CN115368113A - Method for recycling waste porcelain - Google Patents
Method for recycling waste porcelain Download PDFInfo
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- CN115368113A CN115368113A CN202211201168.XA CN202211201168A CN115368113A CN 115368113 A CN115368113 A CN 115368113A CN 202211201168 A CN202211201168 A CN 202211201168A CN 115368113 A CN115368113 A CN 115368113A
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- graphene oxide
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- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/1324—Recycled material, e.g. tile dust, stone waste, spent refractory material
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- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/04—Clay; Kaolin
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- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
-
- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/131—Inorganic additives
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- 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
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Abstract
The invention discloses a method for recycling waste porcelain, belonging to the technical field of ceramics; the method comprises the following steps: mixing and reacting the ceramic slurry, the graphene oxide and an acid solution, and then calcining; the mass ratio of the ceramic slurry to the graphene oxide is 5-6:1; the ceramic slurry comprises the following preparation raw materials in parts by mass: 100 parts of waste porcelain, 70-80 parts of kaolin, 25-30 parts of bentonite and 20-25 parts of ethyl orthosilicate; the calcining temperature is 1000-1200 ℃; the calcining atmosphere is a reducing atmosphere. The invention fixes other preparation raw materials through tetraethoxysilane; and reducing the graphene oxide into graphene by using a reducing atmosphere, so that the strength of the ceramic material is improved.
Description
Technical Field
The invention belongs to the technical field of ceramics, and particularly relates to a method for recycling waste porcelain.
Background
During the production of ceramics, a large amount of waste porcelain is produced every day. The method for treating the waste domestic porcelain in the related technology is to perform landfill treatment or use the waste domestic porcelain after crushing as building filler; the waste household porcelain is subjected to landfill treatment, a large amount of land resources are occupied, and the waste household porcelain is difficult to naturally degrade due to high sintering degree, namely, the soil structure can be damaged and the ground surface can be settled after the landfill treatment; the waste daily porcelain powder is used as building filler after being crushed, and the strength of the waste daily porcelain powder is found to be low in the using process and can only be used as building filler of a common road; if the pore-forming agent is added, the waste domestic porcelain is produced into porous ceramic which is used as a light building material; however, the porous ceramics in the related art have low porosity and low strength.
Therefore, the invention provides a method for recycling waste porcelain, which improves the strength of the porcelain.
Disclosure of Invention
The present invention has been made to solve at least one of the problems and disadvantages of the related art, and it is an object of the present invention to provide a method for recycling waste porcelain.
The invention provides a method for recycling waste porcelain, which comprises the following steps:
mixing and reacting the ceramic slurry, the graphene oxide and an acid solution, and calcining;
the mass ratio of the ceramic slurry to the graphene oxide is 5-6:1;
the ceramic slurry comprises the following preparation raw materials in parts by mass:
100 parts of waste porcelain, 70-80 parts of kaolin, 25-30 parts of bentonite and 20-25 parts of ethyl orthosilicate;
the calcining temperature is 1000-1200 ℃;
the calcining atmosphere is a reducing atmosphere.
According to one technical scheme of the waste porcelain recycling method, the method at least comprises the following steps
Has the advantages that:
according to the method, rich oxygen-containing functional groups are contained on the surface of the graphene oxide, so that the graphene oxide plays a role in connection in the hydrolysis process of the ethyl orthosilicate, and the graphene oxide is uniformly dispersed in sol formed after the ethyl orthosilicate is hydrolyzed; meanwhile, the ethyl orthosilicate and the waste porcelain, the kaolin and the bentonite in the ceramic slurry are fully mixed to form sol, so that the waste porcelain, the kaolin and the bentonite are fixed, and the preparation raw materials of the ceramic material are fully dispersed and fixed; therefore, the uniformity among the preparation raw materials is good in the calcining process.
In addition, the graphene oxide is reduced into graphene by utilizing a reducing atmosphere, so that the strength of the ceramic material is improved.
The invention also controls the calcining temperature, and realizes the molding of the ceramic material by controlling the calcining temperature.
According to some embodiments of the invention, the graphene oxide has a particle size of 5 μm to 20 μm.
The dispersion difficulty of the graphene oxide in the later reaction process is increased due to the overlarge granularity of the graphene oxide; resulting in poor uniformity; the too small particle size of the graphene oxide can result in poor carrying capacity of the graphene oxide on the ceramic slurry, so that uniform dispersion of the ceramic slurry cannot be realized, and the performance of the final ceramic material is affected.
According to some embodiments of the invention, the temperature of the reaction is between 70 ℃ and 80 ℃.
If the reaction temperature is too low, the reaction speed is too slow; and the reaction temperature is too high, the reaction rate is too fast, and the tetrabutyl silane is hydrolyzed too fast, so that the dispersion effect of the ceramic slurry and the graphene oxide is influenced, and the performance of the calcined ceramic is influenced.
According to some embodiments of the invention, the pH of the reaction is between 1 and 3.
If the pH is too low, the hydrolysis speed of the tetraethoxysilane is too slow; if the pH is too high, the hydrolysis rate of the tetraethoxysilane is too high, thereby affecting the uniformity of the reaction system.
According to some embodiments of the invention, the reaction time is 1h to 3h.
According to some embodiments of the invention, the calcination is for a time period of 1h to 2h.
According to some embodiments of the present invention, the raw material for preparing the ceramic slurry further includes 50 to 60 parts of ethanol.
According to some embodiments of the invention, the ceramic slurry comprises the following preparation raw materials in parts by weight:
100 parts of waste porcelain, 70-80 parts of kaolin, 25-30 parts of bentonite, 20-25 parts of ethyl orthosilicate and 50-60 parts of ethanol.
According to some embodiments of the invention, the waste porcelain is waste household porcelain.
In the invention, the dissolubility of the ethyl orthosilicate is improved by adding the ethanol, so that the ethyl orthosilicate is fully mixed with other raw materials in the ceramic slurry.
According to some embodiments of the invention, the ceramic slurry is subjected to a grinding process; the fineness of the ceramic slurry after grinding treatment is 10-20 mu m.
According to some embodiments of the invention, the kaolin has an oil absorption number of 100 to 140.
According to some embodiments of the invention, the kaolin has a particle size (D50) in the range of 0.5 μm to 1 μm.
According to some embodiments of the invention, the acid solution comprises at least one of a hydrochloric acid and an acetic acid solution.
According to some embodiments of the invention, the acid solution has a molar concentration of 0.5mol/L to 1.5mol/L.
The acid solution plays a role in dispersing graphene oxide, and if the concentration of the acid is too high, the dispersion effect of the graphene oxide is affected; and the hydrolysis rate of the tetraethoxysilane is influenced by the excessively low concentration of the acid.
According to some embodiments of the invention, the reducing gas consists of a protective gas and hydrogen.
According to some embodiments of the invention, the volume fraction of hydrogen in the reducing gas is between 5% and 20%.
According to some embodiments of the invention, the volume fraction of hydrogen in the reducing gas is between 5% and 10%.
According to some embodiments of the invention, the protective gas comprises at least one of nitrogen and a noble gas.
According to some embodiments of the invention, the graphene oxide is dispersed in water to form a graphene oxide solution.
According to some embodiments of the invention, the graphene oxide solution has a graphene oxide mass concentration of 5mg/mL to 10mg/mL.
According to some embodiments of the invention, the method for recycling waste porcelain comprises the following steps:
and mixing and reacting the ceramic slurry, the acid solution and the graphene oxide solution, and calcining.
According to some embodiments of the invention, the ceramic slurry is added to the graphene oxide solution to form a first mixture; the acid solution is then added to the first mixture for reaction.
According to some embodiments of the invention, the method for recycling waste porcelain comprises the following steps:
s1, adding the ceramic slurry into the graphene oxide dispersion liquid for dispersion to obtain a first mixture;
s2, adding the acid solution into the first mixture for dispersing, heating for reaction after the dispersion is finished, and preparing a second mixture after the reaction is finished;
and S3, calcining the second mixture.
According to some embodiments of the invention, the speed of dispersion in step S1 is between 300r/min and 500r/min.
According to some embodiments of the invention, the time of said dispersing in step S1 is between 20min and 40min.
According to some embodiments of the invention, the speed of dispersion in step S2 is between 300r/min and 500r/min.
According to some embodiments of the invention, the time of said dispersing in step S2 is between 20min and 40min.
According to some embodiments of the invention, the dispersion rate during the temperature-increasing reaction in step S2 is 300r/min to 500r/min.
Detailed Description
The idea of the invention and the resulting technical effects will be clearly and completely described below in connection with the embodiments, so that the objects, features and effects of the invention can be fully understood. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and other embodiments obtained by those skilled in the art without inventive efforts are within the protection scope of the present invention based on the embodiments of the present invention.
In the description of the present invention, reference to the description of the terms "one embodiment," "some embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples," etc., means 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, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. 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 embodiment does not indicate specific conditions, and the method is performed according to conventional conditions or conditions suggested by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
The graphene oxide used in the embodiment of the present invention was obtained from HGP-50 (particle size of 50 μm), HGP-20 (particle size of 18 μm), HGP-10 (particle size of 8 μm) and HGP-3A (particle size of 3 μm) of Qingdao rock-ocean carbon materials, inc.
Waste household porcelain: the Hunan China Union porcelain industry, inc. waste daily porcelain.
Kaolin: neoGen 2000 from Chenjin materials science and technology, D50 is 0.7 μm, and oil absorption value is 120.
Bentonite: lingshou county Hongrun mineral processing factory.
CAS number for ethyl orthosilicate is: 78-10-4.
The CAS number of butyl orthosilicate is: 4766-57-8.
Example 1
The embodiment is a method for recycling waste porcelain, which comprises the following steps:
s1, preparation of raw materials:
adding 1g of graphene oxide (HGP-10) to water to form a graphene oxide dispersion (7.5 mg/mL);
preparing ceramic slurry, wherein the ceramic slurry is prepared from the following preparation raw materials in parts by weight:
100 parts of waste household porcelain, 75 parts of kaolin, 30 parts of bentonite, 25 parts of ethyl orthosilicate and 50 parts of ethanol.
Mixing the preparation raw materials of the ceramic slurry, and then grinding the mixture by using a horizontal grinder, wherein the fineness of the ceramic slurry after grinding is 10-20 microns;
s2, firing ceramic:
adding the ceramic slurry prepared in the step S1 into the graphene oxide dispersion liquid, and dispersing for 30min at a stirring speed of 400r/min; preparing a first mixture;
wherein the mass ratio of the graphene oxide to the ceramic slurry in the graphene oxide dispersion liquid is 5:1;
adding 1mol/L hydrochloric acid into the first mixture, and dispersing for 30min at a stirring speed of 400r/min; then raising the temperature to 60 ℃ for reaction for 3h, wherein the stirring speed in the reaction process is 400r/min; preparing a second mixture after the reaction is finished;
calcining the second mixture at 1200 ℃ for 2h; the atmosphere for calcination was a mixture of nitrogen and hydrogen (5% by volume of hydrogen).
Example 2
The present embodiment is a method for recycling waste porcelain, and the difference from embodiment 1 is that: graphene oxide (HGP-20) was used in this example.
Example 3
The present embodiment is a method for recycling waste porcelain, and the difference from embodiment 1 is that: in this example, graphene oxide (HGP-50) was used.
Example 4
The present embodiment is a method for recycling waste porcelain, and the difference from embodiment 1 is that: in this example, graphene oxide (HGP-3A) was used.
Example 5
The present embodiment is a method for recycling waste porcelain, and the difference from embodiment 1 is that: in this embodiment, the mass ratio of the graphene oxide to the ceramic slurry in the graphene oxide dispersion liquid is 6:1.
Example 6
This example is a method for recycling waste porcelain, and the difference from example 1 is that: the atmosphere for calcination in this example was a mixed gas of nitrogen and hydrogen (the volume fraction of hydrogen is 10%).
Example 7
The present embodiment is a method for recycling waste porcelain, and the difference from embodiment 1 is that: the atmosphere for calcination in this example was a mixture of nitrogen and hydrogen (20% by volume of hydrogen).
Example 8
This example is a method for recycling waste porcelain, and the difference from example 1 is that: the present embodiment is a method for recycling waste porcelain, and the difference from embodiment 1 is that: the atmosphere for calcination in this example was a mixed gas of nitrogen and hydrogen (hydrogen in a volume fraction of 2%).
Comparative example 1
The comparative example is a method for recycling waste porcelain, and is different from the example 1 in that: in this comparative example, ethyl orthosilicate was replaced with butyl orthosilicate.
Comparative example 2
The comparative example is a method for recycling waste porcelain, and the difference from the example 1 is that: in the comparative example, the mass ratio of the graphene oxide to the ceramic slurry in the graphene oxide dispersion liquid is 4:1.
Comparative example 3
The comparative example is a method for recycling waste porcelain, and is different from the example 1 in that: in the comparative example, the mass ratio of the graphene oxide to the ceramic slurry in the graphene oxide dispersion liquid is 7:1.
Comparative example 4
The comparative example is a method for recycling waste porcelain, and is different from the example 1 in that: the temperature of calcination in this comparative example was 800 ℃.
Comparative example 5
The comparative example is a method for recycling waste porcelain, and the difference from the example 1 is that: the comparative example is a method for recycling waste porcelain, and the difference from the example 1 is that: the temperature of calcination in this comparative example was 1300 ℃.
The test standard for the compressive strength of the ceramic materials in examples 1 to 8 of the present invention and comparative examples 1 to 5 is as follows: GB/T4740-1999.
The results of the compressive strength tests of the ceramic materials of examples 1 to 8 of the present invention and comparative examples 1 to 5 are shown in Table 1.
TABLE 1 compression Strength test results of ceramic materials in inventive examples 1 to 8 and comparative examples 1 to 5
The difference between embodiment 1 of the present invention and embodiments 2 to 4 is that: the particle size of the graphene; from the data in table 1 it follows: the particle size of the graphene is controlled within a certain range, so that the performance of the ceramic material is further improved.
The difference between example 1 of the present invention and example 5 and comparative examples 2 to 3 is that: the mass ratio of graphene oxide to ceramic slurry was different, and it was found from the data in table 1 that: the mass ratio of the graphene oxide to the ceramic slurry is controlled within a certain range, so that the performance of the ceramic material is further improved.
The difference between embodiment 1 of the present invention and embodiments 6 to 8 is that: the volume fraction of hydrogen in the calcination atmosphere varied and is known from the data in table 1: the volume fraction of the hydrogen is controlled within a certain range, which is beneficial to further improving the performance of the ceramic material.
The difference between example 1 of the present invention and comparative examples 4 to 5 is that: the temperature of the calcination is known from the data in table 1: the calcination temperature is controlled within a certain range, which is beneficial to further improving the performance of the ceramic material.
In summary, the graphene oxide surface contains rich oxygen-containing functional groups, so that the graphene oxide surface plays a role in connection in the hydrolysis process of the tetraethoxysilane, and the graphene oxide is uniformly dispersed in the sol formed after the tetraethoxysilane is hydrolyzed; meanwhile, the ethyl orthosilicate and the waste porcelain, the kaolin and the bentonite in the ceramic slurry are fully mixed to form sol, so that the waste porcelain, the kaolin and the bentonite are fixed, and the preparation raw materials of the ceramic material are fully dispersed and fixed; therefore, in the calcining process, the uniformity among the preparation raw materials is good. In addition, the graphene oxide is reduced into graphene by utilizing a reducing atmosphere, so that the strength of the ceramic material is improved. The invention also controls the calcining temperature, and realizes the molding of the ceramic material by controlling the calcining temperature.
The above-mentioned embodiments, objects, technical solutions and advantages of the present invention are further described in detail, it should be understood that the above-mentioned embodiments are only examples of the present invention, and should not be construed as limiting the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for recycling waste porcelain is characterized by comprising the following steps:
mixing and reacting the ceramic slurry, the graphene oxide and an acid solution, and calcining;
the mass ratio of the ceramic slurry to the graphene oxide is 5-6:1;
the ceramic slurry comprises the following preparation raw materials in parts by mass:
100 parts of waste porcelain, 70-80 parts of kaolin, 25-30 parts of bentonite and 20-25 parts of ethyl orthosilicate;
the calcining temperature is 1000-1200 ℃;
the calcining atmosphere is a reducing atmosphere.
2. The method for recycling waste porcelain according to claim 1, wherein the graphene oxide is 5 to 20 μm in size.
3. The method of claim 1, wherein the reaction temperature is 70 ℃ to 80 ℃.
4. The method of recycling waste porcelain according to claim 1, wherein the reaction has a pH of 1 to 3.
5. The method for recycling waste porcelain according to claim 1, wherein the reaction time is 1 to 3 hours.
6. The method for recycling waste porcelain according to claim 1, wherein the calcination time is 1 to 2 hours.
7. The method for recycling waste porcelain according to claim 1, wherein the raw material for preparing the ceramic slurry further comprises 50 to 60 parts of ethanol.
8. The method for recycling waste porcelain according to claim 6, wherein the ceramic slurry is subjected to grinding treatment; the fineness of the ceramic slurry after grinding treatment is 10-20 mu m.
9. The method of recycling waste porcelain according to any one of claims 1 to 8, wherein the acid solution includes at least one of hydrochloric acid and acetic acid solution.
10. The method of claim 9, wherein the molar concentration of the acid solution is 0.5mol/L to 1.5mol/L.
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