CN116063094A - Formula and method for preparing ceramic particles from slag and refuse factory incineration slag - Google Patents

Formula and method for preparing ceramic particles from slag and refuse factory incineration slag Download PDF

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CN116063094A
CN116063094A CN202310137484.3A CN202310137484A CN116063094A CN 116063094 A CN116063094 A CN 116063094A CN 202310137484 A CN202310137484 A CN 202310137484A CN 116063094 A CN116063094 A CN 116063094A
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slag
ceramic particles
parts
refuse
particles
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陈伟光
陈永晖
陈艺文
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Jiangmen Yujia Technology Co ltd
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Jiangmen Yujia Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/009Porous or hollow ceramic granular materials, e.g. microballoons
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/14Shaped 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 silica
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62204Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427Silicates other than clay, e.g. water glass
    • C04B2235/3463Alumino-silicates other than clay, e.g. mullite
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/349Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
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    • C04B2235/77Density
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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    • Y02P40/60Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes

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Abstract

The invention discloses a formula and a method for preparing ceramic particles by utilizing slag and refuse factory incineration slag, which relate to the field of ceramic particles, wherein the ceramic particles are prepared by weighing materials according to the weight parts of each component in the formula, uniformly mixing the materials in a ball milling mode, ageing and homogenizing the materials, then performing spray drying, granulating the materials and a binder into particles together, grading or air-flow grading the particles in a stirring fluidized bed by utilizing a bag filter, drying the particles and then sintering the particles in a kiln to obtain ceramic particles, thereby solving the environmental pollution caused by a large amount of slag and refuse factory incineration slag, and fully recycling and reutilizing waste resources; the production and preparation consume a large amount of slag and waste incineration slag of a garbage factory, effectively relieve environmental pollution, and fully recycle and reuse waste resources; by generating chemical bonds and physical adsorption, stress is transferred in the compression shearing process to block the sliding among the polymer chain segments, so that the bonding strength is improved, and the aim of improving the mechanical property is fulfilled.

Description

Formula and method for preparing ceramic particles from slag and refuse factory incineration slag
Technical Field
The invention relates to the field of ceramic particles, in particular to a formula and a method for preparing ceramic particles by utilizing slag and refuse factory incinerator slag.
Background
With the rapid development of urban process of social economy in China and the rapid improvement of the living standard of people, the waste generated in the incineration slag of slag and garbage factories is also increased rapidly, the environmental pollution and the influence on the health of people are also more obvious, the great increase of the incineration slag of slag and garbage factories makes the garbage treatment more and more difficult, and the problems of environmental pollution and the like caused by the great increase of the incineration slag of slag and garbage factories gradually bring about the wide attention of all social circles, so the industrialization, recycling, reduction and harmlessness of the incineration slag of slag and garbage factories are urgently needed to be realized, the environmental pollution is reduced, and the environmental protection standard is achieved.
Ceramic particles have advantages of low density, high strength, abrasion resistance and corrosion resistance, and from the viewpoints of a relatively simple manner, low cost and capability of mass production of ceramic products, a dry high pressure molding method has been used as a method for producing ceramic products, and when ceramic products are produced by this method, ceramic particles are usually granulated into ceramic particles, and for the purposes of easy transportation of powder, filling and workability of molding, etc., there are two popular methods for granulating ceramic particles, one method (spray drying method) is to spray-dry an aqueous slurry comprising a ceramic material, a binder and water with a spray dryer to produce ceramic particles, and the other method (vibration extrusion method) is to granulate ceramic particles into ceramic particles by repeated drying and vibration extrusion.
The spray drying process allows for a very convenient control of the particle distribution, which is suitable for producing a large number of ceramic particles having a relatively small particle size, whereas the vibration extrusion process can be operated very conveniently, which is suitable for producing relatively dense particles in a small-scale plant, from which the granulation is appropriately selected, depending on the molded product to be produced, the shaping die used, the production scale, etc.
However, the ceramic particles prepared at present have the problems that the segregation, solidification or partial conversion of the binder into fine particles is caused by long-term storage or distillation of water, so that certain properties such as fluidity, crushing property under low pressure or anti-adhesion property of the ceramic particles are changed during production, and the toughness of the ceramic particles is poor, so that the ceramic particles are not suitable for high-strength equipment and operation process, and the product performance is easily reduced.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a formula and a method for preparing ceramic particles by using slag and refuse factory incineration slag, wherein the formula comprises the following steps:
weighing the materials according to the weight parts of the components in the formula, uniformly mixing the materials by a ball milling mode, ageing and homogenizing, performing spray drying after ageing and homogenizing, granulating the materials and the binder into particles, grading or air-current grading in a stirring fluidized bed by using a bag filter, feeding hot air into the stirring fluidized bed, drying, sintering in a kiln, discharging from the kiln, processing to obtain ceramic particles, solving the environmental pollution caused by a large amount of slag and refuse factory incineration slag, and fully recycling and reutilizing waste resources;
adding 3, 4-diaminodiphenyl ether into a three-neck flask, adding dry 3,3', 4' -benzophenone tetracarboxylic dianhydride to obtain an intermediate A, uniformly mixing SiO2 and B4C, adding a silane coupling agent to obtain an intermediate B, adding the intermediate B into the intermediate A, and stirring to obtain the binder, thereby solving the problems that the conventional ceramic particles can not meet the high temperature resistance requirement due to segregation, solidification or partial conversion of the binder into fine particles, and the crushing performance or anti-adhesion performance of the ceramic particles under low pressure caused by long-term storage or distillation action of water, and solving the problem that the plasticizer has high temperature defects;
mixing triisopropylphenyl phosphate and phosphorus pentoxide in a round-bottom flask, then dripping absolute ethyl alcohol to obtain an intermediate C, mixing 12-hydroxystearic acid, glacial acetic acid and phosphoric acid in the round-bottom flask, dripping hydrogen peroxide, washing to neutrality by using distilled water to obtain an intermediate D, dissolving the intermediate D in solvent toluene, adding a reaction bottle, mixing the solvent toluene, the intermediate C and triphenylphosphine, dripping the mixture into the reaction bottle, and titrating the reaction mixture with a sodium hydroxide standard solution until the pH value is 7 to obtain the plasticizer, thereby solving the problems that the toughness of the existing ceramic particles is poor, the ceramic particles are not suitable for high-strength equipment and operation processes, and the product performance is easy to be reduced.
The aim of the invention can be achieved by the following technical scheme:
a formula for preparing ceramic particles by utilizing slag and refuse factory incineration slag comprises the following components in parts by weight:
60.0-70.0 parts of sand, 1.0-2.0 parts of bentonite, 3.0-5.0 parts of raw mineral mud, 1.0-2.0 parts of feldspar, 50.0-70.0 parts of slag and waste incineration slag of a garbage factory, 9.0-10.0 parts of porcelain sand and 2-5 parts of plasticizer;
the ceramic particles are prepared by the following steps:
s1: weighing the materials according to the weight parts of the components in the formula, uniformly mixing the materials by a ball milling mode, and then aging and homogenizing the materials;
s2: after ageing and homogenizing, spray drying to obtain powder, granulating the powder and binder together into granules, and classifying in a stirring fluidized bed or air-flow classification by using a bag filter to remove fine particles with particle size not more than 10-15 μm;
s3: the hot air with the temperature of 50-80 ℃ is supplied to a stirring type fluidized bed, the temperature of the stirring type fluidized bed is regulated to be in the range of 20-50 ℃, and the stirring type fluidized bed is dried and then is put into a kiln for sintering, wherein the sintering atmosphere is a reducing atmosphere, and the sintering temperature is 1050-1250 ℃;
s4: and taking out of the kiln, and after the ceramic particles are cooled, processing the ceramic particles to obtain the ceramic particles.
As a further scheme of the invention: the slag and garbage factory incineration slag comprises the following components in percentage by mass: 14-17 parts of silicon dioxide, 9-11 parts of aluminum oxide, 54.5-58 parts of ferric oxide, 8.4-11 parts of titanium dioxide, 2.5-3.8 parts of calcium oxide, 0.51-0.63 part of magnesium oxide, 0.07-0.09 part of potassium oxide and 4-6 parts of sodium oxide.
As a further scheme of the invention: the mass of the binder in the step S2 is 2-3% of the mass of the powder.
As a further scheme of the invention: the preparation steps of the binder in the step S2 are as follows:
s41: adding 3, 4-diaminodiphenyl ether into a three-neck flask, controlling the temperature at 15-25 ℃, adding solvent N, N-dimethylacetamide, stirring under the protection of nitrogen, adding dried 3,3', 4' -benzophenone tetracarboxylic dianhydride, and mechanically stirring for 12-24 hours to obtain an intermediate A;
s42: uniformly mixing SiO2 and B4C, adding a silane coupling agent, adding solvent ethanol, stirring for 2-3h, ultrasonically dispersing for 1-1.5h, and drying in a drying oven at 75-95 ℃ for 5-6h to obtain an intermediate B;
s43: adding the intermediate B into the intermediate A, stirring for 1-2h, heating to 200-220 ℃ at the speed of 5-10 ℃/min, preserving heat for 1-2h, heating to 280-300 ℃ at the speed of 1-3 ℃/min, preserving heat for 3-5h, and naturally cooling to room temperature to obtain the adhesive.
As a further scheme of the invention: the molar ratio of the 3, 4-diaminodiphenyl ether to the 3,3', 4' -benzophenone tetracarboxylic dianhydride in the step S41 is 1.2 to 1.3:1.
as a further scheme of the invention: the dosage ratio of SiO2, B4C and the silane coupling agent in the step S42 is 5g:10g:1g, the ratio of the amount of the intermediate A to the amount of the intermediate B in the step S43 is 1g:1g.
As a further scheme of the invention: the plasticizer is prepared by the following steps:
s71: mixing triisopropylphenyl phosphate and phosphorus pentoxide in a round bottom flask with a mechanical stirrer, a thermometer and a constant pressure dropping funnel, stirring at 60-70 ℃ for 2-3 hours to generate a polymeric phosphate intermediate, then dripping absolute ethyl alcohol, controlling the dripping speed to be 1-2 drops/s, and continuing to react at 100-110 ℃ for 18-20 hours to obtain an intermediate C;
s72: mixing 12-hydroxystearic acid, glacial acetic acid and phosphoric acid in a round bottom flask with a mechanical stirrer, a thermometer and a constant pressure dropping funnel, dripping hydrogen peroxide in 30-60 min, controlling the dripping speed to be 1-2 drops/s, stirring at 50-60 ℃ for reaction for 4-6h, washing with distilled water to be neutral, and distilling at 60-70 ℃ under reduced pressure to obtain an intermediate D;
s73: dissolving the intermediate D in toluene solvent, adding the toluene solvent into a reaction bottle, mixing the toluene solvent, the intermediate C solvent and triphenylphosphine at 45-50 ℃, dripping the mixture into the reaction bottle within 30-60mi n, controlling the dripping speed to be 1-2 drops/s, reacting for 5-8h at 75-90 ℃, titrating the reaction mixture with a sodium hydroxide standard solution until the pH value is 7, and distilling at 65-80 ℃ under reduced pressure to obtain the plasticizer.
As a further scheme of the invention: the dosage ratio of the triisopropylphenyl phosphate, the phosphorus pentoxide and the absolute ethyl alcohol in the step S71 is 150.5g:28.2g:50mL.
As a further scheme of the invention: the dosage ratio of the 12-hydroxystearic acid, the glacial acetic acid, the phosphoric acid and the hydrogen peroxide in the step S72 is 89.6g:14g:1g:50mL of the ratio of intermediate D, intermediate C to triphenylphosphine in step S73 was 98.3g: intermediate a:0.1g.
A preparation method for preparing ceramic particles by utilizing slag and refuse factory incineration slag comprises the following steps:
s1: weighing the materials according to the weight parts of the components in the formula, uniformly mixing the materials by a ball milling mode, and then aging and homogenizing the materials;
s2: after ageing and homogenizing, spray drying to obtain powder, granulating the powder and binder together into granules, and classifying in a stirring fluidized bed or air-flow classification by using a bag filter to remove fine particles with particle size not more than 10-15 μm;
s3: the hot air with the temperature of 50-80 ℃ is supplied to a stirring type fluidized bed, the temperature of the stirring type fluidized bed is regulated to be in the range of 20-50 ℃, and the stirring type fluidized bed is dried and then is put into a kiln for sintering, wherein the sintering atmosphere is a reducing atmosphere, and the sintering temperature is 1050-1250 ℃;
s4: and taking out of the kiln, and after the ceramic particles are cooled, processing the ceramic particles to obtain the ceramic particles.
The invention has the beneficial effects that:
the invention is to weigh the materials according to the weight proportion of each component in the formula, mix them evenly by ball milling, then age and homogenize, spray-dry after aging and homogenize, granulate into particles with binder, use the bag filter to carry on classification or air classification in the stirring fluid bed, through supplying the hot air to the stirring fluid bed, enter the kiln to burn after drying, exit the kiln, process, get the ceramic particles, consume a large amount of slag and refuse factory incinerator slag through production and preparation, relieve the environmental pollution effectively, fully recycle and reuse the waste resources;
adding 3, 4-diaminodiphenyl ether into a three-neck flask, adding dry 3,3', 4' -benzophenone tetracarboxylic dianhydride to obtain an intermediate A, uniformly mixing SiO2 and B4C, adding a silane coupling agent to obtain an intermediate B, adding the intermediate B into the intermediate A, stirring to obtain the binder, uniformly dispersing nano Si 02 with small size into a matrix, performing dispersion strengthening function in the matrix, absorbing impact energy in the matrix, thereby enhancing mechanical properties of a system, acting as physical adsorption and chemical reaction active points of the system, establishing firm connection between a polymer molecular chain and the nano active points, and transmitting stress in a compression shearing process by generating a chemical bond and physical adsorption mode to prevent slippage between polymer chain segments so as to improve bonding strength;
mixing triisopropylphenyl phosphate and phosphorus pentoxide in a round-bottom flask, then dripping absolute ethyl alcohol to obtain an intermediate C, mixing 12-hydroxystearic acid, glacial acetic acid and phosphoric acid in the round-bottom flask, dripping hydrogen peroxide, washing to neutrality by using distilled water to obtain an intermediate D, dissolving the intermediate D in solvent toluene, adding a reaction bottle, mixing the solvent toluene, the intermediate C and triphenylphosphine, dripping the mixture into the reaction bottle, and titrating the reaction mixture with a sodium hydroxide standard solution until the pH value is 7 to obtain the plasticizer, wherein the molecular structure contains more convertible functional groups, so that the toughness of ceramic particles is effectively improved, and the aim of improving the mechanical property is fulfilled.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
the embodiment is a formula for preparing ceramic particles by utilizing slag and refuse factory incineration slag, and the formula comprises the following components in parts by weight:
60.0 parts of sand, 1.0 part of bentonite, 3.0 parts of raw mineral mud, 1.0 part of feldspar, 50.0 parts of slag and garbage factory incinerator slag, 9.0 parts of porcelain sand and 2 parts of plasticizer;
the ceramic particles are prepared by the following steps:
s1: weighing the materials according to the weight parts of the components in the formula, uniformly mixing the materials by a ball milling mode, and then aging and homogenizing the materials;
s2: after ageing and homogenizing, spray drying to prepare powder, granulating the powder and a binder together into particles, and classifying in a stirring fluidized bed or air-flow classification by using a bag filter so as to remove fine particles with the particle size not more than 10 mu m;
s3: the method comprises the steps of supplying hot air at 80 ℃ to a stirring type fluidized bed, adjusting the temperature of the stirring type fluidized bed to 50 ℃, drying, and sintering in a kiln, wherein the sintering atmosphere is a reducing atmosphere, and the sintering temperature is 1250 ℃;
s4: taking out of the kiln, and after the ceramic particles are cooled, processing to obtain ceramic particles;
the preparation steps of the adhesive are as follows:
s41: adding 3, 4-diaminodiphenyl ether into a three-neck flask, controlling the temperature at 15 ℃, adding solvent N, N-dimethylacetamide, stirring under the protection of nitrogen, adding dried 3,3', 4' -benzophenone tetracarboxylic dianhydride, and mechanically stirring for 12 hours to obtain an intermediate A;
s42: uniformly mixing SiO2 and B4C, adding a silane coupling agent, adding solvent ethanol, stirring for 2 hours, performing ultrasonic dispersion for 1 hour, and transferring to a drying oven at 75 ℃ for drying for 6 hours to obtain an intermediate B;
s43: adding the intermediate B into the intermediate A, stirring for 1h, heating to 200 ℃ at the rate of 5 ℃/min, preserving heat for 1h, heating to 280 ℃ at the rate of 1 ℃/min, preserving heat for 3h, and naturally cooling to room temperature to obtain the adhesive;
the plasticizer is prepared by the following steps:
s71: mixing triisopropylphenyl phosphate and phosphorus pentoxide in a round-bottom flask with a mechanical stirrer, a thermometer and a constant pressure dropping funnel, stirring at 60 ℃ for reaction for 2 hours to generate a polyphosphate intermediate, then dripping absolute ethyl alcohol, controlling the dripping speed to be 1 drop/s, and continuing to react at 100 ℃ for 20 hours to obtain an intermediate C;
s72: mixing 12-hydroxystearic acid, glacial acetic acid and phosphoric acid in a round bottom flask with a mechanical stirrer, a thermometer and a constant pressure dropping funnel, dripping hydrogen peroxide in 30 min, controlling the dripping speed to be 1 drop/s, stirring at 50 ℃ for reaction for 4 hours, washing with distilled water to be neutral, and distilling at 60 ℃ under reduced pressure to obtain an intermediate D;
s73: dissolving the intermediate D in toluene solvent, adding the toluene solvent into a reaction bottle, mixing the toluene solvent, the intermediate C solvent and triphenylphosphine at 45 ℃, dripping the mixture into the reaction bottle within 30 min, controlling the dripping speed to be 1 drop/s, reacting for 5 hours at 75 ℃, titrating the reaction mixture with a sodium hydroxide standard solution until the pH value is 7, and distilling at 65 ℃ under reduced pressure to obtain the plasticizer.
Example 2:
the embodiment is a formula for preparing ceramic particles by utilizing slag and refuse factory incineration slag, and the formula comprises the following components in parts by weight:
60.0 parts of sand, 2.0 parts of bentonite, 5.0 parts of raw mineral mud, 2.0 parts of feldspar, 50.0 parts of slag and waste incineration slag of a garbage factory, 10.0 parts of porcelain sand and 2 parts of plasticizer;
the ceramic particles are prepared by the following steps:
s1: weighing the materials according to the weight parts of the components in the formula, uniformly mixing the materials by a ball milling mode, and then aging and homogenizing the materials;
s2: after ageing and homogenizing, spray drying to prepare powder, granulating the powder and a binder together into particles, and classifying in a stirring fluidized bed or air-flow classification by using a bag filter so as to remove fine particles with the particle size not more than 10 mu m;
s3: the hot air at 50 ℃ is supplied to a stirring type fluidized bed, the temperature of the stirring type fluidized bed is regulated to be within the range of 50 ℃, and the stirring type fluidized bed is dried and then is put into a kiln for sintering, wherein the sintering atmosphere is a reducing atmosphere, and the sintering temperature is 1250 ℃;
s4: taking out of the kiln, and after the ceramic particles are cooled, processing to obtain ceramic particles;
the preparation steps of the adhesive are as follows:
s41: adding 3, 4-diaminodiphenyl ether into a three-neck flask, controlling the temperature at 15 ℃, adding solvent N, N-dimethylacetamide, stirring under the protection of nitrogen, adding dried 3,3', 4' -benzophenone tetracarboxylic dianhydride, and mechanically stirring for 12 hours to obtain an intermediate A;
s42: uniformly mixing SiO2 and B4C, adding a silane coupling agent, adding solvent ethanol, stirring for 2 hours, performing ultrasonic dispersion for 1 hour, and transferring to a drying oven at 75 ℃ for drying for 5 hours to obtain an intermediate B;
s43: adding the intermediate B into the intermediate A, stirring for 1h, heating to 200 ℃ at the rate of 5 ℃/min, preserving heat for 1h, heating to 280 ℃ at the rate of 1 ℃/min, preserving heat for 3h, and naturally cooling to room temperature to obtain the adhesive;
the plasticizer is prepared by the following steps:
s71: mixing triisopropylphenyl phosphate and phosphorus pentoxide in a round-bottom flask with a mechanical stirrer, a thermometer and a constant pressure dropping funnel, stirring at 70 ℃ for reaction for 3 hours to generate a polyphosphate intermediate, then dripping absolute ethyl alcohol, controlling the dripping speed to be 2 drops/s, and continuing to react at 110 ℃ for 20 hours to obtain an intermediate C;
s72: mixing 12-hydroxystearic acid, glacial acetic acid and phosphoric acid in a round bottom flask with a mechanical stirrer, a thermometer and a constant pressure dropping funnel, dripping hydrogen peroxide in 60 min, controlling the dripping speed to be 2 drops/s, stirring at 60 ℃ for reaction for 6h, washing with distilled water to be neutral, and distilling at 70 ℃ under reduced pressure to obtain an intermediate D;
s73: dissolving the intermediate D in toluene solvent, adding the toluene solvent into a reaction bottle, mixing the toluene solvent, the intermediate C solvent and triphenylphosphine at 50 ℃, dripping the mixture into the reaction bottle within 60mi < n >, controlling the dripping speed to be 2 drops/s, reacting for 8 hours at 90 ℃, titrating the reaction mixture with a sodium hydroxide standard solution until the pH value is 7, and distilling at 80 ℃ under reduced pressure to obtain the plasticizer.
Example 3:
the embodiment is a formula for preparing ceramic particles by utilizing slag and refuse factory incineration slag, and the formula comprises the following components in parts by weight:
70.0 parts of sand, 2.0 parts of bentonite, 5.0 parts of raw mineral mud, 2.0 parts of feldspar, 70.0 parts of slag and waste incineration slag of a garbage factory, 10.0 parts of porcelain sand and 5 parts of plasticizer;
the ceramic particles are prepared by the following steps:
s1: weighing the materials according to the weight parts of the components in the formula, uniformly mixing the materials by a ball milling mode, and then aging and homogenizing the materials;
s2: after ageing and homogenizing, spray drying to prepare powder, granulating the powder and a binder together into particles, and classifying in a stirring fluidized bed or air-flow classification by using a bag filter so as to remove fine particles with the particle size not more than 15 mu m;
s3: the method comprises the steps of supplying hot air at 80 ℃ to a stirring type fluidized bed, adjusting the temperature of the stirring type fluidized bed to 50 ℃, drying, and sintering in a kiln, wherein the sintering atmosphere is a reducing atmosphere, and the sintering temperature is 1250 ℃;
s4: taking out of the kiln, and after the ceramic particles are cooled, processing to obtain ceramic particles;
the preparation steps of the adhesive are as follows:
s41: adding 3, 4-diaminodiphenyl ether into a three-neck flask, controlling the temperature at 25 ℃, adding solvent N, N-dimethylacetamide, stirring under the protection of nitrogen, adding dried 3,3', 4' -benzophenone tetracarboxylic dianhydride, and mechanically stirring for 24 hours to obtain an intermediate A;
s42: uniformly mixing SiO2 and B4C, adding a silane coupling agent, adding solvent ethanol, stirring for 3 hours, ultrasonically dispersing for 1.5 hours, and drying for 6 hours in a drying oven at 95 ℃ to obtain an intermediate B;
s43: adding the intermediate B into the intermediate A, stirring for 2h, heating to 220 ℃ at the rate of 10 ℃/min, preserving heat for 2h, heating to 300 ℃ at the rate of 3 ℃/min, preserving heat for 5h, and naturally cooling to room temperature to obtain the adhesive;
the plasticizer is prepared by the following steps:
s71: mixing triisopropylphenyl phosphate and phosphorus pentoxide in a round-bottom flask with a mechanical stirrer, a thermometer and a constant pressure dropping funnel, stirring at 70 ℃ for reaction for 3 hours to generate a polyphosphate intermediate, then dripping absolute ethyl alcohol, controlling the dripping speed to be 2 drops/s, and continuing to react at 110 ℃ for 20 hours to obtain an intermediate C;
s72: mixing 12-hydroxystearic acid, glacial acetic acid and phosphoric acid in a round bottom flask with a mechanical stirrer, a thermometer and a constant pressure dropping funnel, dripping hydrogen peroxide in 60 min, controlling the dripping speed to be 2 drops/s, stirring at 60 ℃ for reaction for 6h, washing with distilled water to be neutral, and distilling at 70 ℃ under reduced pressure to obtain an intermediate D;
s73: dissolving the intermediate D in toluene solvent, adding the toluene solvent into a reaction bottle, mixing the toluene solvent, the intermediate C solvent and triphenylphosphine at 50 ℃, dripping the mixture into the reaction bottle within 60mi < n >, controlling the dripping speed to be 2 drops/s, reacting for 8 hours at 90 ℃, titrating the reaction mixture with a sodium hydroxide standard solution until the pH value is 7, and distilling at 80 ℃ under reduced pressure to obtain the plasticizer.
Comparative example 1:
comparative example 1 differs from example 1 in that no binder was added.
Comparative example 2:
comparative example 2 used commercially available ceramic particles.
The ceramic particles of examples 1-3 and comparative examples 1-2 were tested;
the test results are shown in the following table:
sample of Density/(g cm) 3 ) Forming pressure/ton (ton cm) -2 )
Example 1 3.4 3.9
Example 2 3.4 3.8
Implementation of the embodimentsExample 3 3.4 3.8
Comparative example 1 2.8 1.3
Comparative example 2 3.0 2.5
As is clear from the above table, the density of the examples reached 3.4 g.cm 3 The density of comparative example 1 was 2.8 g.cm 3 The density of comparative example 2 was 3.0g cm 3 The molding pressure of the examples reached 3.8-3.9 tons cm -2 The molding pressure of comparative example 1 was 1.3 ton cm -2 The molding pressure of comparative example 2 was 2.5 tons cm -2 All data of the examples are better than those of the comparative examples, which shows that the ceramic particles prepared by the invention have more excellent mechanical properties.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.

Claims (10)

1. The formula for preparing the ceramic particles by utilizing slag and refuse factory incineration slag is characterized by comprising the following components in parts by weight:
60.0-70.0 parts of sand, 1.0-2.0 parts of bentonite, 3.0-5.0 parts of raw mineral mud, 1.0-2.0 parts of feldspar, 50.0-70.0 parts of slag and waste incineration slag of a garbage factory, 9.0-10.0 parts of porcelain sand and 2-5 parts of plasticizer;
the ceramic particles are prepared by the following steps:
s1: weighing the materials according to the weight parts of the components in the formula, uniformly mixing the materials by a ball milling mode, and then aging and homogenizing the materials;
s2: after ageing and homogenizing, spray drying to prepare powder, granulating the powder and a binder together into particles, and classifying in a stirring fluidized bed or air classification by using a bag filter;
s3: the hot air is supplied to a stirring fluidized bed, and the fluidized bed is dried and then put into a kiln for sintering, wherein the sintering atmosphere is a reducing atmosphere;
s4: and taking out of the kiln, and after the ceramic particles are cooled, processing the ceramic particles to obtain the ceramic particles.
2. The formula for preparing ceramic particles by using slag and refuse-derived incineration slag according to claim 1, wherein the slag and refuse-derived incineration slag comprise the following components in percentage by mass: 14-17 parts of silicon dioxide, 9-11 parts of aluminum oxide, 54.5-58 parts of ferric oxide, 8.4-11 parts of titanium dioxide, 2.5-3.8 parts of calcium oxide, 0.51-0.63 part of magnesium oxide, 0.07-0.09 part of potassium oxide and 4-6 parts of sodium oxide.
3. The formulation for preparing ceramic particles from slag and refuse-derived incineration slag according to claim 1, wherein the mass of the binder in step S2 is 2-3% of the mass of the powder.
4. The formulation for preparing ceramic particles from slag and refuse-derived incineration slag according to claim 1, wherein the binder preparation step in step S2 is as follows:
s41: adding 3, 4-diaminodiphenyl ether into a three-neck flask, adding a solvent N, N-dimethylacetamide, and adding dried 3,3', 4' -benzophenone tetracarboxylic dianhydride to obtain an intermediate A;
s42: siO is made of 2 And B 4 Mixing uniformly, adding a silane coupling agent, adding solvent ethanol, stirring, performing ultrasonic dispersion, and transferring to a drying oven for drying to obtain an intermediate B;
s43: intermediate B was added to intermediate a and stirred to obtain the binder.
5. The formulation for preparing ceramic particles from slag and refuse-derived incineration slag according to claim 4, wherein the molar ratio of 3, 4-diaminodiphenyl ether to 3,3', 4' -benzophenone tetracarboxylic dianhydride in step S41 is 1.2 to 1.3:1.
6. the formulation for preparing ceramic particles from slag and refuse-derived incinerator slag as claimed in claim 4, wherein said SiO in step S42 is as follows 2 、B 4 The dosage ratio of C to the silane coupling agent is 5g:10g:1g, the ratio of the amount of the intermediate A to the amount of the intermediate B in the step S43 is 1g:1g.
7. A formulation for preparing ceramic particles from slag and refuse-derived incineration slag according to claim 1, characterised in that the plasticiser is obtained by the following preparation steps:
s71: mixing triisopropylphenyl phosphate and phosphorus pentoxide in a round-bottom flask to generate a polymeric phosphate intermediate, and then dripping absolute ethyl alcohol to obtain an intermediate C;
s72: mixing 12-hydroxystearic acid, glacial acetic acid and phosphoric acid in a round bottom flask, dripping hydrogen peroxide, and washing with distilled water to neutrality to obtain an intermediate D;
s73: intermediate D is dissolved in solvent toluene and added into a reaction bottle, after the solvent toluene, intermediate C and triphenylphosphine are mixed, the mixture is dripped into the reaction bottle, and the reaction mixture is titrated with sodium hydroxide standard solution until the pH value is 7, so that the plasticizer is obtained.
8. The formulation for preparing ceramic particles from slag and refuse-derived incineration slag according to claim 7, wherein the dosage ratio of triisopropylphenyl phosphate, phosphorus pentoxide and absolute ethanol in step S71 is 150.5g:28.2g:50mL.
9. The formulation for preparing ceramic particles from slag and refuse-derived incineration slag according to claim 7, wherein the ratio of the amounts of 12-hydroxystearic acid, glacial acetic acid, phosphoric acid and hydrogen peroxide in step S72 is 89.6g:14g:1g:50mL of the ratio of intermediate D, intermediate C to triphenylphosphine in step S73 was 98.3g: intermediate a:0.1g.
10. A method for producing ceramic particles from slag and refuse-derived incinerator slag according to any one of claims 1 to 9, comprising the steps of:
s1: weighing the materials according to the weight parts of the components in the formula, uniformly mixing the materials by a ball milling mode, and then aging and homogenizing the materials;
s2: after ageing and homogenizing, spray drying to prepare powder, granulating the powder and a binder together into particles, and classifying in a stirring fluidized bed or air classification by using a bag filter;
s3: the hot air is supplied to a stirring fluidized bed, and the fluidized bed is dried and then put into a kiln for sintering, wherein the sintering atmosphere is a reducing atmosphere;
s4: and taking out of the kiln, and after the ceramic particles are cooled, processing the ceramic particles to obtain the ceramic particles.
CN202310137484.3A 2023-02-20 2023-02-20 Formula and method for preparing ceramic particles from slag and refuse factory incineration slag Pending CN116063094A (en)

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Publication number Priority date Publication date Assignee Title
CN103435330A (en) * 2013-08-19 2013-12-11 佛山市亮剑陶瓷有限公司 Anti-static ceramic material manufactured by vanadium slags and manufacturing method thereof,
US20200048147A1 (en) * 2017-04-19 2020-02-13 Qingdao Yi Eco-Environmental Protection Technology Co. Ltd Method for preparing ceramsite by using municipal sludge as raw material
CN113477926A (en) * 2021-07-20 2021-10-08 扬州金鑫管业有限公司 Production process of high-performance ceramic lining composite steel pipe
CN114736473A (en) * 2022-05-19 2022-07-12 江苏正康新材料科技股份有限公司 Environment-friendly degradable PVC floor and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103435330A (en) * 2013-08-19 2013-12-11 佛山市亮剑陶瓷有限公司 Anti-static ceramic material manufactured by vanadium slags and manufacturing method thereof,
US20200048147A1 (en) * 2017-04-19 2020-02-13 Qingdao Yi Eco-Environmental Protection Technology Co. Ltd Method for preparing ceramsite by using municipal sludge as raw material
CN113477926A (en) * 2021-07-20 2021-10-08 扬州金鑫管业有限公司 Production process of high-performance ceramic lining composite steel pipe
CN114736473A (en) * 2022-05-19 2022-07-12 江苏正康新材料科技股份有限公司 Environment-friendly degradable PVC floor and preparation method thereof

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