CN102765751A - Preparation method of nanometer titanium dioxide - Google Patents
Preparation method of nanometer titanium dioxide Download PDFInfo
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- CN102765751A CN102765751A CN2012102435564A CN201210243556A CN102765751A CN 102765751 A CN102765751 A CN 102765751A CN 2012102435564 A CN2012102435564 A CN 2012102435564A CN 201210243556 A CN201210243556 A CN 201210243556A CN 102765751 A CN102765751 A CN 102765751A
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Abstract
The invention provides a preparation method of nanometer titanium dioxide, and relates to the preparation field of inorganic chemical materials. In the method, metatitanic acid intermediate from titanium dioxide preparation by a sulfur acid process is used as a raw material, and nanometer titanium dioxide is prepared through technical processes of pulping, dispersing, filter pressing, calcining and crushing. Compared with a prior art, the preparation method provided by the invention has the beneficial effects as follows: a selective catalytic reduction (SCR) denitration catalyst made of nanometer titanium dioxide provided by the invention is more applicable to coal characteristics and smoke conditions of domestic coal-fired power plants, beneficial to controlling the production of various raw materials in catalyst production companies and effectively reducing the production cost of the catalyst; and the catalyst made of the product provided by the invention is better adapted to smoke characteristics of the domestic coal-fired power plants and achieves higher denitration efficiency.
Description
Technical field
The present invention relates to the preparation method of inolrganic chemicals, particularly a kind of preparation method of nano titanium oxide.
Background technology
Oxynitride (NOx) is one of main atmospheric polluting material, is the important presoma that brings out photo-chemical smog and acid rain, sets up low-carbon (LC) and environmentally friendly Economic development mode is imperative.Wherein coal power station, Industrial Boiler flue gas are the largest sources of NOx, and it accounts for total NOx quantity discharged about 60%.Classify the NOx quantity discharged as restrictive index clearly in country's " 12 " planning outline draft; Time and the NOx emission standard in " thermal power plant's atmosphere pollutants emission standards " (carrying out on January 1st, 2012) of national environmental protection portion in July, 2011 promulgation simultaneously thermal power plant's denitration implemented have all had more strict requirement, explicitly call for the newly-built existing thermal power plant discharged nitrous oxides that reaches to be controlled at 100mg/Nm
3In.Therefore denitrating catalyst market is about to extensive the startup, and state inner catalyst market has explosive growth.Ammine selectivity catalytic reduction technology (NH
3-SCR) be present both at home and abroad denitration industry one preferred technique, also having only this method can satisfy the fuel-burning power plant can qualified discharge when high environmental protection standard-required.Catalyzer is the core of SCR denitration technology, is the most key technology fully and account for the nano TiO 2 carrying system of catalyst weight more than 80%.Nano titanium oxide is ideal catalyst support materials because of characteristics such as its typical vesicular structure and high thermal stabilities.
The nano titanium oxide that at present is used to prepare denitrating catalyst is mostly from external import, not only wastes more foreign exchange but also seriously restricts the development of denitration environmental protection industry.Simultaneously, restrict because of receiving many objective factors such as resource characteristics, imbalance between supply and demand, the ature of coal that domestic coal power station uses is uneven, causes flue gas condition such as NOx, SO
2, the ash index of grading is also comparatively harsh, then uses the catalyzer of import nano titanium oxide preparation " not acclimatized " phenomenon to occur.
Summary of the invention
The present invention proposes a kind of preparation method of nano titanium oxide; Solved deficiency of the prior art; The SCR denitrating catalyst that utilizes the nano titanium oxide among the present invention to prepare more is applicable to domestic flue gas condition, has reduced the cost of making, and is stronger to the characteristics flexibility of domestic coal steam-electric plant smoke; Cost is lower, and denitration efficiency is high.
Technical scheme of the present invention is achieved in that
A kind of preparation method of nano titanium oxide, it is a raw material with the midbody metatitanic acid of method for producing gtitanium dioxide with sulphuric acid, through the technological process of making beating, dispersion, press filtration, calcining and pulverizing, prepares nano titanium oxide.
As preferably, the technology of said making beating does, metatitanic acid is added the deionized water making beating, and to be diluted to concentration be 7-9%, stirs 0.5-1h.
As preferably, said dispersive technology does, adds in the slurries behind ammoniacal liquor or volatile salt to the beating process, and adjustment slurry environments pH value is 6-8, and slurries are heated to 70-80 ℃, and stirring 2-3h once disperses fully slurries; Add dispersion agent then, addition stirs 1h by in titanium oxide quality 0.5%, the slurries secondary is disperseed and the maintenance dispersion state.
As preferably, the technology of said press filtration does, the slurries after the press filtration dispersing technology is handled make solid content be controlled at 40-50%, filter cake.
As preferably, said incinerating technology is that the filter cake behind the filter-pressing process is calcined 9h under 110-570 ℃ of condition.
As preferably, the technology of said pulverizing does, solids behind the calcining process is pulverized, and particle diameter is controlled at 0.8-1.6um.
As preferably, the dispersion agent that adds in the said dispersing technology process is the yellow thiamines of ammonium citrate, Sodium hexametaphosphate 99 or pentadecyl.
As preferably, the filter cake behind the filter-pressing process is calcined 9h under 110-570 ℃ of condition, be specially: filter cake is calcined 2h down at 110-250 ℃; Calcine 2h down at 250-350 ℃ then; Continuation is calcined 2h down at 350-480 ℃; Calcine 3h down at 480-570 ℃ at last.
The key technical index of the nano titanium oxide that the method among utilization the present invention is produced is:
Grain fineness number: 10-22nm
SO
4 2-Content: 0.7-3.5wt% (dry)
Specific surface area: 70-100m
2/ g
Aggregation size: 0.8-1.6um
Compared with prior art, the invention has the beneficial effects as follows:
1, the selection wide material sources of main raw material, the price of metatitanic acid is lower, and the source is wide, has reduced manufacturing cost;
2, use the titanium oxide among the present invention to prepare the fine flue gas condition that is applicable to domestic harshness of SCR denitrating catalyst ability, stronger to the characteristics flexibility of domestic coal steam-electric plant smoke, cost is lower, and denitration efficiency is high;
3, this product cleaner production, the production process environmental pollution is little;
4, improve the technology content of ordinary titanium powder simultaneously, promoted industrial upgrading, widened the industry chain (supply chain) in denitration environmental protection and titanium white field.Common white titanium pigment is had many uses general: coating, pigment, papermaking, rubber, food, medicine etc., but can not be used for the preparation of denitrating catalyst.
Embodiment
Embodiment 1:
Take by weighing the 25kg metatitanic acid and (amount to TiO
2Meter, this raw material TiO
2Content is about 28%), place the reaction kettle that disposes whisking appliance, add about 223kg deionized water and make slurries TiO
2Content is about 8%, stirs 0.5h; In slurries, add ammoniacal liquor adjustment pH value to 6, with steam slurries are heated to 70 ℃, insulation is also stirred 2.0h, and an amount of simultaneously ammoniacal liquor that replenishes makes slurries pH maintain 6; In slurries, add the 0.125kg ammonium citrate, stir 1h; Slurries are about 40% packaged filter cake through press filtration to solid content; With the filter cake calcining, wherein calcine 2h, 250 ℃ of calcining 2h, 350 ℃ of calcining 2h, 480 ℃ of calcining 3h for 150 ℃; It is 1.22um that solid after the calcining is crushed to particle diameter D50 through powder beater, obtains the nanometer titanium dioxide titanium products.
Embodiment 2:
Take by weighing the 25kg metatitanic acid and (amount to TiO
2Meter, this raw material TiO
2Content is about 28%), place the reaction kettle that disposes whisking appliance, add about 223kg deionized water and make slurries TiO2 content be about 8%, stir 0.8h; In slurries, add ammoniacal liquor adjustment pH value to 7, with steam slurries are heated to 70 ℃, insulation is also stirred 2.5h, and an amount of simultaneously ammoniacal liquor that replenishes makes slurries pH maintain 7; In slurries, add the 0.125kg ammonium citrate, stir 1h; Slurries are about 50% packaged filter cake through press filtration to solid content; With the filter cake calcining, wherein calcine 2h, 300 ℃ of calcining 2h, 400 ℃ of calcining 2h, 490 ℃ of calcining 3h for 180 ℃; It is 1.15um that solid after the calcining is crushed to particle diameter D50 through powder beater, obtains the nanometer titanium dioxide titanium products.
Embodiment 3:
Take by weighing the 25kg metatitanic acid and (amount to TiO
2Meter, this raw material TiO
2Content is about 28%), place the reaction kettle that disposes whisking appliance, add about 188kg deionized water and make slurries TiO2 content be about 9%, stir 1h; In slurries, add volatile salt pH value to 7, with steam slurries are heated to 75 ℃, insulation is also stirred 2.5h, and an amount of simultaneously volatile salt that replenishes makes slurries pH maintain 7; In slurries, add the yellow thiamines of 0.125kg pentadecyl, stir 1h; Slurries are about 45% packaged filter cake through press filtration to solid content; With the filter cake calcining, wherein calcine 2h, 300 ℃ of calcining 2h, 390 ℃ of calcining 2h, 520 ℃ of calcining 3h for 150 ℃; It is 1.38um that solid after the calcining is crushed to particle diameter D50 through powder beater, obtains the nanometer titanium dioxide titanium products.
Embodiment 4:
Take by weighing the 25kg metatitanic acid and (amount to TiO
2Meter, this raw material TiO
2Content is about 28%), place the reaction kettle that disposes whisking appliance, add about 188kg deionized water and make slurries TiO2 content be about 9%, stir 1h; In slurries, add ammoniacal liquor adjustment pH value to 8, with steam slurries are heated to 80 ℃, insulation is also stirred 2.5h, and an amount of simultaneously ammoniacal liquor that replenishes makes slurries pH maintain 8; In slurries, add the 0.125kg ammonium citrate, stir 1h; Slurries are about 50% packaged filter cake through press filtration to solid content; With the filter cake calcining, wherein calcine 2h, 280 ℃ of calcining 2h, 400 ℃ of calcining 2h, 500 ℃ of calcining 3h for 130 ℃; It is 1.29um that solid after the calcining is crushed to particle diameter D50 through powder beater, obtains the nanometer titanium dioxide titanium products.
Embodiment 5:
Take by weighing the 25kg metatitanic acid and (amount to TiO
2Meter, this raw material TiO
2Content is about 28%), place the reaction kettle that disposes whisking appliance, add about 268kg deionized water and make slurries TiO2 content be about 7%, stir 1h; In slurries, add volatile salt adjustment pH value to 8, with steam slurries are heated to 80 ℃, insulation is also stirred 3h, and an amount of simultaneously volatile salt that replenishes makes slurries pH maintain 8; In slurries, add the 0.125kg Sodium hexametaphosphate 99, stir 1h; Slurries are about 50% packaged filter cake through press filtration to solid content; With the filter cake calcining, wherein calcine 2h, 270 ℃ of calcining 2h, 420 ℃ of calcining 2h, 550 ℃ of calcining 3h for 130 ℃; It is 1.34um that solid after the calcining is crushed to particle diameter D50 through powder beater, obtains the nanometer titanium dioxide titanium products.
The technology of preparation SCR denitrating catalyst is: the nano titanium oxide for preparing among the present invention and other various raw materials are prepared burden by formula rate is strict; Preparing the back mixer, to carry out mixed at high speed even; It is mixing to carry out the filtering type extruding with special-purpose pre-filtering forcing machine again through the raw material after preliminary mixing; The blank that refining is good is put frame base car and is carried out the ageing of certain hour; Blank after ageing gets into the powerful vacuum forcing machine again and is squeezed into the successive green honeycomb body, through synchronization cutting mechanism cutting automatically (Cutting Length of general base substrate is 1200-1500mm), is removed automatically to printed line by manipulator fixture through the honeycomb base substrate behind the well cutting more again; And then bring up to drying cart by automatic carrying machine working together with printed line; Base substrate through the microwave drying of preserving moisture of hyperchannel high temperature, gets in the net belt type low temperature electrical kiln and burns till (other kiln also can) at last on drying cart, promptly prepare the SCR denitrating catalyst.
The index of above-mentioned embodiment product and its preparation catalyst applications performance is as shown in the table:
Claims (8)
1. the preparation method of a nano titanium oxide, it is characterized in that: it is a raw material with the midbody metatitanic acid of method for producing gtitanium dioxide with sulphuric acid, through the technological process of making beating, dispersion, press filtration, calcining and pulverizing, prepares nano titanium oxide.
2. the preparation method of nano titanium oxide according to claim 1 is characterized in that: the technology of said making beating does, metatitanic acid is added the deionized water making beating, and to be diluted to concentration be 7-9%, stirs 0.5-1h.
3. the preparation method of nano titanium oxide according to claim 1; It is characterized in that: said dispersive technology does; In the slurries behind interpolation ammoniacal liquor or volatile salt to the beating process, adjustment slurry environments pH value is 6-8, and slurries are heated to 70-80 ℃; Stir 2-3h, slurries are once disperseed fully; Add dispersion agent then, addition stirs 1h by in titanium oxide quality 0.5%, the slurries secondary is disperseed and the maintenance dispersion state.
4. the preparation method of nano titanium oxide according to claim 1 is characterized in that: the technology of said press filtration does, the slurries after the press filtration dispersing technology is handled make solid content be controlled at 40-50%, filter cake.
5. the preparation method of nano titanium oxide according to claim 1, it is characterized in that: said incinerating technology is that the filter cake behind the filter-pressing process is calcined 9h under 110-570 ℃ of condition.
6. the preparation method of nano titanium oxide according to claim 1 is characterized in that: the technology of said pulverizing does, solids behind the calcining process is pulverized, and particle diameter is controlled at 0.8-1.6um.
7. the preparation method of nano titanium oxide according to claim 3 is characterized in that: the dispersion agent that adds in the said dispersing technology process is the yellow thiamines of ammonium citrate, Sodium hexametaphosphate 99 or pentadecyl.
8. the preparation method of nano titanium oxide according to claim 5 is characterized in that: the filter cake behind the filter-pressing process is calcined 9h under 110-570 ℃ of condition, be specially: filter cake is calcined 2h down at 110-250 ℃; Calcine 2h down at 250-350 ℃ then; Continuation is calcined 2h down at 350-480 ℃; Calcine 3h down at 480-570 ℃ at last.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105385205A (en) * | 2015-12-30 | 2016-03-09 | 唐伟 | Anti-corrosion antibacterial nano coating |
| CN105504915A (en) * | 2015-12-30 | 2016-04-20 | 唐伟 | Wear-resisting and antibacterial nano paint |
| CN106362730A (en) * | 2016-10-12 | 2017-02-01 | 清华大学 | Preparing method for vanadium based composite titanium dioxide catalyst used in ammonium bisulfate decomposition during De-NOxDenitration |
| CN109928425A (en) * | 2019-04-23 | 2019-06-25 | 广西民族大学 | A method of it reducing metatitanic acid and is converted into rutile titanium dioxide calcination temperature |
| CN111362302A (en) * | 2020-03-18 | 2020-07-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing nano titanium dioxide |
| CN114014355A (en) * | 2021-09-16 | 2022-02-08 | 攀枝花学院 | Method for purifying and deironing industrial metatitanic acid |
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| CN101029187A (en) * | 2006-03-03 | 2007-09-05 | 攀钢集团攀枝花钢铁研究院 | High-water-dispersibility titanium dioxide and preparation method thereof |
| CN101318697A (en) * | 2008-07-11 | 2008-12-10 | 四川华铁钒钛科技股份有限公司 | Method for preparing titanium dioxide product for high-specific surface area denitrating catalyst |
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2012
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Patent Citations (2)
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| CN101029187A (en) * | 2006-03-03 | 2007-09-05 | 攀钢集团攀枝花钢铁研究院 | High-water-dispersibility titanium dioxide and preparation method thereof |
| CN101318697A (en) * | 2008-07-11 | 2008-12-10 | 四川华铁钒钛科技股份有限公司 | Method for preparing titanium dioxide product for high-specific surface area denitrating catalyst |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105385205A (en) * | 2015-12-30 | 2016-03-09 | 唐伟 | Anti-corrosion antibacterial nano coating |
| CN105504915A (en) * | 2015-12-30 | 2016-04-20 | 唐伟 | Wear-resisting and antibacterial nano paint |
| CN106362730A (en) * | 2016-10-12 | 2017-02-01 | 清华大学 | Preparing method for vanadium based composite titanium dioxide catalyst used in ammonium bisulfate decomposition during De-NOxDenitration |
| CN109928425A (en) * | 2019-04-23 | 2019-06-25 | 广西民族大学 | A method of it reducing metatitanic acid and is converted into rutile titanium dioxide calcination temperature |
| CN109928425B (en) * | 2019-04-23 | 2021-09-17 | 广西民族大学 | Method for reducing calcination temperature of metatitanic acid converted into rutile type titanium dioxide |
| CN111362302A (en) * | 2020-03-18 | 2020-07-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing nano titanium dioxide |
| CN111362302B (en) * | 2020-03-18 | 2022-07-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing nano titanium dioxide |
| CN114014355A (en) * | 2021-09-16 | 2022-02-08 | 攀枝花学院 | Method for purifying and deironing industrial metatitanic acid |
| CN114014355B (en) * | 2021-09-16 | 2023-07-25 | 攀枝花学院 | Industrial meta-titanic acid purifying and deironing method |
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Application publication date: 20121107 |