CN114477279A - Green preparation method of nano titanium dioxide - Google Patents
Green preparation method of nano titanium dioxide Download PDFInfo
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- CN114477279A CN114477279A CN202210063182.1A CN202210063182A CN114477279A CN 114477279 A CN114477279 A CN 114477279A CN 202210063182 A CN202210063182 A CN 202210063182A CN 114477279 A CN114477279 A CN 114477279A
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- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 90
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 56
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000012798 spherical particle Substances 0.000 claims abstract description 37
- 239000000243 solution Substances 0.000 claims abstract description 34
- 238000005507 spraying Methods 0.000 claims abstract description 32
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 30
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 26
- 229920000742 Cotton Polymers 0.000 claims abstract description 22
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 229920002678 cellulose Polymers 0.000 claims abstract description 14
- 239000001913 cellulose Substances 0.000 claims abstract description 14
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000001856 Ethyl cellulose Substances 0.000 claims abstract description 13
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000012501 ammonium carbonate Nutrition 0.000 claims abstract description 13
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 229920001249 ethyl cellulose Polymers 0.000 claims abstract description 13
- 235000019325 ethyl cellulose Nutrition 0.000 claims abstract description 13
- 239000011780 sodium chloride Substances 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000009718 spray deposition Methods 0.000 claims abstract description 7
- 239000000725 suspension Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 24
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 238000000034 method Methods 0.000 claims 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 239000004408 titanium dioxide Substances 0.000 abstract description 4
- 238000009833 condensation Methods 0.000 abstract description 2
- 230000005494 condensation Effects 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000000413 hydrolysate Substances 0.000 abstract description 2
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 238000007789 sealing Methods 0.000 abstract description 2
- 238000009827 uniform distribution Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000005003 food packaging material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000005348 self-cleaning glass Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses a green preparation method of nano titanium dioxide, which comprises the following steps: adding n-butyl titanate into anhydrous ether, adding sodium chloride and ammonium carbonate to obtain a suspension, and extruding and granulating at constant temperature to obtain spherical particles; adding ethyl cellulose into ethanol and ethyl ether to form a cellulose alcohol solution, uniformly spraying the cellulose alcohol solution on spherical particles, drying, placing the coated spherical particles into a reaction kettle for constant-temperature reaction, adding a mixed solution of glycerol and ethanol for ultrasonic treatment, filtering and washing to obtain filter cotton; and (3) putting the filter cotton into anhydrous ether for low-temperature ultrasonic treatment, and performing spray deposition to obtain the nano titanium dioxide. The uniform and stable distribution of the n-butyl titanate in the spherical particles is realized through dispersion, wrapping and fixation, and the uniform distribution of the hydrolysate in the filter cotton is realized through the sealing of the spherical particles and in-situ hydrolysis, so that the nano-scale titanium dioxide with uniform particles is formed. The solvent of the whole preparation process can be recovered in a lossless manner, the solvent can be recycled, the environment is protected, and the recovery mode belongs to cooling condensation recovery.
Description
Technical Field
The invention belongs to the technical field of nano material preparation methods, and particularly relates to a green preparation method of nano titanium dioxide.
Background
The nano titanium dioxide has excellent optical property and shows good development prospect in various fields. The nanometer titanium dioxide also has high chemical stability, thermal stability, super-hydrophilicity and non-migration property, so the nanometer titanium dioxide is widely applied to the fields of ultraviolet-resistant materials, textiles, photocatalysis catalysts, self-cleaning glass, sun cream, coatings, printing ink, food packaging materials, paper industry and the like. The existing main preparation method has the problems of uneven product particle size, non-environment-friendly preparation process and the like.
Disclosure of Invention
The invention aims to provide a green preparation method of nano titanium dioxide, which is used for forming nano titanium dioxide with uniform particles.
The invention adopts the technical scheme that the green preparation method of the nano titanium dioxide is implemented according to the following steps:
step 1, adding tetrabutyl titanate into anhydrous ether, and uniformly stirring to form a stable dissolved solution;
step 2, adding sodium chloride and ammonium carbonate into the dissolved solution, and uniformly stirring to obtain a suspension; then extruding and granulating at constant temperature to obtain spherical particles;
step 3, adding ethyl cellulose into the mixed solution of ethanol and ether, uniformly stirring to form a cellulose alcohol solution, uniformly spraying the cellulose alcohol solution on the spherical particles, and drying to obtain coated spherical particles;
step 4, placing the coated spherical particles into a reaction kettle for constant-temperature reaction, then adding the coated spherical particles into a mixed solution of glycerol and ethanol for ultrasonic treatment, filtering and washing by adopting ethanol to obtain filter cotton;
and 5, putting the filter cotton into anhydrous ether for low-temperature ultrasonic treatment, taking out the filter cotton, and performing spray deposition on the solution to obtain the nano titanium dioxide.
The present invention is also characterized in that,
in the step 1, the concentration of the n-butyl titanate in the anhydrous ether is 100-200 g/L.
In the step 2, the addition amount of the sodium chloride is 80-90% of the mass of the n-butyl titanate, the addition amount of the ammonium carbonate is 28-35% of the mass of the n-butyl titanate, the stirring speed is 1000-2000r/min, the temperature of the constant-temperature extrusion granulation is 40-45 ℃, and the pressure is 0.3-0.5 MPa.
In the step 3, the concentration of the ethyl cellulose in the mixed solution of the ethanol and the ether is 100-200g/L, and the volume ratio of the ethanol to the ether is 1: 3-4; the uniform spraying temperature is 40-50 deg.C, and the spraying amount is 10-30mL/cm2The drying temperature is 40-50 ℃.
In the step 4, the constant temperature reaction temperature is 90-100 ℃, the time is 30-50min, and the pressure is 0.4-0.7 MPa; the volume ratio of glycerol to ethanol is 1:3-5, the ultrasonic treatment frequency is 70-90kHz, the ultrasonic treatment time is 30-50min, and the temperature is 40-60 ℃.
In the step 5, the ultrasonic temperature is 5-10 ℃, the ultrasonic time is 60-90min, and the ultrasonic frequency is 50-80 kHz; the spraying temperature is 60-90 deg.C, and the spraying amount is 20-40 mL/min.
The invention has the beneficial effects that: the uniform and stable distribution of the n-butyl titanate in the spherical particles is realized through dispersion, wrapping and fixation, and favorable conditions are created for avoiding agglomeration of the subsequent products. The uniform distribution of the hydrolysate in the filter cotton is realized through the steps of spherical particle sealing, in-situ hydrolysis and the like, and the nano-scale titanium dioxide with uniform particles is formed through washing, desorption and solution spraying. In addition, the solvent in the whole preparation process can be recycled, so that the double effects of saving cost and protecting environment can be realized.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments.
The invention relates to a green preparation method of nano titanium dioxide, which is implemented according to the following steps:
step 1, adding tetrabutyl titanate into anhydrous ether, and uniformly stirring to form a stable dissolved solution;
the concentration of the n-butyl titanate in the anhydrous ether is 100-200 g/L;
step 2, adding sodium chloride and ammonium carbonate into the dissolved solution, and uniformly stirring to obtain a suspension; then extruding and granulating at constant temperature to obtain spherical particles;
the adding amount of sodium chloride is 80-90% of the mass of the n-butyl titanate, the adding amount of ammonium carbonate is 28-35% of the mass of the n-butyl titanate, the stirring speed is 1000-;
step 3, adding ethyl cellulose into the mixed solution of ethanol and ether, uniformly stirring to form a cellulose alcohol solution, uniformly spraying the cellulose alcohol solution on the spherical particles, and drying to obtain coated spherical particles;
mixing ethyl cellulose in ethanol and diethyl etherThe concentration of the solution is 100-200g/L, and the volume ratio of the ethanol to the ether is 1: 3-4; the temperature of uniform spraying is 40-50 deg.C, and the spraying amount is 10-30mL/cm2The drying temperature is 40-50 ℃;
step 4, placing the coated spherical particles into a reaction kettle for constant-temperature reaction for 30-50min, then adding the coated spherical particles into a mixed solution of glycerol and ethanol for ultrasonic treatment for 30-50min, filtering and washing with ethanol to obtain filter cotton;
the constant temperature reaction temperature is 90-100 ℃, the pressure is 0.4-0.7MPa, the volume ratio of glycerol to ethanol is 1:3-5, the ultrasonic treatment temperature is 70-90kHz, and the temperature is 40-60 ℃;
step 5, putting the filter cotton into anhydrous ether, performing low-temperature ultrasonic treatment for 60-90min, taking out the filter cotton, and performing spray deposition on the solution to obtain nano titanium dioxide;
the temperature of low temperature ultrasonic treatment is 5-10 deg.C, the frequency of ultrasonic treatment is 50-80kHz, the temperature of spraying is 60-90 deg.C, and the spraying amount is 20-40 mL/min.
The solvent can be recovered in a lossless manner and recycled, and the recovery mode belongs to cooling condensation recovery.
Example 1
The invention relates to a green preparation method of nano titanium dioxide, which is implemented according to the following steps:
step 1, adding tetrabutyl titanate into anhydrous ether, and uniformly stirring to form a stable dissolved solution;
the concentration of the n-butyl titanate in the anhydrous ether is 100 g/L;
step 2, adding sodium chloride and ammonium carbonate into the dissolved solution, and uniformly stirring to obtain a suspension; then extruding and granulating at constant temperature to obtain spherical particles;
the adding amount of sodium chloride is 80 percent of the mass of the n-butyl titanate, the adding amount of ammonium carbonate is 28 percent of the mass of the n-butyl titanate, the stirring speed is 1000r/min, the temperature of constant-temperature extrusion granulation is 40 ℃, and the pressure is 0.3 MPa;
step 3, adding ethyl cellulose into the mixed solution of ethanol and ether, uniformly stirring to form a cellulose alcohol solution, uniformly spraying the cellulose alcohol solution on the spherical particles, and drying to obtain coated spherical particles;
the concentration of the ethyl cellulose in the mixed solution of the ethanol and the ether is 100g/L, and the volume ratio of the ethanol to the ether is 1: 3; the temperature of the uniform spraying is 40 ℃, and the spraying amount is 10mL/cm2The drying temperature is 40 ℃;
step 4, placing the coated spherical particles into a reaction kettle for constant-temperature reaction for 30min, then adding the coated spherical particles into a mixed solution of glycerol and ethanol for ultrasonic treatment for 30min, filtering and washing with ethanol to obtain filter cotton;
the constant temperature reaction temperature is 90 ℃, the pressure is 0.4MPa, and the volume ratio of the glycerol to the ethanol is 1:3, the temperature of ultrasonic treatment is 70kHz and 40 ℃;
step 5, putting the filter cotton into anhydrous ether, performing low-temperature ultrasonic treatment for 60min, taking out the filter cotton, and performing spray deposition on the solution to obtain nano titanium dioxide;
the temperature of low-temperature ultrasonic treatment is 5 ℃, the frequency of ultrasonic treatment is 50kHz, the temperature of spraying is 60 ℃, and the spraying amount is 20 mL/min.
Example 2
The invention relates to a green preparation method of nano titanium dioxide, which is implemented according to the following steps:
step 1, adding tetrabutyl titanate into anhydrous ether, and uniformly stirring to form a stable dissolved solution;
the concentration of the n-butyl titanate in the anhydrous ether is 150 g/L;
step 2, adding sodium chloride and ammonium carbonate into the dissolved solution, and uniformly stirring to obtain a suspension; then extruding and granulating at constant temperature to obtain spherical particles;
the adding amount of sodium chloride is 85 percent of the mass of the n-butyl titanate, the adding amount of ammonium carbonate is 30 percent of the mass of the n-butyl titanate, the stirring speed is 1500r/min, the temperature of constant-temperature extrusion granulation is 45 ℃, and the pressure is 0.4 MPa;
step 3, adding ethyl cellulose into the mixed solution of ethanol and ether, uniformly stirring to form a cellulose alcohol solution, uniformly spraying the cellulose alcohol solution on the spherical particles, and drying to obtain coated spherical particles;
the concentration of ethyl cellulose in the mixed solution of ethanol and ether is 150 g-L, the volume ratio of ethanol to ether is 1: 4; the temperature of the uniform spraying is 45 ℃, and the spraying amount is 20mL/cm2The drying temperature is 45 ℃;
step 4, placing the coated spherical particles into a reaction kettle for constant-temperature reaction for 40min, then adding the coated spherical particles into a mixed solution of glycerol and ethanol for ultrasonic treatment for 40min, filtering and washing with ethanol to obtain filter cotton;
the constant temperature reaction temperature is 95 ℃, the pressure is 0.5MPa, and the volume ratio of the glycerol to the ethanol is 1: 4, the temperature of ultrasonic treatment is 80kHz and 50 ℃;
step 5, putting the filter cotton into anhydrous ether, performing low-temperature ultrasonic treatment for 70min, taking out the filter cotton, and performing spray deposition on the solution to obtain nano titanium dioxide;
the temperature of low-temperature ultrasonic treatment is 8 ℃, the frequency of ultrasonic treatment is 60kHz, the temperature of spraying is 70 ℃, and the spraying amount is 30 mL/min.
Example 3
The invention relates to a green preparation method of nano titanium dioxide, which is implemented according to the following steps:
step 1, adding tetrabutyl titanate into anhydrous ether, and uniformly stirring to form a stable dissolved solution;
the concentration of the n-butyl titanate in the anhydrous ether is 200 g/L;
step 2, adding sodium chloride and ammonium carbonate into the dissolved solution, and uniformly stirring to obtain a suspension; then extruding and granulating at constant temperature to obtain spherical particles;
the adding amount of sodium chloride is 90 percent of the mass of the n-butyl titanate, the adding amount of ammonium carbonate is 35 percent of the mass of the n-butyl titanate, the stirring speed is 2000r/min, the temperature of constant-temperature extrusion granulation is 45 ℃, and the pressure is 0.5 MPa;
step 3, adding ethyl cellulose into the mixed solution of ethanol and ether, uniformly stirring to form a cellulose alcohol solution, uniformly spraying the cellulose alcohol solution on the spherical particles, and drying to obtain coated spherical particles;
the concentration of the ethyl cellulose in the mixed solution of the ethanol and the ether is 200g/L, and the volume ratio of the ethanol to the ether is 1: 4; the temperature of the uniform spraying is 50 ℃, and the spraying amount is 30mL/cm2The drying temperature is 50 ℃;
step 4, placing the coated spherical particles into a reaction kettle for reacting for 50min at a constant temperature, then adding the coated spherical particles into a mixed solution of glycerol and ethanol for ultrasonic treatment for 50min, filtering and washing with ethanol to obtain filter cotton;
the constant temperature reaction temperature is 100 ℃, the pressure is 0.7MPa, and the volume ratio of the glycerol to the ethanol is 1: 5, the temperature of ultrasonic treatment is 90kHz and 60 ℃;
step 5, putting the filter cotton into anhydrous ether, performing low-temperature ultrasonic treatment for 90min, taking out the filter cotton, and performing spray deposition on the solution to obtain nano titanium dioxide;
the temperature of low-temperature ultrasonic treatment is 10 ℃, the frequency of ultrasonic treatment is 80kHz, the temperature of spraying is 90 ℃, and the spraying amount is 40 mL/min.
Claims (6)
1. The green preparation method of the nano titanium dioxide is characterized by comprising the following steps:
step 1, adding tetrabutyl titanate into anhydrous ether, and uniformly stirring to form a stable dissolved solution;
step 2, adding sodium chloride and ammonium carbonate into the dissolved solution, and uniformly stirring to obtain a suspension; then extruding and granulating at constant temperature to obtain spherical particles;
step 3, adding ethyl cellulose into the mixed solution of ethanol and ether, uniformly stirring to form a cellulose alcohol solution, uniformly spraying the cellulose alcohol solution on the spherical particles, and drying to obtain coated spherical particles;
step 4, placing the coated spherical particles into a reaction kettle for constant-temperature reaction, then adding the coated spherical particles into a mixed solution of glycerol and ethanol for ultrasonic treatment, filtering and washing by adopting ethanol to obtain filter cotton;
and 5, putting the filter cotton into anhydrous ether for low-temperature ultrasonic treatment, taking out the filter cotton, and performing spray deposition on the solution to obtain the nano titanium dioxide.
2. The method as claimed in claim 1, wherein in step 1, the concentration of n-butyl titanate in anhydrous ether is 100-200 g/L.
3. The green preparation method of nano titanium dioxide as claimed in claim 1, wherein in the step 2, the addition amount of sodium chloride is 80-90% of the mass of n-butyl titanate, the addition amount of ammonium carbonate is 28-35% of the mass of n-butyl titanate, the stirring speed is 1000-2000r/min, the temperature of constant temperature extrusion granulation is 40-45 ℃, and the pressure is 0.3-0.5 MPa.
4. The method as claimed in claim 1, wherein in the step 3, the concentration of the ethyl cellulose in the mixed solution of ethanol and ether is 100-200g/L, and the volume ratio of ethanol to ether is 1: 3-4; the uniform spraying temperature is 40-50 deg.C, and the spraying amount is 10-30mL/cm2The drying temperature is 40-50 ℃.
5. The green preparation method of nano titanium dioxide according to claim 1, characterized in that in the step 4, the constant temperature reaction temperature is 90-100 ℃, the time is 30-50min, and the pressure is 0.4-0.7 MPa; the volume ratio of glycerol to ethanol is 1:3-5, the ultrasonic treatment frequency is 70-90kHz, the ultrasonic treatment time is 30-50min, and the temperature is 40-60 ℃.
6. The green preparation method of nano titanium dioxide according to claim 1, wherein in the step 5, the ultrasonic temperature is 5-10 ℃, the time is 60-90min, and the frequency is 50-80 kHz; the spraying temperature is 60-90 deg.C, and the spraying amount is 20-40 mL/min.
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| CN112871162A (en) * | 2021-02-22 | 2021-06-01 | 浙江工业大学上虞研究院有限公司 | Preparation method of mesoporous ruthenium-aluminum composite catalyst |
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2022
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| CN102815748A (en) * | 2012-08-24 | 2012-12-12 | 奇瑞汽车股份有限公司 | Titanium dioxide material, preparation method thereof, and dye sensitization solar cell |
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