CN104098133A - Preparation method for high-efficient photocatalyst-nanometer titanium dioxide water-based colloid - Google Patents
Preparation method for high-efficient photocatalyst-nanometer titanium dioxide water-based colloid Download PDFInfo
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- CN104098133A CN104098133A CN201410312547.5A CN201410312547A CN104098133A CN 104098133 A CN104098133 A CN 104098133A CN 201410312547 A CN201410312547 A CN 201410312547A CN 104098133 A CN104098133 A CN 104098133A
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Abstract
The invention discloses a preparation method for a high-efficient photocatalyst-nanometer titanium dioxide water-based colloid. The preparation method comprises the following steps: adopting metal titanium as titanium source; adopting hydrogen peroxide to oxidize nulvalent metal Ti into quadrivalent TiO<2+>; further conducting complexing on the TiO<2+> and the hydrogen peroxide to obtain water-soluble TiO[H2O2]<2+> yellow complex; obtaining yellow complex colloid after evaporating and removing excess hydrogen peroxide and ammonia; conducting hydrothermal reaction by high pressure water of 150-200 DEG C; transporting the TiO[H2O2]<2+> yellow complex into pure white Ti(OH)4 water-based emulsion; adding mineral acid to adjust the pH value of the emulsion to the range of 2-4; conducting temperature control to enable the temperature of water bath to be 60-80 DEG C; continually stirring for 3-6 hours to enable the Ti(OH)4 water-based emulsion to gradually gel into nanometer titanium dioxide water-based colloid. The preparation method uses no organic solvent; no waste water or waste gas generates in the reaction process; particle diameters of colloid granular are less than 10 nanometers; degree of crystallinity is high; high photocatalytic activity is provided; coating property and film forming property on porous base material are extremely good.
Description
Technical field
The present invention relates to a kind of preparation method of high efficiency photocatalyst, belong to the Application Areas that nano titanium dioxide photocatalysis is curbed environmental pollution.
Background technology
Optically catalytic TiO 2 technology is applied to the control of environmental pollution, is particularly used for thoroughly decomposing various poisonous, harmful organic pollutants have become that countries in the world generally acknowledge one of effective means.
In 863 national major scientific and technological project industrialization biddings documents, point out: the practical mark of photocatalysis technology is " two is high one low; " the difficult problem in high efficiency photocatalyst and highly effective photocatalytic reactor development to be solved technically, the requirement of low cost movement will be reached economically.
Nanotechnology is the one preferred technique that obtains high efficiency photocatalyst.
Over nearly 20 years, experts and scholars both domestic and external have done a large amount of R&D works preparing aspect nano titanium dioxide photocatalyst, also there is many patents, comprised the preparation methods' such as nano titanium oxide solid state powder, nano titanium oxide solvent-borne type colloid, nanometer titanium dioxide water colloid patented technology.As everyone knows, nano titanium oxide solid state powder is difficult disperses, easily reunites; In nano titanium oxide solvent-borne type colloid, organic solvent is volatile, difficult preserves; Therefore the tool actual application prospect of the nanometer titanium dioxide water colloid of highly dispersed state.
But, in the patented technology of preparing at numerous nanometer titanium dioxide water colloids, mostly adopting organic titanium is main raw material (as titanic acid ester or title titanium alkoxide, titan-alkoxide etc.), in building-up process, also need to add organic solvent (as ethanol, propyl alcohol, Virahol etc.), hydrolysis inhibitor (as diethanolamine, trolamine etc.), sequestrant (as quadrol, methyl ethyl diketone etc.), not only raw materials cost is high, and can cause environmental pollution.
Summary of the invention
The object of the invention is to provide a kind of preparation method of high efficiency photocatalyst-nanometer titanium dioxide water colloid, and this preparation method is it is inorganic synthetic completely, does not use any organic solvent, in reaction process, produce without waste water, waste gas, and be a kind of clean preparation technology; The theoretical earning rate of titanium dioxide is up to 166%, and raw materials cost reduces greatly compared with other patent technique; The nanometer titanium dioxide water colloidal solid particle diameter that adopts the present invention to prepare is less than 10 nanometers, and degree of crystallinity is high, has very strong photocatalytic activity; And the coating property on porous substrate and film forming properties are very good, high efficiency photocatalysis agent film be can make and air and water purification field are applied in, can various poisonous, the harmful organic pollutants of oxygenolysis under the irradiation of UV-light, high and removal time of formaldehyde clearance shortens greatly, and sterilizing rate is high and the time is short simultaneously.
For achieving the above object, the technical solution used in the present invention comprises the following steps: a kind of preparation method of high efficiency photocatalyst-nanometer titanium dioxide water colloid, comprises the following steps:
Step 1, metal titanium is put into glass beaker, add aqueous hydrogen peroxide solution to form mixed solution, the mol ratio of metal titanium and hydrogen peroxide is 1:8 ~ 12, and described metal titanium is particle titanium sponge;
Step 2, glass beaker is placed in to ice-water bath, ice-water bath temperature is controlled between 5～15 DEG C, and middling speed stirs described mixed solution thing and forms intermediate reaction thing;
Step 3, a certain amount of ammoniacal liquor is poured in the flask with arm and piston, flask is placed in to hot water bath, bath temperature is controlled at 60 DEG C of left and right, heating makes ammonia volatilization form ammonia steam, this ammonia steam enters in intermediate reaction thing by arm, regulate interior acquisition of pH value to 8 ~ 11 scope of intermediate reaction thing to regulate rear intermediate reaction thing, now the mol ratio of metal titanium and ammonia is 1:9 ~ 15;
Intermediate reaction thing 3 ~ 8 hours after step 4, lasting stirring and adjusting, until obtain the transparent yellow complex aqueous solution;
Step 5, the yellow complex aqueous solution is transferred in the flask with arm, puts into the hot water bath of 60 DEG C of left and right, excessive hydrogen peroxide and ammonia are removed in evaporation, obtain yellow complex colloid;
Step 6, yellow complex colloid is poured in autoclave, 150 DEG C ~ 200 DEG C hydro-thermal reactions 4 ~ 8 hours, obtain pure white water-based emulsion;
Step 7, pure white water-based emulsion is refunded in glass beaker, under normal temperature, add while stirring mineral acid, regulate pH value to 2 ~ 4 of emulsion to obtain water-based emulsion after acidifying;
Step 8, glass beaker is put into 60～80 DEG C of water bath devices, continue to stir within 3～6 hours, make acidifying after water-based emulsion gradually gel become nanometer titanium dioxide water colloid.
In technique scheme, further improved plan is as follows:
1. in such scheme, in described aqueous hydrogen peroxide solution, content of hydrogen peroxide is 30%, proportion 1.1g/ml.
2. in such scheme, described middling speed stir speed (S.S.) is 300 ~ 600 revs/min.
3. in such scheme, described ammoniacal liquor content 26%, proportion 0.9g/ml.
4. in such scheme, the ammonia evaporating in described step 5 passes in pure water, recyclablely uses again.
5. in such scheme, described mineral acid is any one in dilute hydrochloric acid, dilute sulphuric acid or rare nitric acid.
Because technique scheme is used, the present invention compared with prior art has following advantages and effect:
The preparation method of high efficiency photocatalyst-nanometer titanium dioxide water colloid of the present invention, it is it is inorganic synthetic completely, does not use any organic solvent, in reaction process, produce without waste water, waste gas, be a kind of clean preparation technology; Secondly, adopt high-purity titanium sponge, aqueous hydrogen peroxide solution as main raw material and in conjunction with specific processing step and parameter, can make the theoretical earning rate of titanium dioxide up to 166%, raw materials cost reduces greatly compared with other patent technique, greatly reduce the probability of the introducing of raw material impurity, thereby improved the stability of product and purity and performance; Again, adopt the nanometer titanium dioxide water colloidal solid particle diameter prepared of the present invention to be less than 10 nanometers and uniform particles good, degree of crystallinity is high, has very strong photocatalytic activity; And the coating property on porous substrate and film forming properties are very good, can make high efficiency photocatalysis agent film, be applied in air and water purification field, can various poisonous, the harmful organic pollutants of oxygenolysis under the irradiation of UV-light, high and removal time of formaldehyde clearance shortens greatly, and sterilizing rate is high and the time is short simultaneously.
Brief description of the drawings
Accompanying drawing 1 amplifies 140,000 times of nano-TiOs for the present invention
2aqueous colloidal transmission electron microscope shape appearance figure;
Accompanying drawing 2 is nano-TiO of the present invention
2aqueous colloidal particle size distribution figure;
Application example--the Formaldehyde decomposition curve that accompanying drawing 3 is high efficiency photocatalyst of the present invention;
Application example--the sterilization effect curve that accompanying drawing 4 is high efficiency photocatalyst of the present invention.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1: a kind of preparation method of high efficiency photocatalyst-nanometer titanium dioxide water colloid, comprises the following steps:
Step 1,5 grams of metal titaniums are put into 500 milliliters of glass beakers, add 85 milliliters of aqueous hydrogen peroxide solutions, the mol ratio of metal titanium and hydrogen peroxide is 1:8, and described metal titanium is particle titanium sponge;
Step 2, glass beaker is placed in to ice-water bath, ice-water bath temperature is controlled at 10 DEG C of left and right, and middling speed stirs described mixed solution thing and forms intermediate reaction thing;
Step 3,75 milliliters of ammoniacal liquor are poured in 500 ml flasks with arm and piston, flask is placed in to the temperature control hot water bath of 60 DEG C of left and right, add thermosetting ammonia steam, ammonia steam enters by arm in the intermediate reaction thing of middling speed stirring, in the time that reaching 9 left and right, the pH value of intermediate reaction thing closes the piston on flask arm, stop logical ammonia, the mol ratio of metal titanium and ammonia is approximately 1:10;
Step 4, lasting stirring reaction 6 hours, can repeatedly open the piston on flask arm during this time, and logical ammonia, to keep pH value in 9 left and right, obtains transparent yellow complex TiO[(H
2o
2)]
2+the aqueous solution;
Step 5, by yellow complex TiO[(H
2o
2)]
2+the aqueous solution is transferred in the flask with arm, puts into the hot water bath of 60 DEG C of left and right, and excessive hydrogen peroxide and ammonia are removed in evaporation, obtain yellow complex colloid, and the ammonia evaporating passes in pure water, recyclablely uses again;
Step 6, yellow complex colloid is poured in autoclave, 150 DEG C of hydro-thermal reactions 8 hours, obtain lily Ti (OH) again
4water-based emulsion;
Step 7, by lily Ti (OH)
4water-based emulsion is refunded in glass beaker, drips while stirring rare nitric acid of 40% under normal temperature, water-based emulsion after the pH value of adjusting emulsion obtains acidifying within 2 ~ 2.5 scopes;
Step 8, glass beaker is put into heated for controlling temperature water bath device, bath temperature is controlled at 60 DEG C of left and right, churning time is 5 hours, continue stir under make acidifying after water-based emulsion gradually gel become nanometer titanium dioxide water colloid, heavily approximately 80 grams of left and right, in colloid, the content of titanium dioxide is approximately 10% wt.
In above-mentioned aqueous hydrogen peroxide solution, content of hydrogen peroxide is 30%, proportion 1.1g/ml, and above-mentioned middling speed stir speed (S.S.) is 400 revs/min;
Above-mentioned ammoniacal liquor content 26%, proportion 0.9g/ml; The ammonia evaporating in above-mentioned steps five passes in pure water, recyclablely uses again.
Fig. 1 is the nanometer titanium dioxide water colloid transmission electron microscope photo that the preparation method of the present embodiment high efficiency photocatalyst obtains, from photo, can show that particle presents near-spherical, particle diameter is less than the scale contrast of lower right corner 100nm in 10nm(and figure), the bright colloidal solid of right chart belongs to anatase phase.
Fig. 2 is the nanometer titanium dioxide water colloidal solid size distribution figure that the preparation method of the present embodiment high efficiency photocatalyst obtains, and average particulate diameter is less than 10nm.
Fig. 3 is that the nanometer titanium dioxide water colloid that the preparation method of the present embodiment high efficiency photocatalyst obtains sprays on porous ceramics base material, sintering is made high efficiency photocatalysis agent film, the Formaldehyde decomposition curve recording under ultraviolet light irradiation, mechanism for testing is Chinese environmental and energy nano material development center, through the light-catalyzed reaction of 60 minutes, concentration of formaldehyde drops to 0.05ppm from initial 1.05ppm, and clearance is high and the removal time is short.
Fig. 4 is that the nanometer titanium dioxide water colloid that the preparation method of the present embodiment high efficiency photocatalyst obtains sprays on porous ceramics base material, sintering is made high efficiency photocatalysis agent film, the sterilization effect curve recording under ultraviolet light irradiation, Environment in Shanghai protection product quality supervision and inspection master station is detected, test condition: 23 ~ 27 DEG C of temperature, relative humidity 40 ~ 60%, 30 cubic metres of experimental cabins of the test space; Draw total bacterium clearance from accompanying drawing 4: 30 minutes, exceed 70%; 60 minutes, exceed 99%.
Embodiment 2: a kind of preparation method of high efficiency photocatalyst-nanometer titanium dioxide water colloid, comprises the following steps:
Step 1,5 grams of metal titaniums are put into glass beaker, add 107mL aqueous hydrogen peroxide solution to form mixed solution, the mol ratio of metal titanium and hydrogen peroxide is 1:10, and described metal titanium is particle titanium sponge;
Step 2, glass beaker is placed in to ice-water bath, ice-water bath temperature is controlled between 12 DEG C, and middling speed stirs described mixed solution thing and forms intermediate reaction thing;
Step 3, the ammoniacal liquor of 91mL is poured in the flask with arm and piston, flask is placed in to hot water bath, bath temperature is controlled at 60 DEG C of left and right, heating makes ammonia volatilization form ammonia steam, this ammonia steam enters in intermediate reaction thing by arm, in pH value to 9.5 scope of adjusting intermediate reaction thing, obtain and regulate rear intermediate reaction thing, now the mol ratio of metal titanium and ammonia is 1:12;
Intermediate reaction thing 5 hours after step 4, lasting stirring and adjusting, until obtain transparent yellow complex TiO[(H
2o
2)]
2+the aqueous solution;
Step 5, the yellow complex aqueous solution is transferred in the flask with arm, puts into the hot water bath of 60 DEG C of left and right, excessive hydrogen peroxide and ammonia are removed in evaporation, obtain yellow complex colloid;
Step 6, yellow complex colloid is poured in autoclave, 175 DEG C of hydro-thermal reactions 7 hours, obtain pure white Ti (OH)
4water-based emulsion;
Step 7, by pure white Ti (OH)
4water-based emulsion is refunded in glass beaker, adds while stirring mineral acid under normal temperature, water-based emulsion after pH value to the 3.0 ~ 3.5 acquisition acidifying of adjusting emulsion;
Step 8, glass beaker is put into 70 DEG C of water bath devices, continue to stir within 4.5 hours, make acidifying after water-based emulsion gradually gel become nanometer titanium dioxide water colloid, heavily approximately 110 grams of left and right, in colloid, the content of titanium dioxide is approximately 7.6% wt.
As preferably, the metal titanium of employing is particle titanium sponge, has greatly reduced the probability of the introducing of raw material impurity, thereby improves the stability of product and purity and performance.
As preferably, adopt in step 3 flask is placed in to hot water bath, bath temperature is controlled at 60 DEG C of left and right, and heating makes ammonia volatilization form ammonia steam, and this ammonia steam enters in intermediate reaction thing by arm.Adopting the way of leading to ammonia instead of dripping ammoniacal liquor to regulate the reason of pH value is in order to keep the concentration of hydrogen peroxide in reactant, avoids dripping ammoniacal liquor meeting dilute reaction solution, thereby can make speed of response reduce, and the reaction times increases.
Above-described embodiment is only explanation technical conceive of the present invention and feature, and its object is to allow person skilled in the art can understand content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences that spirit is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.
Claims (6)
1. a preparation method for high efficiency photocatalyst-nanometer titanium dioxide water colloid, is characterized in that: comprise the following steps:
Step 1, metal titanium is put into glass beaker, add aqueous hydrogen peroxide solution to form mixed solution, the mol ratio of metal titanium and hydrogen peroxide is 1:8 ~ 12, and described metal titanium is particle titanium sponge;
Step 2, glass beaker is placed in to ice-water bath, ice-water bath temperature is controlled between 5～15 DEG C, and middling speed stirs described mixed solution thing and forms intermediate reaction thing;
Step 3, a certain amount of ammoniacal liquor is poured in the flask with arm and piston, flask is placed in to hot water bath, bath temperature is controlled at 60 DEG C of left and right, heating makes ammonia volatilization form ammonia steam, this ammonia steam enters in intermediate reaction thing by arm, regulate in pH value to 8 ~ 11 scope of intermediate reaction thing, obtain and regulate rear intermediate reaction thing, now the mol ratio of metal titanium and ammonia is 1:9 ~ 15;
Intermediate reaction thing 3 ~ 8 hours after step 4, lasting stirring and adjusting, until obtain the transparent yellow complex aqueous solution;
Step 5, the yellow complex aqueous solution is transferred in the flask with arm, puts into the hot water bath of 60 DEG C of left and right, excessive hydrogen peroxide and hydrogen peroxide ammonia are removed in evaporation, obtain yellow complex colloid;
Step 6, yellow complex colloid is poured in autoclave, 150 DEG C ~ 200 DEG C hydro-thermal reactions 4 ~ 8 hours, obtain pure white water-based emulsion;
Step 7, pure white water-based emulsion is refunded in glass beaker, under normal temperature, add while stirring mineral acid, regulate pH value to 2～4 of emulsion to obtain water-based emulsion after acidifying;
Step 8, glass beaker is put into 60～80 DEG C of water bath devices, continue to stir within 3～6 hours, make after acidifying water-based emulsion gradually gel become nanometer titanium dioxide water colloid.
2. the preparation method of high efficiency photocatalyst-nanometer titanium dioxide water colloid according to claim 1, is characterized in that: in described aqueous hydrogen peroxide solution, content of hydrogen peroxide is 30%, proportion 1.1g/ml.
3. the preparation method of high efficiency photocatalyst-nanometer titanium dioxide water colloid according to claim 1, is characterized in that: described middling speed stir speed (S.S.) is 300 ~ 600 revs/min.
4. the preparation method of high efficiency photocatalyst-nanometer titanium dioxide water colloid according to claim 1, is characterized in that: described ammoniacal liquor content 26%, proportion 0.9g/ml.
5. the preparation method of high efficiency photocatalyst-nanometer titanium dioxide water colloid according to claim 1, is characterized in that: the hydrogen peroxide evaporating in described step 5 and ammonia pass in pure water, recyclablely uses again.
6. the preparation method of high efficiency photocatalyst-nanometer titanium dioxide water colloid according to claim 1, is characterized in that: described mineral acid is any one in dilute hydrochloric acid, dilute sulphuric acid or rare nitric acid.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104477987A (en) * | 2014-12-12 | 2015-04-01 | 中国科学院过程工程研究所 | Clean production method of high-purity titanium dioxide |
| CN106629835A (en) * | 2016-11-18 | 2017-05-10 | 浙江理工大学 | Controllable preparation method of titanium dioxide nanoparticles |
| CN107473770A (en) * | 2017-06-27 | 2017-12-15 | 伦慧东 | The manufacture craft of photocatalyst film composite ceramics |
| WO2022007764A1 (en) * | 2020-07-06 | 2022-01-13 | 宁波极微纳新材料科技有限公司 | Method for preparing titanium dioxide and method for improving titanium dioxide dispersibility |
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| JP2007246301A (en) * | 2006-03-13 | 2007-09-27 | Matsumoto Fine Chemical Co Ltd | Method for producing brookite-type titanium dioxide |
| CN102730754A (en) * | 2012-06-07 | 2012-10-17 | 江苏恒智纳米科技有限公司 | Preparation method of aqueous nano-TiO2 colloid |
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| JP2006182616A (en) * | 2004-12-28 | 2006-07-13 | Tohoku Univ | Method of manufacturing water-soluble titanium compound and manufacturing method of titanium oxide powder using it |
| JP2007246301A (en) * | 2006-03-13 | 2007-09-27 | Matsumoto Fine Chemical Co Ltd | Method for producing brookite-type titanium dioxide |
| CN102730754A (en) * | 2012-06-07 | 2012-10-17 | 江苏恒智纳米科技有限公司 | Preparation method of aqueous nano-TiO2 colloid |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104477987A (en) * | 2014-12-12 | 2015-04-01 | 中国科学院过程工程研究所 | Clean production method of high-purity titanium dioxide |
| CN104477987B (en) * | 2014-12-12 | 2016-04-06 | 中国科学院过程工程研究所 | A kind of clean preparation method of high-purity titanium dioxide |
| CN106629835A (en) * | 2016-11-18 | 2017-05-10 | 浙江理工大学 | Controllable preparation method of titanium dioxide nanoparticles |
| CN106629835B (en) * | 2016-11-18 | 2018-03-23 | 浙江理工大学 | A kind of controllable method for preparing of titania nanoparticles |
| CN107473770A (en) * | 2017-06-27 | 2017-12-15 | 伦慧东 | The manufacture craft of photocatalyst film composite ceramics |
| WO2022007764A1 (en) * | 2020-07-06 | 2022-01-13 | 宁波极微纳新材料科技有限公司 | Method for preparing titanium dioxide and method for improving titanium dioxide dispersibility |
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