CN106866115B - Preparation method of far infrared antibacterial ceramic - Google Patents

Preparation method of far infrared antibacterial ceramic Download PDF

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CN106866115B
CN106866115B CN201710164931.9A CN201710164931A CN106866115B CN 106866115 B CN106866115 B CN 106866115B CN 201710164931 A CN201710164931 A CN 201710164931A CN 106866115 B CN106866115 B CN 106866115B
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far infrared
slurry
xenotime
infrared antibacterial
vanadium
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CN106866115A (en
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邓怡
张珂玮
杨为中
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Sichuan University
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Sichuan University
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Abstract

The invention relates to a preparation method of far infrared antibacterial ceramics in the field of building materials, which comprises the steps of mixing vanadium-titanium waste residues, bastnaesite, cerite, xenotime, Minjiang clay, quartzite, calcite, sepiolite, kaolinite and limestone according to a formula, adding a slurry cosolvent to perform wet ball milling treatment to obtain slurry, and performing spray granulation, dry pressing molding, demolding and drying on the slurry to obtain a far infrared antibacterial ceramic product, wherein the formula comprises, by mass, 20-50% of the vanadium-titanium waste residues, 3-5% of the bastnaesite, 2-4% of the xenotime, 2-6% of the xenotime, 10-30% of Minjiang clay, 15-45% of the quartzite, 5-15% of the calcite, 2-6% of the sepiolite, 2-10% of the kaolinite and 4-8% of the limestone.

Description

Preparation method of far infrared antibacterial ceramic
Technical Field
The invention relates to the field of building materials, in particular to a preparation method of far infrared antibacterial ceramics.
Background
Compared with the traditional ion antibacterial ceramic, the ion antibacterial ceramic has the defects that the released metal ions (such as silver ions and the like) can kill bacteria and human body cells, and can cause adverse effects on human health after long-term use, the far infrared rays released by the far infrared antibacterial ceramic cause bacterial atom and molecular resonance to destroy the bioactivity, but can be well absorbed by a human body and converted into internal energy of organisms, activate biological macromolecules such as protein and the like, so that the biological cells are at the highest vibration level, the capillary vessels are expanded, the blood circulation is promoted, the metabolism among tissues is enhanced, the regeneration capacity of tissues is increased, and the immunity of the organisms is improved.
Disclosure of Invention
The invention aims to overcome the defects of low far infrared emissivity, poor sterilization effect, low ceramic strength and high cost of the existing far infrared antibacterial ceramic, and provides a preparation method of far infrared antibacterial ceramics, which has high far infrared emissivity, good sterilization effect, high ceramic strength and low cost.
The purpose of the invention is realized by the following technical scheme:
the preparation method of far infrared antibacterial ceramic is characterized in that vanadium-titanium waste residue, bastnaesite, phosphacerite, xenotime, Minjiang clay, quartzite, calcite, sepiolite, kaolinite and limestone are mixed according to a formula, a slurry cosolvent is added for wet ball milling treatment to obtain slurry, and the slurry is subjected to spray granulation, dry pressing molding, demolding and drying to obtain a far infrared antibacterial ceramic product; wherein the formula comprises the following components in percentage by mass: 20-50% of vanadium-titanium waste residues, 3-5% of bastnaesite, 2-4% of lanthanum phosphorite, 2-6% of xenotime, 10-30% of Minjiang clay, 15-45% of quartzite, 5-15% of calcite, 2-6% of sepiolite, 2-10% of kaolinite and 4-8% of limestone.
In the scheme, the chemical components of the vanadium-titanium waste residue mainly contain Fe in percentage by mass2O345～65%，SiO210～20%，TiO28～15%，Na2O 2～4%，Al2O34～8%，CaO 1～3%，MgO 1～2%。
In the above scheme, the chemical components of the bastnaesite mainly contain CeO in percentage by mass250～70%，SiO21～2%，CaO 3～7%，Fe2O32～5%。
In the scheme, the chemical components of the cerite lanthanum ore mainly contain CeO in percentage by mass215～25%，La2O330～45%，ThO210～15%，CaO 5～12%。
In the scheme, the chemical components of the xenotime mainly comprise Y in percentage by mass2O360%～85%，CeO25～12%，Er2O31～5%，SiO23～5%。
In the scheme, the slurry cosolvent is sodium tripolyphosphate, and the addition amount of the sodium tripolyphosphate is 2-3% of the slurry in percentage by mass.
In the scheme, the firing temperature is 1050-1200 ℃, the firing time is 2-5 h, and the heat preservation time is 5-30 min.
The preparation method of the far infrared antibacterial ceramic has the following beneficial effects:
(1) the far infrared antibacterial ceramic takes vanadium-titanium waste residues as main raw materials, not only greatly reduces the production cost of the far infrared ceramic, but also fully utilizes solid waste resources, reduces the harm of vanadium-titanium waste residue accumulation to the environment, simultaneously changes waste into valuable, has great economic benefit and social benefit, and meets the development requirements of establishing resources and energy-saving society in China.
(2) The vanadium-titanium waste residues in the raw materials required by the preparation of the far infrared antibacterial ceramic and the rare earth minerals are subjected to oxidation-reduction reaction at high temperature, so that the phenomena of valence change, rearrangement and mutual substitution of metal ions on lattice points are caused, and lattice distortion induces the generation of high infrared radiation performance. The prepared far infrared antibacterial ceramic has high far infrared emissivity (the far infrared emissivity in the wavelength range of 8-14 mu m is up to 90-95%), the resonance of molecules in bacteria can be effectively triggered by utilizing good far infrared radiation performance, and the heat effect generated by the friction among the molecules exceeds the bearable range of the bacteria, so that the sterilization effect (obvious bacteriostatic ring) is achieved. Meanwhile, far infrared rays released by the ceramic tiles can be well absorbed by a human body and converted into internal energy of an organism, and the ceramic tiles have the effects of activating histiocytes, preventing aging and strengthening an immune system. Compared with the traditional ion antibacterial ceramic, the ion antibacterial ceramic has the advantages of avoiding toxic and side effects on human bodies caused by ion antibacterial, and having stable and lasting antibacterial performance. The far infrared antibacterial agent can not only effectively kill bacteria, but also is beneficial to human health.
(3) According to the invention, natural silicate minerals are used as ceramic aggregates, and silicate ceramic substrates existing in vanadium-titanium waste residues are fully matched and utilized to form required oxides, so that the prepared far infrared antibacterial ceramic also has the characteristic of high strength (the breaking strength reaches 28-32 MPa), the use of the far infrared antibacterial ceramic in the field of buildings is effectively widened, and the performance requirements of large-scale building use can be met.
(4) The invention has simple process, low-temperature quick firing process (the firing temperature is reduced by about 50 ℃ compared with the prior art, the heat preservation time is reduced by about 30 min) is adopted in the firing system, the raw material cost is low (can be saved by more than 20 percent), and the invention is beneficial to realizing energy conservation, emission reduction and industrialization.
In conclusion, the invention overcomes the defects of low far infrared emissivity, poor sterilization effect, low ceramic strength and high cost of the existing far infrared antibacterial ceramic, and provides the preparation method of the far infrared antibacterial ceramic.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The present invention will be described in further detail in with reference to examples, but the present invention is not limited to these examples.
Example
The preparation method of the far infrared antibacterial ceramic comprises the following steps: by mass percentage, the vanadium-titanium waste residue is 30%, the bastnaesite is 3%, the monazite is 4%, the xenotime is 4%, the Minjiang clay is 15%, the quartzite is 25%, the calcite is 7%, the sepiolite is 3%, the kaolinite is 5%, and the limestone is 4%.
The chemical components of the vanadium-titanium waste residue mainly contain Fe in percentage by mass2O345～65%，SiO210～20%，TiO28～15%，Na2O 2～4%，Al2O34-8%, CaO 1-3%, MgO 1-2%, and the shape is any kinds or combination of several kinds of granular, sand or powder.
The chemical components of the bastnaesite mainly contain CeO in percentage by mass250～70%，SiO21～2%，CaO 3～7%，Fe2O32-5%, and any kinds or combination of several kinds of granular, sand or powder.
The chemical components of the monazite mainly comprise CeO in percentage by mass215～25%，La2O330～45%，ThO210～15%，CaO 5～12%The shape is any kinds or combination of several kinds of granular, sand-like or powder-like.
The chemical composition of the xenotime mainly comprises Y in percentage by mass2O360%～85%，CeO25～12%，Er2O31～5%，SiO23-5%, and the shape is any kinds or combination of several kinds of granular, sand or powder.
The process comprises the following steps:
(1) mixing the natural minerals and the vanadium-titanium waste residues according to the formula, adding a slurry cosolvent to perform wet ball milling treatment to obtain slurry with the ball milling fineness of 325 and the standard screen residue of 3.0 percent; the mud cosolvent is sodium tripolyphosphate, and the addition amount of the sodium tripolyphosphate is 2% of the slurry in percentage by mass.
(2) And carrying out spray granulation and dry pressing at 20MPa on the slurry to obtain a green body with the water content of 7%.
(3) And demolding the green body, drying at 100 ℃ for 80min, and then sintering at 1100 ℃ for 4h, and keeping the temperature for 20min to obtain the far infrared antibacterial ceramic product.
The performance indexes are as follows: far infrared emissivity (within 8-14 mu m): 0.89, antibacterial activity against Escherichia coli: presence of zone of inhibition, antibacterial activity against staphylococcus aureus: presence of bacteriostatic rings, flexural strength: 32.5 MPa.
The far infrared emissivity is measured by a Fourier far infrared converter and an infrared emissivity test carrying device thereof (FT-IR, NEXUS 670); the flexural strength was measured according to the national ceramic industry Standard (GB/T4100-2015).
Example two
The preparation method of the far infrared antibacterial ceramic comprises the following steps: by mass percent, 35 percent of vanadium-titanium waste residue, 4 percent of bastnaesite, 2 percent of monazite, 5 percent of xenotime, 17 percent of Minjiang clay, 19 percent of quartzite, 6 percent of calcite, 4 percent of sepiolite, 3 percent of kaolinite and 5 percent of limestone.
The process comprises the following steps:
(1) mixing the natural minerals and the vanadium-titanium waste residues according to the formula, adding a slurry cosolvent to perform wet ball milling treatment to obtain slurry with the ball milling fineness of 325 and the standard screen residue of 2.0 percent; the mud cosolvent is sodium tripolyphosphate, and the addition amount of the sodium tripolyphosphate is 3% of the slurry in percentage by mass.
(2) And carrying out spray granulation and dry pressing forming under 15MPa on the slurry to obtain a green body with the water content of 6%.
(3) And demolding the green body, drying at 105 ℃ for 100min, and then sintering at 1080 ℃ for 3.5h and keeping the temperature for 25min to obtain the far infrared antibacterial ceramic product.
The performance indexes are as follows: far infrared emissivity (within 8-14 mu m): 0.91, antibacterial activity against E.coli: presence of zone of inhibition, antibacterial activity against staphylococcus aureus: presence of bacteriostatic rings, flexural strength: 36.8 MPa.
The remainder of the description is the same as in example .
EXAMPLE III
The preparation method of the far infrared antibacterial ceramic comprises the following steps: by mass percentage, the vanadium-titanium waste residue is 30%, the bastnaesite is 5%, the monazite is 4%, the xenotime is 3%, the Minjiang clay is 10%, the quartzite is 25%, the calcite is 7%, the sepiolite is 2%, the kaolinite is 6%, and the limestone is 8%.
The process comprises the following steps:
(1) the natural minerals and the vanadium-titanium waste residues are mixed according to the formula, and then the slurry cosolvent is added for wet ball milling treatment, so that the ball milling fineness of the slurry is 325, and the standard screen residue is 5.0%.
(2) And carrying out spray granulation and dry pressing forming under 25MPa on the slurry to obtain a green body with the water content of 7%.
(3) And demolding the green body, drying at 120 ℃ for 90min, and then sintering at 1150 ℃ for 5h, and keeping the temperature for 15min to obtain the far infrared antibacterial ceramic product.
The performance indexes are as follows: far infrared emissivity (within 8-14 mu m): 0.90, antibacterial activity against Escherichia coli: presence of zone of inhibition, antibacterial activity against staphylococcus aureus: presence of bacteriostatic rings, flexural strength: 33.1 MPa.
The remainder of the description is the same as in example .
Example four
The preparation method of the far infrared antibacterial ceramic comprises the following steps: by mass percentage, the vanadium-titanium waste residue is 40%, the bastnaesite is 3%, the monazite is 2%, the xenotime is 6%, the Minjiang clay is 10%, the quartzite is 15%, the calcite is 6%, the sepiolite is 4%, the kaolinite is 7%, and the limestone is 7%.
The process comprises the following steps:
(1) the natural minerals and the vanadium-titanium waste residues are mixed according to the formula, and then the slurry cosolvent is added for wet ball milling treatment, so that the ball milling fineness of the slurry is 325, and the standard screen residue is 4.0%.
(2) And carrying out spray granulation and 10MPa dry pressing forming on the slurry to obtain a green body with the water content of 8%.
(3) And demolding the green body, drying at 100 ℃ for 80min, and sintering at 1200 ℃ for 4h, and keeping the temperature for 15min to obtain the far infrared antibacterial ceramic product.
The performance indexes are as follows: far infrared emissivity (within 8-14 mu m): 0.87, antibacterial activity against E.coli: presence of zone of inhibition, antibacterial activity against staphylococcus aureus: presence of bacteriostatic rings, flexural strength: 35.2 MPa.
The remainder of the description is the same as in example .
EXAMPLE five
The preparation method of the far infrared antibacterial ceramic comprises the following steps: by mass percent, the vanadium-titanium waste residue is 50 percent, the bastnaesite is 3 percent, the monazite is 2 percent, the xenotime is 2 percent, the Minjiang clay is 10 percent, the quartzite is 15 percent, the calcite is 5 percent, the sepiolite is 4 percent, the kaolinite is 2 percent, and the limestone is 7 percent.
The process comprises the following steps:
(1) the natural minerals and the vanadium-titanium waste residues are mixed according to the formula, and then the slurry cosolvent is added for wet ball milling treatment, so that the ball milling fineness of the slurry is 325, and the standard screen residue is 4.0%.
(2) And carrying out spray granulation and 10MPa dry pressing forming on the slurry to obtain a green body with the water content of 8%.
(3) And demolding the green body, drying at 100 ℃ for 80min, and sintering at 1050 ℃ for 5h and keeping the temperature for 30min to obtain the far infrared antibacterial ceramic product.
The performance indexes are as follows: far infrared emissivity (within 8-14 mu m): 0.92, antibacterial activity against E.coli: presence of zone of inhibition, antibacterial activity against staphylococcus aureus: presence of bacteriostatic rings, flexural strength: 40.6 MPa.
The remainder of the description is the same as in example .
EXAMPLE six
The preparation method of the far infrared antibacterial ceramic comprises the following steps: by mass percentage, the vanadium-titanium waste residue is 20%, the bastnaesite is 5%, the monazite is 4%, the xenotime is 6%, the Minjiang clay is 23%, the quartzite is 15%, the calcite is 15%, the sepiolite is 6%, the kaolinite is 2%, and the limestone is 4%.
The process comprises the following steps:
(1) the natural minerals and the vanadium-titanium waste residues are mixed according to the formula, and then the slurry cosolvent is added for wet ball milling treatment, so that the ball milling fineness of the slurry is 325, and the standard screen residue is 4.0%.
(2) And carrying out spray granulation and dry pressing under 20MPa on the slurry to obtain a green body with the water content of 8%.
(3) And demolding the green body, drying at 100 ℃ for 80min, and then sintering at 1150 ℃ for 2h, and keeping the temperature for 5min to obtain the far infrared antibacterial ceramic product.
The performance indexes are as follows: far infrared emissivity (within 8-14 mu m): 0.88, antibacterial activity against E.coli: presence of zone of inhibition, antibacterial activity against staphylococcus aureus: presence of bacteriostatic rings, flexural strength: 31.2 MPa.
The remainder of the description is the same as in example .
EXAMPLE seven
The preparation method of the far infrared antibacterial ceramic comprises the following steps: by mass percentage, the vanadium-titanium waste residue is 24%, the bastnaesite is 4%, the monazite is 3%, the xenotime is 4%, the Minjiang clay is 30%, the quartzite is 15%, the calcite is 5%, the sepiolite is 4%, the kaolinite is 5%, and the limestone is 6%.
The process comprises the following steps:
(1) the natural minerals and the vanadium-titanium waste residues are mixed according to the formula, and then the slurry cosolvent is added for wet ball milling treatment, so that the ball milling fineness of the slurry is 325, and the standard screen residue is 4.0%.
(2) And carrying out spray granulation and dry pressing under 20MPa on the slurry to obtain a green body with the water content of 8%.
(3) And demolding the green body, drying at 100 ℃ for 80min, and then sintering at 1150 ℃ for 3h, and keeping the temperature for 20min to obtain the far infrared antibacterial ceramic product.
The performance indexes are as follows: far infrared emissivity (within 8-14 mu m): 0.90, antibacterial activity against Escherichia coli: presence of zone of inhibition, antibacterial activity against staphylococcus aureus: presence of bacteriostatic rings, flexural strength: 33.7 MPa.
The remainder of the description is the same as in example .
Example eight
The preparation method of the far infrared antibacterial ceramic comprises the following steps: the vanadium-titanium waste residue is 21 percent, the bastnaesite is 4 percent, the monazite is 3 percent, the xenotime is 4 percent, the Minjiang clay is 10 percent, the quartzite is 45 percent, the calcite is 5 percent, the sepiolite is 2 percent, the kaolinite is 2 percent, and the limestone is 4 percent.
The process comprises the following steps:
(1) the natural minerals and the vanadium-titanium waste residues are mixed according to the formula, and then the slurry cosolvent is added for wet ball milling treatment, so that the ball milling fineness of the slurry is 325, and the standard screen residue is 4.0%.
(2) And carrying out spray granulation and dry pressing forming under 15MPa on the slurry to obtain a green body with the water content of 8%.
(3) And demolding the green body, drying at 100 ℃ for 80min, and then sintering at 1150 ℃ for 3h, and keeping the temperature for 20min to obtain the far infrared antibacterial ceramic product.
The performance indexes are as follows: far infrared emissivity (within 8-14 mu m): 0.88, antibacterial activity against E.coli: presence of zone of inhibition, antibacterial activity against staphylococcus aureus: presence of bacteriostatic rings, flexural strength: 36.5 MPa.
The remainder of the description is the same as in example .
Example nine
The preparation method of the far infrared antibacterial ceramic comprises the following steps: by mass percent, the vanadium-titanium waste residue is 29 percent, the bastnaesite is 4 percent, the monazite is 3 percent, the xenotime is 4 percent, the Minjiang clay is 15 percent, the quartzite is 20 percent, the calcite is 5 percent, the sepiolite is 4 percent, the kaolinite is 10 percent, and the limestone is 6 percent.
The process comprises the following steps:
(1) the natural minerals and the vanadium-titanium waste residues are mixed according to the formula, and then the slurry cosolvent is added for wet ball milling treatment, so that the ball milling fineness of the slurry is 325, and the standard screen residue is 4.0%.
(2) And carrying out spray granulation and 10MPa dry pressing forming on the slurry to obtain a green body with the water content of 8%.
(3) And demolding the green body, drying at 100 ℃ for 80min, and then sintering at 1150 ℃ for 3h, and keeping the temperature for 20min to obtain the far infrared antibacterial ceramic product.
The performance indexes are as follows: far infrared emissivity (within 8-14 mu m): 0.87, antibacterial activity against E.coli: presence of zone of inhibition, antibacterial activity against staphylococcus aureus: presence of bacteriostatic rings, flexural strength: 34.1 MPa.
The remainder of the description is the same as in example .

Claims (6)

  1. The preparation method of far infrared antibacterial ceramics is characterized by mixing vanadium-titanium waste residues, bastnaesite, phosphasite, xenotime, Minjiang clay, quartzite, calcite, sepiolite, kaolinite and limestone according to a formula, adding a slurry cosolvent to perform wet ball milling treatment to obtain slurry, and sintering the slurry after spray granulation, dry pressing molding, demolding and drying to obtain the far infrared antibacterial ceramic product, wherein the formula comprises, by mass, 20-50% of the vanadium-titanium waste residues, 3-5% of the bastnaesite, 2-4% of the xenotime, 2-6% of the xenotime, 10-30% of Minjiang clay, 15-45% of the quartzite, 5-15% of the calcite, 2-6% of the sepiolite, 2-10% of the kaolinite and 4-8% of the limestone, and the slurry cosolvent is sodium tripolyphosphate and the addition amount of the sodium tripolyphosphate is 2-3% of the slurry.
  2. 2. The method for preparing far-infrared antibacterial ceramics according to claim 1, characterized in that the chemical composition of the vanadium-titanium waste residue mainly contains Fe by mass percentage2O345～65％，SiO210～20％，TiO28～15％，Na2O 2～4％，Al2O34～8％，CaO 1～3％，MgO 1～2％。
  3. 3. The method for preparing far-infrared antibacterial ceramics according to claim 1, characterized in that the chemical composition of the bastnaesite mainly contains CeO in mass percentage250～70％，SiO21～2％，CaO 3～7％，Fe2O32～5％。
  4. 4. The method for preparing far infrared antibacterial ceramics according to claim 1, characterized in that the chemical composition of the monazite mainly contains CeO in mass percentage215～25％，La2O330～45％，ThO210～15％，CaO 5～12％。
  5. 5. The method for preparing far-infrared antibacterial ceramics according to claim 1, characterized in that the chemical composition of the xenotime mainly contains Y in mass percentage2O360％～85％，CeO25～12％，Er2O31～5％，SiO23～5％。
  6. 6. The method for preparing far infrared antibacterial ceramics according to claim 1, characterized in that the firing temperature is 1050 to 1200 ℃, the firing time is 2 to 5 hours, and the heat preservation time is 5 to 30 min.
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