equipment (produced by Process engineering research institute of Chinese academy of sciences) with the power of 80KW, wherein the sintering flame temperature is 1200 ℃, the sintering time is 10s, and magnetic nano-micro porous particles with the particle size of 120 mu m and the internal pore size of 0.1-3.0 mu m are prepared.
(4) The prepared magnetic nano-micro porous particles, calcium oxide, sodium silicate and water are prepared into slurry, wherein the mass fractions of the four components are 15%, 12%, 3% and 70%, and the total mass fraction is 13 kg. And putting the slurry into a centrifugal mold, centrifuging to obtain a preliminarily molded ceramic green body, putting the ceramic green body into an oven, drying for 4h at 90 ℃, and then drying for 1h at 150 ℃.
(5) And (3) putting the ceramic green body formed by primary sintering into a high-temperature furnace, and sintering for 2 hours at 1400 ℃ to obtain the magnetic nano-micro porous ceramic.
Example 3
(1) Mechanically mixing oil-containing waste residue of North China oil field, bauxite (Zhengzhou Yanxia refractory Co., Ltd.) and ammonium chloride at mass percentages of 35%, 60% and 3% respectively, and drying at 102 deg.C for 4 hr, pulverizing the above particles to particle size below 500 mesh in a pulverizer, and mixing well.
(2) And dispersing the uniformly mixed powder into 3kg of ferrous nitrate solution with the mass fraction of 12%, soaking for 1h for sufficient adsorption, then filtering, and drying the filtered solid mixture at 105 ℃ for 1h to obtain a sintering precursor.
(3) And (2) performing transient high-temperature sintering on the precursor by using thermal plasma equipment (produced by Process engineering research institute of Chinese academy of sciences) with the power of 80KW, wherein the sintering flame temperature is 800 ℃, the sintering time is 15s, and magnetic nano-micro porous particles with the particle size of 12 mu m and the internal pore size of 0.1-1.0 mu m are prepared.
(4) The prepared magnetic nano-micro porous particles, calcium oxide, sodium silicate and water are prepared into slurry, wherein the mass fractions of the four components are respectively 25%, 8%, 6% and 61%, and the total mass fraction is 13 kg. And putting the slurry into a centrifugal mold, centrifuging to obtain a preliminarily formed ceramic green body, putting the ceramic green body into a drying box, drying for 3 hours at 75 ℃, and then drying for 3 hours at 120 ℃.
(5) And (3) putting the ceramic green body formed by primary sintering into a high-temperature furnace, and sintering for 12 hours at 1200 ℃ to obtain the magnetic nano-micro porous ceramic.
Example 4
The end face of the magnetic nano-micro porous ceramic prepared in the above examples 1 to 3 is cut by a metallographic cutter, and the pore size inside the magnetic nano-micro porous ceramic is measured by a mercury intrusion detector, and the result shows that the magnetic nano-micro porous ceramic has a porous structure inside and the pore size is 0.1 to 18.0 μm, which is shown in table 1, wherein the photograph of the end face of the magnetic nano-micro porous ceramic 1 measured by an end face scanning electron microscope is shown in fig. 1.
TABLE 1 pore size of magnetic nanoporous ceramics
Example 5
The magnetic nano-micro porous ceramics prepared in the above examples 1 to 3 are used as a filter plate for treating oily wastewater, and the oily wastewater produced in a Hongkong oilfield is treated. Meanwhile, a commercial large-channel dense porous ceramic membrane (produced by Zhou porcelain industry Co., Ltd. in south of the river) is purchased for comparison, and various indexes of the oily wastewater before and after treatment are shown in Table 2.
TABLE 2 technical indexes before and after treatment of oily wastewater
Table 2 shows that the magnetic nano-micro porous ceramic has good oily wastewater treatment effect and is superior to the existing large-channel dense porous ceramic.
Example 6
The pressure-bearing strength of the magnetically modified porous ceramics prepared in examples 1 to 3 was measured in a pressure tester (Meits Co.), and the test results are shown in Table 3.
TABLE 3 compressive strength of magnetic nanoporous ceramics
Table 3 shows that the pressure-bearing strength of the magnetic nano-micro porous ceramic is higher than 10Mpa, and the magnetic nano-micro porous ceramic has good mechanical strength.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made in the above embodiments by those of ordinary skill in the art without departing from the principle and spirit of the present invention. The scope of the invention is defined by the claims and their equivalents.
Claims (6)
1. The preparation method of the nano-micro porous ceramic based on the oil-containing waste residue resource is characterized by comprising the following steps:
(1) mixing the oil-containing waste residue, bauxite and a pore-forming agent, drying and crushing to obtain a mixture; the composition of the mixture is as follows: by weight, 30-40% of oil-containing waste residue, 55-68% of bauxite and 2-5% of pore-forming agent;
(2) dispersing the mixture obtained in the step (1) into a ferrous salt solution, soaking to enable the mixture to fully adsorb ferrous ions, then filtering, and drying a filter cake to obtain a sintering precursor; the weight ratio of the mixture to the ferrous salt solution is as follows: 20-50% of mixture and 50-80% of ferrite solution;
(3) sintering the sintering precursor obtained in the step (2) by adopting thermal plasma transient high temperature to obtain magnetic nano-micro porous particles;
(4) dispersing the magnetic nano-micro porous particles obtained in the step (3) with calcium hydroxide and sodium silicate in water to prepare slurry, putting the slurry into a centrifugal die for centrifugation to obtain a preliminarily molded ceramic green body, and drying the ceramic green body; the slurry comprises the following components: by weight, 15 to 35 percent of magnetic nano-micro porous particles, 3 to 12 percent of calcium hydroxide, 3 to 10 percent of sodium silicate and 43 to 79 percent of water;
(5) sintering the dried ceramic green body in a high-temperature furnace to prepare nano-micro porous ceramic;
the inside of the nano-micro porous ceramic has a porous structure, and the pore size of the nano-micro porous ceramic is 0.1-20.0 mu m.
2. The preparation method of the nano-micro porous ceramic based on the oil-containing waste residue resource utilization according to claim 1, wherein the pore-forming agent in the step (1) is one or more of ammonium sulfate, ammonium chloride and ammonium nitrate, and the crushed mixture is below 500 meshes.
3. The method for preparing nano-micro porous ceramics based on oil-containing waste residue resource utilization according to claim 1, wherein the ferrous salt in the step (2) is one or more of ferrous sulfate, ferrous gluconate, ferrous nitrate and ferrous chloride, and the ferrous salt solution has a mass concentration of 2-20%.
4. The method for preparing the nano-micro porous ceramic based on the resource utilization of the oil-containing waste residue according to claim 1, wherein the sintering temperature in the step (3) is 800-2200 ℃, and the sintering time is 5-120 s.
5. The preparation method of the nano-micro porous ceramic based on the oil-containing waste residue resource utilization according to claim 1, wherein the sintering temperature in the step (5) is 1000-1400 ℃, and the sintering time is 2-24 h.
6. The application of the nano-micro porous ceramic prepared by the preparation method according to any one of claims 1 to 5 in the purification treatment of oily wastewater in oil fields, factories and mines or the daily chemical industry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210416871.6A CN114516750B (en) | 2022-04-21 | 2022-04-21 | Nano-micro porous ceramic based on oil-containing waste residue recycling and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210416871.6A CN114516750B (en) | 2022-04-21 | 2022-04-21 | Nano-micro porous ceramic based on oil-containing waste residue recycling and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114516750A CN114516750A (en) | 2022-05-20 |
| CN114516750B true CN114516750B (en) | 2022-07-01 |
Family
ID=81600348
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210416871.6A Active CN114516750B (en) | 2022-04-21 | 2022-04-21 | Nano-micro porous ceramic based on oil-containing waste residue recycling and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114516750B (en) |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003079266A (en) * | 2001-09-07 | 2003-03-18 | Kenji Shinohara | Concrete member for cleaning water and improving seabed |
| CN102826706B (en) * | 2012-09-28 | 2014-02-12 | 湖南科技大学 | Oilfield produced water treatment method and device |
| CN103241970B (en) * | 2013-05-08 | 2014-09-24 | 清远绿由环保科技有限公司 | Sintering expansion type light ceramsite produced by using oily sludge and manufacture method of sintering expansion type light ceramsite |
| CN103920475B (en) * | 2014-05-11 | 2016-06-08 | 萍乡市同凯科技有限公司 | A kind of magnetic material for removing coal pyrolysis oil-polluted water ash float |
| CN106430833A (en) * | 2016-10-28 | 2017-02-22 | 博天环境工程（北京）有限公司 | Treatment method of oil-containing waste water |
| CN106830431B (en) * | 2017-03-07 | 2020-10-02 | 同济大学 | Method for treating waste emulsion by combining magnetic nanoparticles and ultrafiltration membrane |
| CN111196731A (en) * | 2019-12-25 | 2020-05-26 | 山东山科生态环境研究院有限公司 | Method for fixing heavy metal in oil sludge dry slag, porous ceramsite and application |
| CN112110744A (en) * | 2020-09-10 | 2020-12-22 | 中科院过程工程研究所南京绿色制造产业创新研究院 | Magnetic porous ceramic adsorption material and preparation method and application thereof |
-
2022
- 2022-04-21 CN CN202210416871.6A patent/CN114516750B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN114516750A (en) | 2022-05-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103145442B (en) | Method for preparing non-sintered ceramisites by using chemical sludge | |
| CN106904924B (en) | Utilize the system and method for municipal waste and Industrial Solid Waste building 3D printing material | |
| JP2020503225A (en) | Lightweight and high-strength ceramic particles and method for producing the same | |
| CN105906176B (en) | A method of recycling, which is total to, using greasy filth and solid waste prepares light ceramic | |
| CN103241970B (en) | Sintering expansion type light ceramsite produced by using oily sludge and manufacture method of sintering expansion type light ceramsite | |
| CN101962590B (en) | Regenerative coal produced by multiple kinds of oily sludge in oil refinery and preparation method thereof | |
| CN109111208B (en) | Iron tailing baked brick and preparation method thereof | |
| CN106746802B (en) | The system and method for sulphate aluminium cement is prepared using municipal waste and Industrial Solid Waste | |
| CN106810204B (en) | Fenton iron mud cathode and anode integrated ceramsite and method for preparing ceramsite by utilizing Fenton iron mud | |
| CN101955374A (en) | Method for manufacturing zeolite-glass porous light material | |
| CN103553702A (en) | Resource utilization method of residual sludge from petrochemical organic wastewater biological treatment | |
| CN108440013A (en) | A kind of biological aerated filter ceramic grain filter and preparation method thereof | |
| CN113480326A (en) | Method for preparing environment functional material by multi-source solid waste synergy | |
| CN114394800A (en) | Method for resource utilization of sludge biochar | |
| CN113943116A (en) | Process for producing high-alumina cement by using aluminum ash and fly ash generated after waste incineration | |
| CN112957927B (en) | Porous ceramic oil-water separation film taking red mud waste residues as raw materials and preparation method thereof | |
| CN104772214B (en) | A kind of method that fly ash highly removes ferrum | |
| CN114516750B (en) | Nano-micro porous ceramic based on oil-containing waste residue recycling and preparation method and application thereof | |
| CN103148489B (en) | Water-coal-slurry suspension fluidization burn processing discards oil base grout technique | |
| CN111995306A (en) | Non-fired ceramsite based on urban river sludge and regenerated garbage and preparation method thereof | |
| CN109695059B (en) | Preparation method of gypsum whisker | |
| CN111440644A (en) | Harmless recycling treatment method for oily sludge | |
| CN101423626B (en) | Method for preparing fly ash surface functionalized composite coating film layer | |
| CN102174070A (en) | Method for preparing composite foam concrete foaming agent and soil modifying agent by extracting microprotein from sludge through utilizing red mud | |
| Li et al. | Effect of additives on the properties of ceramsite from solid wastes |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |