CN107930609A - Half crystallization titanium oxide powder and preparation method with photocatalysis self-activation effect - Google Patents
Half crystallization titanium oxide powder and preparation method with photocatalysis self-activation effect Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 60
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000002425 crystallisation Methods 0.000 title claims abstract description 41
- 230000008025 crystallization Effects 0.000 title claims abstract description 41
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 29
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 25
- 239000000843 powder Substances 0.000 title claims abstract description 21
- 230000000694 effects Effects 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 30
- 239000001257 hydrogen Substances 0.000 claims abstract description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 claims abstract description 21
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 claims description 2
- 241000736199 Paeonia Species 0.000 claims 1
- 235000006484 Paeonia officinalis Nutrition 0.000 claims 1
- 238000004821 distillation Methods 0.000 claims 1
- 239000002105 nanoparticle Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 20
- 238000000034 method Methods 0.000 abstract description 7
- 150000002431 hydrogen Chemical class 0.000 abstract description 5
- 238000005286 illumination Methods 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 abstract description 2
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 239000011858 nanopowder Substances 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 20
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 8
- 238000012360 testing method Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000004408 titanium dioxide Substances 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- 238000003912 environmental pollution Methods 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 239000003929 acidic solution Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000010842 industrial wastewater Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 208000003174 Brain Neoplasms Diseases 0.000 description 1
- 206010009944 Colon cancer Diseases 0.000 description 1
- 206010064571 Gene mutation Diseases 0.000 description 1
- 208000002454 Nasopharyngeal Carcinoma Diseases 0.000 description 1
- 206010061306 Nasopharyngeal cancer Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000003855 cell nucleus Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 208000029742 colonic neoplasm Diseases 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- -1 glued board Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 201000011216 nasopharynx carcinoma Diseases 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/12—Oxidising
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/22—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1088—Non-supported catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention proposes a kind of half crystallization titanium oxide powder with visible light photocatalysis production hydrogen self-activation effect and preparation method thereof.This titanium oxide is to be prepared at normal temperatures and pressures using simple aqua-solution method.The preparation process of its powder is:Isopropyl titanate is instilled in acidic aqueous solution first;Then add suitable H2O2Aqueous solution, and dry and obtain half crystallization titanium oxide powder.This method has the advantages that process is easy, raw material is cheap, energy conservation and environmental protection.Obtain nano-powder has a Photocatalyzed Hydrogen Production self-activation phenomenon under visible light illumination, i.e., hydrogen-producing speed is continuously increased with the extension of visible ray light application time, available for clean energy resource preparation field.
Description
Technical field
The present invention relates to visible light photocatalysis production hydrogen field.
Technical background
The conductor photocatalysis that target is prepared as with environmental pollution improvement and clean energy resource has attracted material, chemistry, environment
With the great interest of the field scientific worker such as the energy.Photocatalysis can eliminate environmental pollution as a kind of advanced technology
Meanwhile sunlight is converted into hydrogen energy source.Hydrogen Energy is a kind of clean regenerative resource, is generated after calorific value height and energy release
Water, so as to avoid problem of environmental pollution caused by traditional fossil energy, is considered as one of optimal alternative energy source.Formaldehyde
As common are malicious organic pollution in industrial wastewater, Photocatalyzed Hydrogen Production research is seldom used directly to so far.High concentration
The industrial wastewater that formaldehyde is produced essentially from manufacturing industry such as resin, leather, staple fibre, glued board, preservatives, Long Term Contact first
Aldehyde can cause nasopharyngeal carcinoma, colon cancer, brain tumor and cell nucleus gene mutation etc..First in industrial wastewater is decomposed using sunlight photocatalysis
Aldehyde production hydrogen is to realize environmental pollution improvement and effective way prepared by clean energy resource at the same time.
The present invention, which intends preparing under normal temperature and pressure conditions by simple aqua-solution method, new has visible light photocatalysis
Produce half crystallization titania meterial of hydrogen self-activation effect.The material mainly has the advantages that following three aspects:1. good can
See absorbing properties:Traditional titanium dioxide cannot absorb visible ray.But the new half crystallization titanium oxide can effectively absorb not
The visible ray of co-wavelength.2. good visible light photocatalysis active:Experiment shows:The material possesses to be decomposed under visible light exposure
The activity of formaldehyde production hydrogen in water, and common titanium dioxide does not have the activity of visible light photocatalysis production hydrogen.3. self-activation effect:Should
In the photocatalytic process of formaldehyde in decomposing water, photocatalytic activity (hydrogen-producing speed) constantly increases material with the extension of light application time
Add.
The content of the invention
The present invention proposes that a kind of half crystallization photocatalytic titanium oxide that is new, having visible light photocatalysis production hydrogen self-activation effect is urged
Agent powder and preparation method thereof.The half crystallization titania meterial of the present invention does not introduce any foreign matter, is in normal temperature and pressure
It is lower to be prepared using aqua-solution method.
The preparation method of half crystallization titanium oxide proposed by the present invention is:Organic titanium is hydrolyzed in acid condition, and is being hydrolyzed
Substantial amounts of H is added during organic titanium2O2, half crystallization titanium oxide is obtained by being dried after high-speed stirred.
Prepare concretely comprising the following steps for half crystallization titanium oxide:
Measure 0.6-1ml 65% concentrated nitric acid be dissolved in 50-200ml distilled water, under magnetic stir bar strong stirring by
Drop instills 5-10ml isopropyl titanates;5-20ml 30%H are instilled in the white suspension of gained2O2Aqueous solution, liquid are gradual
Become laking, continue stir 6-24 it is small when after, liquid becomes buff, and buff suspension is placed in 40-80 DEG C of baking oven
After the drying of face, up to half crystallization titanium oxide powder.
The present invention while realizes half crystallization of titanium oxide under conditions of foreign matter is not introduced, energy gap it is narrow
Bandization, and self-excitation effect, successfully extend the visible absorption performance of titanium oxide, and obtaining new has self-excitation effect
Half crystallization titanium oxide powder.The purpose of the present invention is integrating the advantages of titanium oxide photochemical catalyst ability is strong, while utilize half crystallization
Amorphous titanium peroxide structural instability in titanium oxide, the characteristic easily recombinated realize the material during visible light photocatalysis
Self-activation and highly effective hydrogen yield, so as to obtain a kind of with self-activation effect, it is seen that light Photocatalyzed Hydrogen Production function admirable it is visible
Photochemical catalyst.
Half crystallization titanium oxide is hydrolyzed at the same time in acid condition using organic titanium at normal temperatures and pressures in the present invention, is added big
Measure H2O2Processing method, it is not necessary to high temperature and pressure, has the advantages that preparation process is easy, raw material is cheap, energy conservation and environmental protection.Obtain
Half crystallization titanium oxide powder have self-excitation effect and visible light photocatalysis H2-producing capacity it is good.
Brief description of the drawings
The high-resolution-ration transmission electric-lens photo of half crystallization titanium oxide of Fig. 1.
The X-ray powder diffraction figure of half crystallization titanium oxide of Fig. 2.
The ultraviolet-visible absorption spectra figure of half crystallization titanium oxide of Fig. 3.
The visible ray light for decomposing formaldehyde in water under the visible ray illumination of half crystallization titanium oxide of Fig. 4 and normal titanium dioxide is urged
Change production hydrogen experiment.
Formaldehyde production hydrogen circulation experiment in water is decomposed under the visible ray illumination of half crystallization titanium oxide of Fig. 5.
Embodiment
Example 1:Preparation, appearance structure characterization and the photocatalysis test of half crystallization titanium oxide powder
The preparation of half crystallization titanium oxide:Accurate measuring 1ml concentration is 65% salpeter solution, adds 100ml deionized waters
Middle formation acid solution;In addition 10ml isopropyl titanates are measured, are added dropwise under the strong stirring of magnetic stirring apparatus acid molten
In liquid;20ml 30%H are added under strong stirring2O2Aqueous solution, obtains yellow suspension TiO2Solution.Yellow suspension is placed on
Half crystallization titanium oxide powder is dried to obtain in 60 DEG C of baking ovens.
Photocatalysis is tested:Weigh half crystallization titanium oxide powders of 200mg, be scattered in 100ml formalin (90ml water+
37% formalins of 10ml) sealed double glazing container in, glass sandwich is passed through the temperature of the accurate control loop water of recirculated water
Spend (25 DEG C);By stirring, after desorption equilibrium to be adsorbed, with additional 420 nanometers of optical filter simulated visible light pair of 300W xenon lamps
Solution irradiates, and carries out Photocatalyzed Hydrogen Production performance test.Certain light application time is spaced, passes through the production of chromatography on-line checking hydrogen
Amount.
X-ray diffraction and transmissioning electric mirror test result show that half crystallization titanium oxide of gained contains substantial amounts of amorphous state
And the mixture (see Fig. 1 and Fig. 2) of anatase titanium dioxide, so as to confirm as half crystallization titanium oxide.
Uv-vis spectra test result shows:Half crystallization titanium oxide of gained can effectively absorb visible ray (Fig. 3)
Photocatalysis test result shows, using the half crystallization titanium oxide powder as photochemical catalyst, photocatalytic activity (production hydrogen speed
Rate) with the extension of light application time, it is continuously increased (Fig. 4 and Fig. 5).Through 5 it is small when simulated solar irradiation irradiate, it is light-catalysed production hydrogen speed
Rate is about 5 times of first hour;The average hydrogen-producing speed of 4th photocatalysis circulation is about first photocatalysis circulation
4 times of hydrogen-producing speed.
Example 2:Change the dosage of hydrogen peroxide in formula, the preparation of half crystallization titanium oxide powder, performance characterization
The salpeter solution that 1ml concentration is 65% is instilled in 100ml deionized waters, forms strongly acidic solution;In addition measure
10ml isopropyl titanates, are added dropwise in strongly acidic solution under the strong stirring of magnetic stirring apparatus and are hydrolyzed;Strongly stirring
Mix in lower addition 30% hydrogen peroxide solutions of 5ml, obtain light yellow suspended titanium dioxide solution.Solution is placed in 60 DEG C of baking ovens
Fully it is dried to obtain powder sample.X-ray diffraction, transmission electron microscope and photocatalysis performance test show, still can under the formula
Synthesize the self-activating half crystallization nano-titanium oxide of photocatalysis.
Example 3:Change the dosage of nitric acid in formula, the preparation of half crystallization titanium oxide powder, performance characterization
The salpeter solution that 0.6ml concentration is 65% is instilled in the 100ml deionized waters of accurate weighing, it is molten to form faintly acid
Liquid;In addition 10ml isopropyl titanates are measured, is added dropwise under the strong stirring of magnetic stirring apparatus in weakly acidic solution and carries out water
Solution;30% hydrogen peroxide solutions of 20ml are added under strong stirring, obtain the yellow titania solution of muddiness.By yellow solution
It is placed in 60 DEG C of baking ovens and is dried to obtain titanium oxide powder.X-ray diffraction, transmission electron microscope and visible light photocatalysis production hydrogen test table
Bright, this method can still obtain the half crystallization nano-titanium oxide with visible light photocatalysis production hydrogen self-activation effect.
Example 4:Change the dosage of isopropyl titanate in formula, the preparation of half crystallization titanium oxide powder, performance characterization
The salpeter solution that 0.6ml concentration is 65% is added in ready 100ml deionized waters, it is molten to form clear
Liquid;Accurate measuring 5ml isopropyl titanates, are added dropwise in acid solution under continuous-stable stirring and are hydrolyzed;Continuously stirring
Lower addition 30% hydrogen peroxide solutions of 20ml are mixed, obtain lurid titanium dioxide turbid solution.Liquid is placed in 60 DEG C of baking ovens and is done
It is dry to obtain half crystallization titanium oxide powder.X-ray diffraction, transmission electron microscope and Photocatalyzed Hydrogen Production test shows, the preparation approach according to
The half crystallization nano-titanium oxide with visible light photocatalysis production hydrogen self-activation effect can so be obtained.
Claims (3)
1. there is half crystallization titanium oxide powder of visible light photocatalysis self-activation, it is characterized in that:Amorphous state and anatase two
Titanium oxide coexists in same nano particle, under visible light exposure, has Photocatalyzed Hydrogen Production self-activation effect.
2. a kind of preparation method of half crystallization titanium oxide powder of claim 1, it is characterized in that:Hydrolyze in acid condition organic
Titanium, and add substantial amounts of H during organic titanium is hydrolyzed2O2, half crystallization titanium oxide is obtained by being dried after high-speed stirred.
3. technology of preparing as claimed in claim 2, it is characterized in that:The concentrated nitric acid for measuring 0.6-1ml 65% is dissolved in 50-200ml distillations
In water, 5-10ml isopropyl titanates are instilled dropwise under magnetic stir bar strong stirring;Instilled in the white suspension of gained
5-20ml 30%H2O2Aqueous solution, liquid gradually become peony, continue stir 6-24 it is small when after, liquid becomes buff, will
Buff suspension is placed on the half crystallization oxidation for after drying, that is, obtaining having the function of photocatalysis self-activation inside 40-80 DEG C of baking oven
Titanium valve body.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109092055A (en) * | 2018-10-16 | 2018-12-28 | 上海朗绿建筑科技股份有限公司 | A kind of formaldehyde adsorbent and preparation method thereof |
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2017
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Application publication date: 20180420 |