CN106890656A - A kind of phosphorus doping TiO 2 sol and preparation method thereof - Google Patents
A kind of phosphorus doping TiO 2 sol and preparation method thereof Download PDFInfo
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- 229910010413 TiO 2 Inorganic materials 0.000 title claims abstract description 38
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 36
- 239000011574 phosphorus Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 22
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 15
- 239000002244 precipitate Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 11
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 241000370738 Chlorion Species 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 150000003608 titanium Chemical class 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- 241000907661 Pieris rapae Species 0.000 claims 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 8
- 238000006731 degradation reaction Methods 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 8
- 229940043267 rhodamine b Drugs 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 230000006641 stabilisation Effects 0.000 abstract description 3
- 238000011105 stabilization Methods 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 230000007774 longterm Effects 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 13
- 238000007146 photocatalysis Methods 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 238000013112 stability test Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000001603 reducing effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000002155 anti-virotic effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052721 tungsten Inorganic materials 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
A kind of phosphorus doping TiO 2 sol solvent structure composition is anatase titanium dioxide and a small amount of amorphous titania.A kind of phosphorus doping TiO 2 sol product cut size of the present invention is small, specific surface area is big, this product is up to 99.9% to the degradation efficiency of rhodamine B in 3 hours, catalytic effect is excellent, heat endurance is good, non-toxic, can be kept in the case of without other any reagents long-term stabilization with it is transparent, a kind of phosphorus doping TiO 2 sol of the present invention makes to form impurity energy level between titanium dioxide forbidden band, expands the range of application of titanium dioxide；Low raw-material cost is easy to get, low production cost, and preparation method is easy to reappear, and production process is safe and reliable, and environment-friendly, the dispergation time is short, with short production cycle, it is adaptable to industrialized production.
Description
Technical field
The present invention relates to a kind of phosphorus doping TiO 2 sol and preparation method thereof.
Background technology
Titanium dioxide is current most promising photochemical catalyst, and it has strong oxidizing property, the pollution of the degradable overwhelming majority
Material.When energy is mapped to semiconductor more than or equal to the illumination of energy gap, semiconductive particles absorb natural light, produce electronics-sky
Cave pair.Photo-induced hole and photoinduced electron have strong oxidizing property and strong reducing property, will adsorb the H in titanium dioxide surface2O、O2Deng thing
Matter redox into the free radical with strong oxidizing property and strong reducing property, and then redox organic pollution materials, so as to reach
The purpose of degradation of contaminant.
At present it is known that nano titanium oxide has anatase, rutile, three kinds of crystal formations of brockite, anatase and rutile belong to
In tetragonal crystal system, brockite belongs to tetragonal system.Nano-titanium dioxide stable performance, under normal temperature hardly with other compounds
Reaction, water insoluble, diluted acid is slightly soluble in alkali and hot nitric acid, not with CO in air2、SO2、O2Deng reaction, with biologically inert.Receive
Rice titanium dioxide has heat endurance, non-toxic.
The particle diameter of nano titanium oxide is small, specific surface area is big, Active sites are more, high catalytic efficiency, and to environment not
Secondary pollution is produced, therefore is widely used in various technical fields.In the case where there is illumination, nano titanium oxide has
Strong oxidisability and Superhydrophilic, can be used for the purification of air, the treatment of sewage, the utilization of solar energy, antibacterial, antivirus and from clear
The field such as clean, with good actual application value.But there are two defects in titanium dioxide optical catalyst, one is can in itself
See that the absorbing wavelength of light need to be too short in below 385nm, Titanium dioxide absorption optical wavelength；The second is nano titanium oxide quantum yield
Low, the two defects strongly limit the range of application of titanium dioxide optical catalyst, prevent titanium dioxide from fully obtaining profit
With.Meanwhile, the optically catalytic TiO 2 effect obtained by prior art is also not ideal, particularly to rhodamine B degradation effect
It is not ideal with degradation speed, therefore, titanium dioxide is modified, it is very necessary to solve above-mentioned technical problem.
The content of the invention
An object of the present disclosure is to provide a kind of phosphorus doping TiO 2 sol.
Another object of the present invention is the preparation method for providing above-mentioned phosphorus doping TiO 2 sol.
The purpose of the present invention is realized by following technical measures：
A kind of phosphorus doping TiO 2 sol, it is characterised in that：The phosphorus doping TiO 2 sol structure composition is sharp
Titanium ore type titanium dioxide and a small amount of amorphous titania, in preparation process are added by doped raw material of phosphoric acid.This is molten
Glue specific surface area is larger, photocatalysis efficiency is higher, and does not produce secondary pollution to environment, prepares TiO 2 sol and keeps for a long time
Stabilization and good photocatalysis effect, beneficial to the application of follow-up titanium dioxide.
A kind of preparation method of phosphorus doping TiO 2 sol, it is characterised in that it is obtained as follows：
1. under 0 DEG C of cryogenic conditions, titanium tetrachloride is added to the mixed solvent of absolute ethyl alcohol and deionized water composition
In, and stir, speed of agitator is 300~1000r/min, obtains mixed solution；
2. the pH value of mixed solution is adjusted in mixed solution and dripping ammoniacal liquor to neutral (pH=7), white precipitate is obtained；
3. white precipitate is centrifuged and is washed with deionized, until not containing chlorion；
4. the white precipitate after washing in step 3 is taken, adds hydrogen peroxide and distilled water to be stirred dispergation, treat dispergation to molten
Untill liquid clear, phosphoric acid is added, it is 1~4h of condensing reflux at 70~100 DEG C to be placed in temperature, obtains clear, yellowish phosphorus
Doped titanium dioxide collosol.
Dispergation of the present invention refers to the process of the gel state by bulky grain into short grained collosol state.
Further, a kind of preparation method of phosphorus doping TiO 2 sol, it is characterised in that four chlorination described in step 1
Titanium, ethanol, the volume ratio of deionized water are 1~5：3~5：3~30.
Further, a kind of preparation method of TiO 2 sol, it is characterised in that the matter of absolute ethyl alcohol described in step 1
Amount concentration is 99.7%.
Further, a kind of preparation method of phosphorus doping TiO 2 sol, it is characterised in that ammoniacal liquor described in step 2
Mass concentration is 25%~28%.
Further, a kind of preparation method of phosphorus doping TiO 2 sol, it is characterised in that ammoniacal liquor adds described in step 2
It is 3~12 that enter amount need to meet volume ratio with inorganic titanium salt:1~3.
Further, a kind of preparation method of phosphorus doping TiO 2 sol, it is characterised in that hydrogen peroxide described in step 4
Mass concentration be 30%.
Further, a kind of preparation method of phosphorus doping TiO 2 sol, it is characterised in that hydrogen peroxide described in step 4
It is 8~12 with the volume ratio of the addition of distilled water and inorganic titanium salt：100~150：1~5.
Further, a kind of preparation method of phosphorus doping TiO 2 sol, it is characterised in that phosphoric acid described in step 4
Mass fraction is 85%.
Further, a kind of preparation method of phosphorus doping TiO 2 sol, it is characterised in that phosphoric acid described in step 4 and
The mol ratio of titanium tetrachloride is 1~10：100~200.
The present invention has following beneficial effect：
A kind of phosphorus doping TiO 2 sol product cut size of the present invention is small, and specific surface area is big, and this product is to rhodamine in 3 hours
The degradation efficiency of B is up to 99.9%, and catalytic effect is excellent, and heat endurance is good, non-toxic, in the feelings without other any reagents
Can be kept under condition long-term stabilization with it is transparent, a kind of phosphorus doping TiO 2 sol of the invention makes to be formed between titanium dioxide forbidden band
Impurity energy level, expands the range of application of titanium dioxide；Low raw-material cost is easy to get, low production cost, and preparation method is easy to reappear,
Production process is safe and reliable, environment-friendly, and the dispergation time is short, with short production cycle, it is adaptable to industrialized production.
Brief description of the drawings
Fig. 1 is degradation rate of the phosphorus doping titanium dioxide to rhodamine B；
Fig. 2 is the UV-Vis abosrption spectrograms of phosphorus doping titanium dioxide；
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to it is pointed out here that be that following examples are only used
It is further described in the present invention, it is impossible to be interpreted as limiting the scope of the invention, without departing substantially from spirit of the invention
In the case of essence, the modification or replacement made to the inventive method, step or condition belong to the scope of the present invention.
Embodiment 1
Under the conditions of 0 DEG C, take titanium tetrachloride 1ml and be added in the mixed liquor that absolute ethyl alcohol 3ml each with deionized water is mixed,
And be stirred vigorously, rotating speed 400r/min obtains mixed solution；Then, in the ammonia that mixed solution and dripping mass concentration is 28%
Aqueous solution 3.7ml adjusts the pH=7 of mixed solution, obtains white precipitate；White precipitate is centrifuged and is washed with deionized,
Until not containing chlorion；The white precipitate after washing is taken, hydrogen peroxide 10.2ml and distilled water 120ml stirring dispergation is added, stirred
Mix after dispergation finishes, add the phosphoric acid 0.05ml that mass fraction is 85%, condensing reflux 4h, obtains under 90 DEG C of heating-up temperature
Clear, yellowish phosphorus doping TiO 2 sol.
Experiment 1：Photocatalysis is tested：
Product obtained by Example 1 carries out photocatalysis experiment.Take 5ml products and be added to 100ml rhodamine B solution
(15mg/L), dark place is preserved 3 hours, opens the light (the use of light source being tungsten lamp), and degradation efficiency is determined every half an hour.Experimental result is such as
Shown in Fig. 1, as seen from the figure, after 3 hours, this product is 99.9% to the degradation efficiency of rhodamine B.Experiment 2：Stability test：
Product obtained by Example 1 carries out stability test.6 months are placed in room conditions afterwards, and product is still
Old to keep stable and transparent, after measured, catalytic effect is still good.
Embodiment 2
Under the conditions of 0 DEG C, take titanium tetrachloride 1ml and be added in the mixed liquor that absolute ethyl alcohol 5ml each with deionized water is mixed,
And be stirred vigorously, rotating speed 900r/min obtains mixed solution；Then, in the ammonia that mixed solution and dripping mass concentration is 25%
Aqueous solution 5.9ml adjusts the pH=7 of mixed solution, obtains white precipitate；White precipitate is centrifuged and is washed with deionized,
Until not containing chlorion；The white precipitate after washing is taken, hydrogen peroxide 9.7ml and distilled water 110ml stirring dispergation, stirring is added
After dispergation is finished, the phosphoric acid 0.07ml that mass fraction is 85% is added, condensing reflux 3h, obtains under 80 DEG C of heating-up temperature
Bright light yellow phosphorus doping TiO 2 sol.
Product obtained by Example 2 carries out photocatalysis experiment respectively by the test method of embodiment 1 and stability is tried
Test, photocatalysis result of the test shows good degrading effect of this product to rhodamine B, stability test result shows product stability
It is good.
Embodiment 3
Under the conditions of 0 DEG C, take titanium tetrachloride 1ml and be added in the mixed liquor that absolute ethyl alcohol 4ml each with deionized water is mixed,
And be stirred vigorously, rotating speed 700r/min obtains mixed solution；Then, in the ammonia that mixed solution and dripping mass concentration is 27%
Aqueous solution 4.6ml adjusts the pH=7 of mixed solution, obtains white precipitate；White precipitate is centrifuged and is washed with deionized,
Until not containing chlorion；The white precipitate after washing is taken, hydrogen peroxide 8.6ml and distilled water 130ml stirring dispergation, stirring is added
After dispergation is finished, the phosphoric acid 0.05ml that mass fraction is 85% is added, condensing reflux 2h, obtains under 100 DEG C of heating-up temperature
Clear, yellowish phosphorus doping TiO 2 sol.
Product obtained by Example 3 carries out photocatalysis experiment respectively by the test method of embodiment 1 and stability is tried
Test, photocatalysis result of the test shows good degrading effect of this product to rhodamine B, stability test result shows product stability
It is good.
Claims (10)
1. a kind of phosphorus doping TiO 2 sol, it is characterised in that：The phosphorus doping TiO 2 sol structure composition is sharp titanium
Ore deposit type titanium dioxide and amorphous titania, in preparation process are added by doped raw material of phosphoric acid.
2. the preparation method of phosphorus doping TiO 2 sol as claimed in claim 1, it is characterised in that it is to make as follows
：
A. under 0 DEG C of cryogenic conditions, titanium tetrachloride is added in the mixed solvent of absolute ethyl alcohol and deionized water composition, and
Stirring, speed of agitator is 300~1000r/min, obtains mixed solution；
B. the pH value of mixed solution is adjusted in mixed solution and dripping ammoniacal liquor to neutral (pH=7), white precipitate is obtained；
C. white precipitate is centrifuged and is washed with deionized, until not containing chlorion；
D. the white precipitate after washing in step C is taken, adds hydrogen peroxide and distilled water to be stirred dispergation, treat that dispergation is clear to solution
It is clear it is bright untill, add phosphoric acid, it is 1~4h of condensing reflux at 70~100 DEG C to be placed in temperature, obtains clear, yellowish phosphorus doping
TiO 2 sol.
3. a kind of preparation method of phosphorus doping TiO 2 sol as claimed in claim 2, it is characterised in that institute in step A
It is 1~5 to state titanium tetrachloride, ethanol, the volume ratio of deionized water：3~5：3~30.
4. as claimed in claim 2 or claim 3 a kind of preparation method of TiO 2 sol, it is characterised in that nothing described in step A
The mass concentration of water-ethanol is 99.7%.
5. a kind of preparation method of the phosphorus doping TiO 2 sol as described in claim 2,3 or 4, it is characterised in that step B
Described in ammoniacal liquor mass concentration be 25%~28%.
6. a kind of preparation method of phosphorus doping TiO 2 sol as claimed in claim 5, it is characterised in that institute in step B
It is 3~12 that state ammoniacal liquor addition need to meet volume ratio with inorganic titanium salt:1~3.
7. the preparation method of a kind of phosphorus doping TiO 2 sol as described in claim 5 or 6, it is characterised in that in step D
The mass concentration of the hydrogen peroxide is 30%.
8. a kind of preparation method of the phosphorus doping TiO 2 sol as described in claim 5,6 or 7, it is characterised in that step D
Described in hydrogen peroxide and distilled water addition and inorganic titanium salt volume ratio be 8~12：100~150：1~5.
9. a kind of preparation method of phosphorus doping TiO 2 sol as claimed in claim 8, it is characterised in that institute in step D
The mass fraction for stating phosphoric acid is 85%.
10. a kind of preparation method of phosphorus doping TiO 2 sol as claimed in claim 9, it is characterised in that institute in step D
The mol ratio for stating phosphoric acid and titanium tetrachloride is 1~10：100~200.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108892167A (en) * | 2018-07-05 | 2018-11-27 | 重庆交通大学 | A kind of two dimension titanium dioxide crystal form, colloidal sol and preparation method thereof |
| CN109529951A (en) * | 2018-11-28 | 2019-03-29 | 深圳市天得环境科技有限公司 | A kind of small particle stabilized scattering nano titanium dioxide synthetic method |
| CN110033960A (en) * | 2019-04-22 | 2019-07-19 | 南京理工大学 | A method of preparing titanium oxide nanoflower electrode |
| CN113272390A (en) * | 2018-12-10 | 2021-08-17 | 克斯塔斯科技有限公司 | Phosphorus-doped surface coating and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049962A (en) * | 2007-05-18 | 2007-10-10 | 广东省生态环境与土壤研究所 | Method for preparing sol of neutral Nano titanium dioxide |
| CN101580276A (en) * | 2009-06-19 | 2009-11-18 | 华南理工大学 | Preparation method of highly dispersive spindle-shaped nano titanium dioxide sol |
| CN101891247A (en) * | 2010-06-24 | 2010-11-24 | 彩虹集团公司 | Method for preparing anatase titanium dioxide sol used for solar batteries |
| CN104338522A (en) * | 2013-08-01 | 2015-02-11 | 京程科技股份有限公司 | Preparing method of titanium dioxide sol photocatalyst and applications of the titanium dioxide sol photocatalyst in decontamination and self-cleaning |
-
2017
- 2017-03-23 CN CN201710176699.0A patent/CN106890656A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049962A (en) * | 2007-05-18 | 2007-10-10 | 广东省生态环境与土壤研究所 | Method for preparing sol of neutral Nano titanium dioxide |
| CN101580276A (en) * | 2009-06-19 | 2009-11-18 | 华南理工大学 | Preparation method of highly dispersive spindle-shaped nano titanium dioxide sol |
| CN101891247A (en) * | 2010-06-24 | 2010-11-24 | 彩虹集团公司 | Method for preparing anatase titanium dioxide sol used for solar batteries |
| CN104338522A (en) * | 2013-08-01 | 2015-02-11 | 京程科技股份有限公司 | Preparing method of titanium dioxide sol photocatalyst and applications of the titanium dioxide sol photocatalyst in decontamination and self-cleaning |
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| CN108892167A (en) * | 2018-07-05 | 2018-11-27 | 重庆交通大学 | A kind of two dimension titanium dioxide crystal form, colloidal sol and preparation method thereof |
| CN108892167B (en) * | 2018-07-05 | 2019-11-26 | 重庆交通大学 | A kind of two dimension titanium dioxide crystal form, colloidal sol and preparation method thereof |
| CN109529951A (en) * | 2018-11-28 | 2019-03-29 | 深圳市天得环境科技有限公司 | A kind of small particle stabilized scattering nano titanium dioxide synthetic method |
| CN109529951B (en) * | 2018-11-28 | 2021-08-03 | 深圳市天得一环境科技有限公司 | Synthesis method of small-particle-size stably-dispersed nano titanium dioxide |
| CN113272390A (en) * | 2018-12-10 | 2021-08-17 | 克斯塔斯科技有限公司 | Phosphorus-doped surface coating and preparation method thereof |
| CN113272390B (en) * | 2018-12-10 | 2023-02-17 | 克斯塔斯科技有限公司 | Phosphorus-doped surface coating and preparation method thereof |
| CN110033960A (en) * | 2019-04-22 | 2019-07-19 | 南京理工大学 | A method of preparing titanium oxide nanoflower electrode |
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