CN104477984A - Preparation method of nano titanium dioxide serving as flue gas denitrification catalyst - Google Patents
Preparation method of nano titanium dioxide serving as flue gas denitrification catalyst Download PDFInfo
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- CN104477984A CN104477984A CN201410671796.3A CN201410671796A CN104477984A CN 104477984 A CN104477984 A CN 104477984A CN 201410671796 A CN201410671796 A CN 201410671796A CN 104477984 A CN104477984 A CN 104477984A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000003054 catalyst Substances 0.000 title claims abstract description 16
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 239000003546 flue gas Substances 0.000 title claims abstract description 13
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title abstract description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 99
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 47
- 239000002253 acid Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000001914 filtration Methods 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 12
- 150000004767 nitrides Chemical class 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000004062 sedimentation Methods 0.000 claims description 9
- 238000000967 suction filtration Methods 0.000 claims description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- 229910019142 PO4 Inorganic materials 0.000 claims description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 7
- 239000012065 filter cake Substances 0.000 claims description 7
- 229910001385 heavy metal Inorganic materials 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 229910021645 metal ion Inorganic materials 0.000 claims description 7
- 239000010452 phosphate Substances 0.000 claims description 7
- 239000011591 potassium Substances 0.000 claims description 7
- 229910052700 potassium Inorganic materials 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 6
- 230000005484 gravity Effects 0.000 claims description 6
- -1 phosphate anion Chemical class 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- GJEAMHAFPYZYDE-UHFFFAOYSA-N [C].[S] Chemical compound [C].[S] GJEAMHAFPYZYDE-UHFFFAOYSA-N 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims description 3
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- 238000002798 spectrophotometry method Methods 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000012467 final product Substances 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 239000007858 starting material Substances 0.000 abstract 1
- 235000010215 titanium dioxide Nutrition 0.000 description 36
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000003245 working effect Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Landscapes
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a preparation method of nano titanium dioxide serving as a flue gas denitrification catalyst. The preparation method comprises the following steps: completing purification of a raw material, namely metatitanic acid (also known as hydrated titanium dioxide) produced by a sulfuric acid method and used as a starting material, through pH value regulating, washing and filtering, dehydrating and drying the metatitanic acid, and then grinding, sieving and packaging to obtain the final product. The preparation method is simple in process and materials. The prepared nano titanium dioxide is large in specific surface area and high in TiO2 content.
Description
[technical field]
The present invention relates to a kind of preparation method of nano material, particularly a kind of preparation method of catalyst for denitrating flue gas nanometer titanium dioxide.
[background technology]
Catalyzed reaction is a surface reaction, and the speed of reaction depends on the surface contact degree of reactant and catalyst exposure, and for catalyst Ti white powder, specific surface area is larger, TiO
2content higher, foreign matter content is lower, and catalytic effect is better, and this is the most important index weighing titanium dioxide quality, and the nanometer titanium dioxide that art methods makes has following defect:
1. comprise in properties-correcting agent, buffer reagent, dispersion agent, inhibitor, promotor, sequestering agent, additive one or more, these on-catalytic working substances occupy the certain proportion of the total substances content of titanium dioxide, make TiO
2content not high enough, catalytic effect is good, to be improved not;
2. making method is rigorous not, and the titanium dioxide specific surface area of preparation is large, to be improved not.
[summary of the invention]
The object of the present invention is to provide the preparation TiO of a kind of low cost, convenient operation
2purity is high, the method for the titanium dioxide that specific surface area is large, to solve complex process, TiO in prior art titanium dioxide
2the large not problem of the not high enough and titanium dioxide specific surface area of content.
The technical solution used in the present invention is: a kind of preparation method of catalyst for denitrating flue gas nanometer titanium dioxide, comprises the steps:
A. the source of metatitanic acid: the metatitanic acid (also referred to as hydrated titanium dioxide) produced by sulfuric acid process, suspended nitride directly can enter lower step link; Generally remove portion of water wherein by the mode of sedimentation and suction filtration or press filtration, obtain by percentage to the quality: moisture between 45% ~ 95%, dry product TiO
2the filter cake of % > 90%;
B. adjusted to ph: the slurry in A or filter cake are mixed with deionized water by 1:2-5 volume ratio, are uniformly dispersed, adds alkali lye, the pH value of adjustment slurry, the pH value of sampling acidometer or pH detection paper solution; Repeat above-mentionedly to add alkali lye, stirring and detecting step, until obtain the metatitanic acid suspended nitride that pH is 6.5 ~ 9;
C. wash, filter: by the mode of sedimentation, filtration be the moisture removal in the metatitanic acid suspended nitride of 6.5 ~ 9 by above-mentioned pH; Remove the metatitanic acid material of most of moisture or rear deionized water wash of again pulling an oar, or wash online with deionized water, then again removed the moisture in suspended nitride by the mode of gravity settling or centrifugal settling, suction filtration or press filtration, repeatedly wash and dewater; The method surveying filtrate specific conductivity is all adopted indirectly to control ionic concn after each washing, when filtrate specific conductivity is lower than 1000us/cm, use sampling instead to detect and repeated washing control ionic concn, until obtain sulfate ion content < 0.9%, phosphate anion content < 0.4%, the metatitanic acid of the equal < 100ppm of content of the metal ions such as heavy metal and potassium, sodium, iron;
D. dry: above-mentioned washing to be removed the metatitanic acid material after portion of water between bake out temperature-20 DEG C ~ 280 DEG C, between pressure-0.1MPa ~ 1MPa, carry out oven dry 1 ~ 30 hour;
E. pulverize, sieve: above-mentioned titanium dioxide is cooled to-20 DEG C ~ room temperature, carry out pulverization process with pulverizer, with 200-500 eye mesh screen or air classification or cyclone classifiedly to sieve, obtain product nanometer titanium dioxide, described nanometer titanium dioxide TiO
2content is between 75% ~ 99%, and the specific surface area of powder is 180 ~ 360m
2/ g;
F. pack: in clean, clean environment, nanometer titanium dioxide is packed.
Further technical scheme of the present invention is: described alkali lye refers to sodium hydroxide, potassium hydroxide in stepb, one or more solution in Trimethylamine 99, triethylamine and ammoniacal liquor; With common alkali lye, complete the adjustment of pH value, cost is low.
Further technical scheme of the present invention is: sedimentation described in step C comprises one or more modes in gravity settling and centrifugal settling, and described filtration comprises one or more modes in suction filtration and press filtration.
Further technical scheme of the present invention is: sample detection described in step C and comprise: detect total sulfur content with carbon sulphur instrument, under wavelength 700nm, detect phosphate content with spectrophotometry, detect the content of heavy metal and potassium, sodium, iron, metal ion with AAS or AES or ICP-AES or ICP-MS; Accurately detect with instrument, be convenient to control ion content, thus improve the quality of products.
Further technical scheme of the present invention is: dry described in step D and comprise freeze-drying, vacuum-drying, one or more methods in air stream drying, spraying dry; Use industrial conventional drying method, remove moisture, be convenient to powder process.
Further technical scheme of the present invention is: pulverizer described in step e is one or more in micronizer mill, Universalpulverizer, Raymond mill, shearing crusher, impact grinder.
The invention has the beneficial effects as follows: owing to adopting technique scheme, preparation method's technique of the present invention and material simply, prepare gained nanometer titanium dioxide specific surface area large, TiO
2content is high.
[embodiment]
Below in conjunction with embodiment, the present invention is described further.
The invention provides a kind of preparation method of catalyst for denitrating flue gas nanometer titanium dioxide, comprise the steps:
A. the source of metatitanic acid: the metatitanic acid (also referred to as hydrated titanium dioxide) produced by sulfuric acid process, suspended nitride directly can enter lower step link; Generally remove portion of water wherein by the mode of sedimentation and suction filtration or press filtration, obtain by percentage to the quality: moisture between 45% ~ 95%, dry product TiO
2the filter cake of % > 90%;
During filtration, most of moisture can be filtered out, foreign ion major part contained in solution washed away, moisture is between 45 ~ 55% simultaneously, the molecular structure of metatitanic acid crystallization and globule size are suitable for, moisture is too low, and grain size number is excessive, and subsequent disposal can have influence on specific surface area, moisture is too high, explanation press filtration is insufficient, can consume more heat transfer, TiO in the treating processes of subsequent step
2% > 36%, ensures the purity of metatitanic acid.
B. adjusted to ph: the slurry in A or filter cake are mixed with deionized water by 1:2-5 volume ratio, are uniformly dispersed, adds alkali lye, the pH value of adjustment slurry, the pH value of sampling acidometer or pH detection paper solution; Repeat above-mentionedly to add alkali lye, stirring and detecting step, until obtain the metatitanic acid suspended nitride that pH is 6.5 ~ 9; Preferably, pH value is 7 or 8;
Potential of hydrogen too high or too low work-ing life that can affect product, pH between 6.5-9, TiO
2potential of hydrogen control in neutral or weakly alkaline, long service life.
C. wash, filter: by the mode of sedimentation, filtration be the moisture removal in the metatitanic acid suspended nitride of 6.5 ~ 9 by above-mentioned pH; Remove the metatitanic acid material of most of moisture or rear deionized water wash of again pulling an oar, or wash online with deionized water, then again removed the moisture in suspended nitride by the mode of gravity settling or centrifugal settling, suction filtration or press filtration, repeatedly wash and dewater; The method surveying filtrate specific conductivity is all adopted indirectly to control ionic concn after each washing, when filtrate specific conductivity is lower than 1000us/cm, use sampling instead to detect and repeated washing control ionic concn, until obtain sulfate ion content < 0.9%, phosphate anion content < 0.4%, the metatitanic acid of the equal < 100ppm of content of the metal ions such as heavy metal and potassium, sodium, iron; Preferably, sulfate ion content is 0.1%, 0.3% or 0.6%, and phosphate anion content is 0.1% or 0.3%, and the content of each heavy metal species and potassium, sodium, iron, metal ion can be all 15ppm, 30ppm, 50ppm, 70ppm or 80ppm;
Above-mentioned ionic concn can affect TiO
2purity, and in use can cause poisoning of catalyst, reduce work-ing life, each ionic concn controls, in above-mentioned scope, improve the purity of titanium dioxide and increase the service life.
D. dry: above-mentioned washing to be removed the metatitanic acid material after portion of water between bake out temperature-20 DEG C ~ 280 DEG C, between pressure-0.1MPa ~ 1MPa, carry out oven dry 1 ~ 30 hour; Preferably, bake out temperature is-15 DEG C, 0 DEG C, 100 DEG C or 180 DEG C, and pressure is-0.09MPa, 0MPa or 1MPa, and drying time is 5 hours, 15 hours or 30 hours;
Preferably, time dry, first adopt convection current hot blast to dry to the metatitanic acid after described washing, remove after preset value until moisture content, described metatitanic acid is stirred, again carries out convection current hot-air seasoning, obtain titanium dioxide; Then, after preliminarily being pulverized by drier titanium dioxide, send in holding furnace and dry, now bake out temperature remains between 50-80 degree; Because raw material metatitanic acid is in block, if carry out flash baking, titanium dioxide is easily caused to lump, really up to the mark, reunite.Therefore, before feeding holding furnace, first preliminarily pulverize filter cake, make its bulk less, then send in holding furnace, with lesser temps, 50-80 degree as above is incubated; Further removal moisture wherein, simultaneously owing to have employed the mode of low-temperature insulation, the crystalline structure of described titanium dioxide is more loose, brilliant formation of not hardening.At low temperatures, the specific surface area of crystal is expanded greatly.
In another preferred scheme, boulton process is adopted to carry out vacuum dehydration to the metatitanic acid after filtration, metatitanic acid after filtering is put into drying oven, and break into pieces as far as possible, keep vacuum tightness at-0.09MP ~-0.06MP, temperature is at 40 DEG C ~ 250 DEG C, and rotating speed per minute turns on dynamic stirring at 5-10, obtains titanium dioxide; Rotating speed is too low, and stir uneven, easily cause caking, rotating speed is too high, has a large amount of dust and extracts out with vacuum, affect product yield; Preferably, maintenance vacuum tightness is-0.09MP, Heating temperature is 60 DEG C, removes after preset value until moisture content, is discharged by drier metatitanic acid after carrying out preliminary fragmentation, send into again in vacuum drying oven and continue drying and dehydrating, now keep vacuum tightness to be-0.03MP, temperature 170 DEG C, until metatitanic acid product weight loss is 5%, 10% or 15%, obtain titanium dioxide.
E. pulverize, sieve: above-mentioned titanium dioxide is cooled to-20 DEG C ~ room temperature, carry out pulverization process with pulverizer, with 200-500 eye mesh screen or air classification or cyclone classifiedly to sieve, obtain product nanometer titanium dioxide, described nanometer titanium dioxide TiO
2content is between 75% ~ 99%, and the specific surface area of powder is 180 ~ 360m
2/ g; Preferably, TiO
2content is 85%, 93% or 99%, and powder specific-surface area detection is 250m
2/ g, 300m
2/ g or 350m
2/ g;
Preferably, by above-mentioned titanium dioxide cool to room temperature, and maintain ambient temperature lower more than 2 hours, crystalline stress can be discharged fully like this, make between xln more loose, especially, before feeding pulverizer, can also carry out water spray process to described titanium dioxide, 1000 kilograms of described titanium dioxides, can spurt the water of 0.1-0.2 kilogram.Owing to having carried out spraying water process to described titanium dioxide, when pulverizing, titanium dioxide has not easily played airborne dust, and avoid the splashing of some bulky crystal when pulverizing, the crystal after pulverizing like this is more even, fine and smooth.
F. pack: in clean, clean environment, nanometer titanium dioxide is packed; TiO is obtained by this preparation method
2content is high, the nanometer titanium dioxide that specific surface area is large, and flue gas denitration catalyst is effective.
Further, described alkali lye refers to sodium hydroxide, potassium hydroxide in stepb, one or more solution in Trimethylamine 99, triethylamine and ammoniacal liquor; Preferably, select ammoniacal liquor as alkali lye, with common alkali lye, complete the adjustment of pH value, cost is low.
Further, sedimentation described in step C comprises one or more modes in gravity settling and centrifugal settling, and described filtration comprises one or more modes in suction filtration and press filtration.
Further, sample detection described in step C and comprise: detect total sulfur content with carbon sulphur instrument, use spectrophotometry phosphate content, detect the content of heavy metal and potassium, sodium, iron, metal ion with AAS or AES or ICP-AES or ICP-MS; Accurately detect with instrument, be convenient to control ion content, thus improve the quality of products.
Further, described in step D, oven dry comprises freeze-drying, vacuum-drying, one or more methods in air stream drying, spraying dry; Use industrial conventional drying method, remove moisture, be convenient to powder process.
Further, pulverizer described in step e is one or more in micronizer mill, Universalpulverizer, Raymond mill, shearing crusher, impact grinder.
Owing to adopting technique scheme, preparation method's technique of the present invention and material simply, prepare gained nanometer titanium dioxide specific surface area large, TiO
2content is high.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. a preparation method for catalyst for denitrating flue gas nanometer titanium dioxide, is characterized in that, comprises the steps:
A. the source of metatitanic acid: the metatitanic acid (also referred to as hydrated titanium dioxide) produced by sulfuric acid process, suspended nitride directly can enter lower step link; Generally remove portion of water wherein by the mode of sedimentation and suction filtration or press filtration, obtain by percentage to the quality: moisture between 45% ~ 95%, dry product TiO
2the filter cake of % > 90%;
B. adjusted to ph: the slurry in A or filter cake are mixed with deionized water by 1:2-5 volume ratio, are uniformly dispersed, adds alkali lye, the pH value of adjustment slurry, the pH value of sampling acidometer or pH detection paper solution; Repeat above-mentionedly to add alkali lye, stirring and detecting step, until obtain the metatitanic acid suspended nitride that pH is 6.5 ~ 9;
C. wash, filter: by the mode of sedimentation, filtration be the moisture removal in the metatitanic acid suspended nitride of 6.5 ~ 9 by above-mentioned pH; Remove the metatitanic acid material of most of moisture or rear deionized water wash of again pulling an oar, or wash online with deionized water, then again removed the moisture in suspended nitride by the mode of gravity settling or centrifugal settling, suction filtration or press filtration, repeatedly wash and dewater; The method surveying filtrate specific conductivity is all adopted indirectly to control ionic concn after each washing, when filtrate specific conductivity is lower than 1000us/cm, use sampling instead to detect and repeated washing control ionic concn, until obtain sulfate ion content < 0.9%, phosphate anion content < 0.4%, the metatitanic acid of the equal < 100ppm of content of the metal ions such as heavy metal and potassium, sodium, iron;
D. dry: above-mentioned washing to be removed the metatitanic acid material after portion of water between bake out temperature-20 DEG C ~ 280 DEG C, between pressure-0.1MPa ~ 1MPa, carry out oven dry 1 ~ 30 hour;
E. pulverize, sieve: above-mentioned titanium dioxide is cooled to-20 DEG C ~ room temperature, pulverization process is carried out with pulverizer, with 200-500 eye mesh screen or air classification or cyclone classifiedly to sieve, obtain product nanometer titanium dioxide, described nanometer titanium dioxide TiO2 content is between 75% ~ 99%, and the specific surface area of powder is 180 ~ 360m
2/ g;
F. pack: in clean, clean environment, nanometer titanium dioxide is packed.
2. the preparation method of catalyst for denitrating flue gas nanometer titanium dioxide as claimed in claim 1, is characterized in that: described alkali lye refers to sodium hydroxide, potassium hydroxide in stepb, one or more solution in Trimethylamine 99, triethylamine and ammoniacal liquor.
3. the preparation method of catalyst for denitrating flue gas nanometer titanium dioxide as claimed in claim 1, is characterized in that: comprise one or more in gravity settling and centrifugal settling in sedimentation described in step C, described filtration comprise in suction filtration and press filtration one or more.
4. the preparation method of catalyst for denitrating flue gas nanometer titanium dioxide as claimed in claim 1, it is characterized in that: sample detection described in step C and comprise: detect total sulfur content with carbon sulphur instrument, under wavelength 700nm, detect phosphate content with spectrophotometry, detect the content of heavy metal and potassium, sodium, iron, metal ion with AAS or AES or ICP-AES or ICP-MS.
5. the preparation method of catalyst for denitrating flue gas nanometer titanium dioxide as claimed in claim 1, is characterized in that: dry described in step D and comprise freeze-drying, vacuum-drying, one or more methods in air stream drying, spraying dry.
6. the preparation method of catalyst for denitrating flue gas nanometer titanium dioxide as claimed in claim 1, is characterized in that: pulverizer described in step e is one or more in micronizer mill, Universalpulverizer, Raymond mill, shearing crusher, impact grinder.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948116A (en) * | 2016-06-30 | 2016-09-21 | 广西金茂钛业有限公司 | Preparation method for titanium dioxide with high specific surface area |
| CN107298460A (en) * | 2017-05-22 | 2017-10-27 | 超彩环保新材料科技有限公司 | Titanium dioxide of low-sulfur superhigh specific surface area and preparation method thereof and purposes |
| CN111573724A (en) * | 2020-04-30 | 2020-08-25 | 广西金茂钛业有限公司 | Method for preparing nano titanium dioxide |
| CN111573723A (en) * | 2020-04-30 | 2020-08-25 | 广西金茂钛业有限公司 | Method for producing titanium dioxide by using neutralization sulfuric acid method |
| CN114733502A (en) * | 2022-04-20 | 2022-07-12 | 河北威达蓝海环保科技股份有限公司 | Regeneration treatment process for titanium dioxide carrier raw material of waste reduction denitration catalyst in wide temperature range |
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| CN107298460B (en) * | 2017-05-22 | 2020-01-07 | 超彩环保新材料科技有限公司 | Low-sulfur titanium dioxide with ultrahigh specific surface area, and preparation method and application thereof |
| CN111573724A (en) * | 2020-04-30 | 2020-08-25 | 广西金茂钛业有限公司 | Method for preparing nano titanium dioxide |
| CN111573723A (en) * | 2020-04-30 | 2020-08-25 | 广西金茂钛业有限公司 | Method for producing titanium dioxide by using neutralization sulfuric acid method |
| CN114733502A (en) * | 2022-04-20 | 2022-07-12 | 河北威达蓝海环保科技股份有限公司 | Regeneration treatment process for titanium dioxide carrier raw material of waste reduction denitration catalyst in wide temperature range |
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