CN102942218B - Method for preparing organic acid and base collaboratively supporting layered titanium dioxide - Google Patents
Method for preparing organic acid and base collaboratively supporting layered titanium dioxide Download PDFInfo
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- CN102942218B CN102942218B CN201210446982.8A CN201210446982A CN102942218B CN 102942218 B CN102942218 B CN 102942218B CN 201210446982 A CN201210446982 A CN 201210446982A CN 102942218 B CN102942218 B CN 102942218B
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 24
- 150000007524 organic acids Chemical class 0.000 title claims abstract description 16
- 150000007530 organic bases Chemical class 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title abstract description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 14
- 239000010936 titanium Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 235000005985 organic acids Nutrition 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- BQFCCCIRTOLPEF-UHFFFAOYSA-N chembl1976978 Chemical compound CC1=CC=CC=C1N=NC1=C(O)C=CC2=CC=CC=C12 BQFCCCIRTOLPEF-UHFFFAOYSA-N 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 3
- 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 3
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical group [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 3
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 150000008431 aliphatic amides Chemical class 0.000 claims description 2
- 230000029087 digestion Effects 0.000 claims description 2
- 150000002632 lipids Chemical class 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract description 2
- 238000003980 solgel method Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 9
- 238000006555 catalytic reaction Methods 0.000 description 7
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 229960000907 methylthioninium chloride Drugs 0.000 description 5
- 229960004756 ethanol Drugs 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- -1 through centrifugal Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- NMGYKLMMQCTUGI-UHFFFAOYSA-J diazanium;titanium(4+);hexafluoride Chemical compound [NH4+].[NH4+].[F-].[F-].[F-].[F-].[F-].[F-].[Ti+4] NMGYKLMMQCTUGI-UHFFFAOYSA-J 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 description 2
- 241000143437 Aciculosporium take Species 0.000 description 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 1
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- PLZVEHJLHYMBBY-UHFFFAOYSA-N Tetradecylamine Chemical compound CCCCCCCCCCCCCCN PLZVEHJLHYMBBY-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019445 benzyl alcohol Nutrition 0.000 description 1
- 229960004217 benzyl alcohol Drugs 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 1
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229940033355 lauric acid Drugs 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Abstract
The invention relates to a method for preparing organic acid and base collaboratively supporting layered titanium dioxide, and belongs to the photocatalysis technical field. The method comprises the following steps of: selecting a cheap titanium source, and adopting a sol-gel method to synthetise the layered titanium dioxide material through organic acid and base collaboratively supporting function. The method has the advantages of wide sources of raw materials, low cost, and simplicity in operation; an effective method for synthetising the layered titanium dioxide is provided. The material has excellent application value on aspect of purifying industrial sewage.
Description
Technical field
The present invention relates to the collaborative preparation method who supports laminar titanium dioxide of a kind of organic acids and base, belong to photocatalysis technology field.
Background technology
Titanium dioxide is a kind of important semiconductor material, because of its have nontoxic, catalytic activity is high, good stability and the advantage such as can reuse, and is widely used in the fields such as photochemical catalysis, sun power conversion, coating, paint and makeup.Wherein titanium dioxide optical catalyst can absorb sunlight, has good using value at aspects such as purified industrial sewage, is therefore considered to a kind of elite clone that is expected to simultaneously alleviate energy shortage and environmental problem.
But, the experimental results show the physics-chem characteristics such as the photochemical activity of titanic oxide material and the pattern of itself closely related.Therefore, develop a kind of method of effectively synthesizing different-shape titanium dioxide and become the focus of domestic and international research.In recent years, people have successfully synthesized the titanic oxide material of the different morphologies such as linear, clavate, spherical and stratiform.Because laminate structure exists larger bedding void, make it have very large application potential thereby can introduce active ion, oxide compound or biomass etc., but there is many deficiencies in the method for preparing laminar titanium dioxide.
For example,, according to Chinese patent CN 102078805: taking ammonium titanium fluoride as titanium source, adopt liquid-phase precipitation method, first by 35 ~ 80 DEG C of low-temperature hydrothermal, more successfully prepared laminar titanium dioxide after high-temperature calcination.But titanium source (ammonium titanium fluoride) price that the method adopts is more expensive, the temperature of this reaction is 35 ~ 80 DEG C needs heating.
For example,, according to Chinese patent CN 101791545: taking titanium tetrafluoride as titanium source, phenylcarbinol is solvent, adopts solvent-thermal method successfully to prepare laminar titanium dioxide.But titanium source (titanium tetrafluoride) price that the method adopts is more expensive, and a large amount of uses of solvent benzol methyl alcohol are also unfavorable for environmental protection.
For example,, according to Chinese patent CN 1543437A: successfully make laminar titanium dioxide by many layered titanates after acid treatment, solution layer and thermal treatment.But the building-up process of the method is comparatively complicated, need be through three step processing.
Summary of the invention
The object of the invention is to propose in order to improve the deficiencies in the prior art the collaborative preparation method who supports laminar titanium dioxide of a kind of organic acids and base; Open up a new way of simply preparing laminar titanium dioxide.
Concrete technical scheme of the present invention is: the collaborative preparation method who supports laminar titanium dioxide of a kind of organic acids and base, and concrete preparation process is as follows: organic acid and organic bases are placed in to container, add solvent orange 2 A that it is dissolved, be designated as solution A; Titanium source is placed in to container, adds solvent B that it is dissolved, be designated as solution B; Solution B is added in solution A, after stirring, with ammoniacal liquor regulator solution pH, continue to stir and react, through aging, centrifugal, washing and the dry laminar titanium dioxide material that to obtain.
The lipid acid that preferably organic acid is different carbon chain lengths, its structural formula is C
nh
2no
2, wherein n=8 ~ 16.Organic bases is the aliphatic amide of different carbon chain lengths, and its structural formula is C
nh
2n+3n, wherein n=8 ~ 18; Solvent orange 2 A is ethanol, Virahol or propyl carbinol.Titanium source is titanium sulfate, titanium tetrachloride or tetrabutyl titanate.Solvent B is sulfuric acid, hydrochloric acid, ethanol or Virahol.The add-on of solvent orange 2 A is for dissolving organic acid and organic bases.The add-on of solvent B is for dissolving titanium source.Preferably the mol ratio in organic acid and titanium source is 0.06 ~ 1.8:1; Organic bases and titanium source mol ratio are 0.05 ~ 1.5:1.The pH of preferred reaction solution is 0.5 ~ 7; Reaction times is 10 ~ 100 hours; Digestion time is 10 ~ 60 hours.
This material light catalysis property test: taking degradation of methylene blue under UV-light (MB) solution as probe reaction, reactor is BI-GHX-V type photochemical catalysis instrument (Shanghai Bi Lang Instrument Ltd.), and ultraviolet source is 500W high voltage mercury lamp.Specific experiment step is as follows: in test tube, add 25mg sample and 30ml 5mg/LMB solution, dark stirring 1 hour, after adsorption equilibrium, turn on light and carry out light-catalyzed reaction, every sampling in 10 minutes, centrifugal, ultraviolet-visible pectrophotometer is surveyed its absorbancy, calculates, and analyzes MB strength of solution changing conditions.
Beneficial effect:
The present invention has significance feature, by sol-gel method, under the collaborative supporting role of organic acids and base, prepares the titanium dioxide with laminate structure.Raw material that the method is selected is cheap and easy to get, reaction process without heating, experimental implementation is simple, equipment requirements is low, is a kind of preparation method of simple possible.The synthetic laminar titanium dioxide of this method is expected to be applied to the fields such as purification of waste water.
Brief description of the drawings
Fig. 1 is the field transmitting Electronic Speculum figure (FE-SEM) of embodiment 1 products therefrom;
Fig. 2 is the Photocatalytic Degradation Property figure of embodiment 1 products therefrom;
Fig. 3 is the field transmitting Electronic Speculum figure (FE-SEM) of embodiment 2 products therefroms;
Fig. 4 is the field transmitting Electronic Speculum figure (FE-SEM) of embodiment 3 products therefroms.
Embodiment
Below by embodiment, further illustrate outstanding feature of the present invention and marked improvement, be only this patent is described and do not limit this patent.
The prepared material light catalysis property test of following examples: taking degradation of methylene blue under UV-light (MB) solution as probe reaction, reactor is BI-GHX-V type photochemical catalysis instrument (Shanghai Bi Lang Instrument Ltd.), and ultraviolet source is 500W high voltage mercury lamp.Specific experiment step is as follows: in test tube, add 25mg sample and 30ml 5mg/L MB solution, dark stirring 1 hour, after adsorption equilibrium, turn on light and carry out light-catalyzed reaction, every sampling in 10 minutes, centrifugal, ultraviolet-visible pectrophotometer was surveyed its absorbancy, calculate, analyze MB strength of solution changing conditions.
[example 1]
Take 17g palmitic acid (C
16h
32o
2) and 5.2g amino dodecane (C
12h
27n) be placed in beaker, add 60ml ethanol, stirring and dissolving, is labeled as solution A.Measure 13.5ml tetrabutyl titanate and be placed in beaker, add 70ml Virahol, stirring and dissolving, is labeled as solution B.Solution B is added in solution A, after stirring, with ammoniacal liquor regulator solution pH be 7.Continue stirring reaction 10 hours, aging 60 hours, obtain white precipitate, through centrifugal, deionized water and dehydrated alcohol be washing alternately, dry, finally obtains laminar titanium dioxide product.Products therefrom has regular laminate structure (see figure 1).The photocatalysis performance of products therefrom, after tested, calculates, and knows that it reaches 99.43%(to methylene blue degradation rate and sees Fig. 2 under UV-light).
[example 2]
Take 1g capric acid (C
10h
20o
2) and 28g tetradecy lamine (C
14h
31n) be placed in beaker, add 80ml propyl carbinol, stirring and dissolving, is labeled as solution A.Measure 9.7ml titanium tetrachloride and be placed in beaker, add 50ml ethanol, stirring and dissolving, is labeled as solution B.Solution B is added to solution A, after stirring, with ammoniacal liquor regulator solution pH be 5.Continue stirring reaction 100 hours, aging 10 hours, obtain white precipitate, through centrifugal, deionized water and dehydrated alcohol be washing alternately, dry, finally obtains laminar titanium dioxide product.Products therefrom has regular laminate structure (see figure 3).The photocatalysis performance of products therefrom, after tested, calculates, and knows that it reaches 95.6% to methylene blue degradation rate under UV-light.
[example 3]
Take 27g laurostearic acid (C
12h
24o
2) and 2.1g stearylamine (C
18h
39n) be placed in beaker, add 70ml Virahol, stirring and dissolving, is labeled as solution A.Take 36g titanium sulfate and be placed in beaker, add 80ml 0.5mol/L sulfuric acid, stirring and dissolving, is labeled as solution B.Solution B is added to solution A, after stirring, with ammoniacal liquor regulator solution pH be 0.5.Continue stirring reaction 60 hours, aging 30 hours, obtain white precipitate, through centrifugal, deionized water and dehydrated alcohol be washing alternately, dry, finally obtains laminar titanium dioxide product.Products therefrom has regular laminate structure (see figure 4).The photocatalysis performance of products therefrom, after tested, calculates, and knows that it reaches 97.8% to methylene blue degradation rate under UV-light.
Claims (4)
1. the collaborative preparation method who supports laminar titanium dioxide of organic acids and base, concrete steps are as follows: organic acid and organic bases are placed in to container, add solvent orange 2 A that it is dissolved, be designated as solution A; Titanium source is placed in to container, adds solvent B that it is dissolved, be designated as solution B; Solution B is added in solution A, after stirring, with ammoniacal liquor regulator solution pH, continue to stir and react, through aging, centrifugal, washing and the dry laminar titanium dioxide material that to obtain; Wherein said organic acid is the lipid acid of different carbon chain lengths, and its structural formula is C
nh
2no
2, wherein n=8～16; Organic bases is the aliphatic amide of different carbon chain lengths, and its structural formula is C
nh
2n+3n, wherein n=8～18; Solvent orange 2 A is ethanol, Virahol or propyl carbinol; Solvent B is sulfuric acid, hydrochloric acid, ethanol or Virahol.
2. preparation method according to claim 1, is characterized in that described titanium source is titanium sulfate, titanyl sulfate, titanium tetrachloride or tetrabutyl titanate.
3. preparation method according to claim 1, is characterized in that described organic acid and the mol ratio in titanium source are 0.06～1.8:1; Organic bases and titanium source mol ratio are 0.05～1.5:1.
4. preparation method according to claim 1, is characterized in that described pH value of solution is 0.5～7, and the reaction times is 10～100h; Digestion time is 10～60h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210446982.8A CN102942218B (en) | 2012-11-09 | 2012-11-09 | Method for preparing organic acid and base collaboratively supporting layered titanium dioxide |
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|---|---|---|---|
| CN201210446982.8A CN102942218B (en) | 2012-11-09 | 2012-11-09 | Method for preparing organic acid and base collaboratively supporting layered titanium dioxide |
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| Publication Number | Publication Date |
|---|---|
| CN102942218A CN102942218A (en) | 2013-02-27 |
| CN102942218B true CN102942218B (en) | 2014-06-25 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1543437A (en) * | 2001-08-20 | 2004-11-03 | ��V��ѧ��ʽ���� | Layered titanic acid, lamellar titanic acid, lamellar titanium oxide and method for producing lamellar titanic acid |
| US7534293B2 (en) * | 2005-05-11 | 2009-05-19 | Agency For Science, Technology And Research | Method and solution for forming anatase titanium dioxide, and titanium dioxide particles, colloidal dispersion and film |
| CN101791545A (en) * | 2010-03-02 | 2010-08-04 | 上海师范大学 | Method for preparing (001) surface-exposed micrometer laminar titanium dioxide photocatalyst |
| CN102078805A (en) * | 2010-12-14 | 2011-06-01 | 华东理工大学 | Preparation method of layered titanium dioxide photochemical catalyst |
-
2012
- 2012-11-09 CN CN201210446982.8A patent/CN102942218B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1543437A (en) * | 2001-08-20 | 2004-11-03 | ��V��ѧ��ʽ���� | Layered titanic acid, lamellar titanic acid, lamellar titanium oxide and method for producing lamellar titanic acid |
| US7534293B2 (en) * | 2005-05-11 | 2009-05-19 | Agency For Science, Technology And Research | Method and solution for forming anatase titanium dioxide, and titanium dioxide particles, colloidal dispersion and film |
| CN101791545A (en) * | 2010-03-02 | 2010-08-04 | 上海师范大学 | Method for preparing (001) surface-exposed micrometer laminar titanium dioxide photocatalyst |
| CN102078805A (en) * | 2010-12-14 | 2011-06-01 | 华东理工大学 | Preparation method of layered titanium dioxide photochemical catalyst |
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