CN103028392A - Preparation method of titanium dioxide for denitration through use of titanium tetrachloride - Google Patents
Preparation method of titanium dioxide for denitration through use of titanium tetrachloride Download PDFInfo
- Publication number
- CN103028392A CN103028392A CN2011103030842A CN201110303084A CN103028392A CN 103028392 A CN103028392 A CN 103028392A CN 2011103030842 A CN2011103030842 A CN 2011103030842A CN 201110303084 A CN201110303084 A CN 201110303084A CN 103028392 A CN103028392 A CN 103028392A
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- CN
- China
- Prior art keywords
- titanium dioxide
- denitration
- titanium
- titanium tetrachloride
- obtains
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 35
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title abstract description 7
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 16
- 150000001875 compounds Chemical class 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 7
- 239000010937 tungsten Substances 0.000 claims abstract description 7
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 7
- 239000013067 intermediate product Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 54
- 239000007788 liquid Substances 0.000 claims description 28
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical group [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 235000006408 oxalic acid Nutrition 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 17
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 16
- 238000005303 weighing Methods 0.000 claims description 16
- 230000001105 regulatory effect Effects 0.000 claims description 8
- 238000004062 sedimentation Methods 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000013049 sediment Substances 0.000 abstract 2
- 238000005660 chlorination reaction Methods 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 238000013019 agitation Methods 0.000 description 2
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of titanium dioxide for denitration through the use of a titanium tetrachloride. The preparation method of the titanium dioxide for denitration through the use of the titanium tetrachloride comprises the steps of taking an intermediate product, namely a titanium tetrachloride solution generated during the production of titanium dioxide through a chlorination process as a raw material; adding a compound of vanadium and a compound of tungsten into the titanium tetrachloride solution; stirring; neutralizing by using an alkaline matter; filtering to obtain sediments; and washing, drying and calcining the sediments to obtain the titanium dioxide for denitration. In comparison with the prior art, the preparation method of the titanium dioxide for denitration through the use of the titanium tetrachloride has few technological steps; and in addition, the production period is shortened and the production cost is lowered.
Description
Technical field
The present invention relates to a kind of preparation method of denitration usefulness titanium dioxide, particularly a kind of method for preparing denitration usefulness titanium dioxide with titanium tetrachloride.
Background technology
Nitrogen oxide is one of Air Pollutants, and it damages the ozone layer, forms acid rain and photochemical fog, influence ecological environment, and harm humans is healthy.Denitration titanium dioxide is doping tungstic acid and vanadic anhydride in titanium dioxide, forms take titanium dioxide as carrier, the denitrating catalyst take tungstic acid and vanadic anhydride as active component.At present, denitration is two step infusion processes with the preparation method of titanium dioxide, after soon titania powder will add thermal agitation in ammonium tungstate solution, drying and calcining, cooled calcined material is pulverized, and pulverizing adds thermal agitation afterwards in ammonium metavanadate solution after, drying and calcining namely obtains denitration titanium dioxide.This method step is many, complex process, and the production cycle is long, and cost is high.
Summary of the invention
For the problems of the prior art, the invention provides a kind of denitration with the preparation method of titanium dioxide, the intermediate product titanium tetrachloride that the method is produced titanium dioxide take chloridising has greatly reduced processing step as raw material, has shortened the production cycle, has reduced production cost.
In order to achieve the above object, technical scheme of the present invention is: a kind of method for preparing denitration usefulness titanium dioxide with titanium tetrachloride, in the intermediate product titanium tetrachloride liquid of chloridising production titanium dioxide, add the compound of vanadium and the compound of tungsten, neutralize with alkaline matter after stirring, the precipitation that obtains after the filtration namely obtains denitration titanium dioxide after washing, oven dry, calcining.
Further, the compound of described vanadium is ammonium metavanadate.
Further, the compound of described tungsten is ammonium tungstate.
Add oxalic acid when further, adding the compound of the compound of vanadium and tungsten in the titanium liquid.
Further, described alkaline matter is NaOH or ammoniacal liquor.
Further, the method may further comprise the steps successively:
1) according to mass ratio WO
3/ TiO
2=1:8 ~ 1:10, V
2O
5/ TiO
2=1:100 ~ 1:200 takes by weighing ammonium tungstate and ammonium metavanadate, takes by weighing the oxalic acid that equates with ammonium tungstate and ammonium metavanadate gross mass, with ammonium tungstate, ammonium metavanadate, the water-soluble wiring solution-forming of oxalic acid;
2) solution with step 1) joins in the titanium tetrachloride liquid, mixes and obtains material liquid;
3) with sodium hydroxide solution or ammoniacal liquor regulating step 2) the material liquid pH to 5 that obtains ~ 6, behind the sedimentation and filtration that obtains, washing;
4) step 3) is obtained be deposited in 80 ~ 130 ℃ lower dry;
5) dried be deposited in 450 ~ 600 ℃ of lower calcinings after, pulverize and namely obtain denitration titanium dioxide.
Compared with prior art, processing step of the present invention is few, has shortened the production cycle, has reduced production cost.
The specific embodiment
Below in conjunction with embodiment the present invention is further specified.
Embodiment 1
1) according to mass ratio WO
3/ TiO
2=1:10, V
2O
5/ TiO
2=1:200 takes by weighing ammonium tungstate and ammonium metavanadate, takes by weighing the oxalic acid that equates with ammonium tungstate and ammonium metavanadate gross mass, with ammonium tungstate, ammonium metavanadate, the water-soluble wiring solution-forming of oxalic acid;
2) solution with step 1) joins in the titanium tetrachloride liquid, mixes and obtains material liquid;
3) with sodium hydroxide solution regulating step 2) the material liquid pH to 6 that obtains, behind the sedimentation and filtration that obtains, washing;
4) step 3) is obtained be deposited in 130 ℃ lower dry;
5) dried be deposited in 600 ℃ of lower calcinings after, pulverize and namely obtain denitration titanium dioxide.
Embodiment 2
1) according to mass ratio WO
3/ TiO
2=1:8, V
2O
5/ TiO
2=1:100 takes by weighing ammonium tungstate and ammonium metavanadate, takes by weighing the oxalic acid that equates with ammonium tungstate and ammonium metavanadate gross mass, with ammonium tungstate, ammonium metavanadate, the water-soluble wiring solution-forming of oxalic acid;
2) solution with step 1) joins in the titanium tetrachloride liquid, mixes and obtains material liquid;
3) with sodium hydroxide solution regulating step 2) the material liquid pH to 5 that obtains, behind the sedimentation and filtration that obtains, washing;
4) step 3) is obtained be deposited in 80 ℃ lower dry;
5) dried be deposited in 450 ℃ of lower calcinings after, pulverize and namely obtain denitration titanium dioxide.
Embodiment 3
1) according to mass ratio WO
3/ TiO
2=1:10, V
2O
5/ TiO
2=1:100 takes by weighing ammonium tungstate and ammonium metavanadate, takes by weighing the oxalic acid that equates with ammonium tungstate and ammonium metavanadate gross mass, with ammonium tungstate, ammonium metavanadate, the water-soluble wiring solution-forming of oxalic acid;
2) solution with step 1) joins in the titanium tetrachloride liquid, mixes and obtains material liquid;
3) with sodium hydroxide solution regulating step 2) the material liquid pH to 5 that obtains, behind the sedimentation and filtration that obtains, washing;
4) step 3) is obtained be deposited in 130 ℃ lower dry;
5) dried be deposited in 450 ℃ of lower calcinings after, pulverize and namely obtain denitration titanium dioxide.
Embodiment 4
1) according to mass ratio WO
3/ TiO
2=1:8, V
2O
5/ TiO
2=1:200 takes by weighing ammonium tungstate and ammonium metavanadate, takes by weighing the oxalic acid that equates with ammonium tungstate and ammonium metavanadate gross mass, with ammonium tungstate, ammonium metavanadate, the water-soluble wiring solution-forming of oxalic acid;
2) solution with step 1) joins in the titanium tetrachloride liquid, mixes and obtains material liquid;
3) with ammoniacal liquor regulating step 2) the material liquid pH to 6 that obtains, behind the sedimentation and filtration that obtains, washing;
4) step 3) is obtained be deposited in 130 ℃ lower dry;
5) dried be deposited in 600 ℃ of lower calcinings after, pulverize and namely obtain denitration titanium dioxide.
Embodiment 5
1) according to mass ratio WO
3/ TiO
2=1:9, V
2O
5/ TiO
2=1:150 takes by weighing ammonium tungstate and ammonium metavanadate, takes by weighing the oxalic acid that equates with ammonium tungstate and ammonium metavanadate gross mass, with ammonium tungstate, ammonium metavanadate, the water-soluble wiring solution-forming of oxalic acid;
2) solution with step 1) joins in the titanium tetrachloride liquid, mixes and obtains material liquid;
3) with ammoniacal liquor regulating step 2) the material liquid pH to 5.5 that obtains, behind the sedimentation and filtration that obtains, washing;
4) step 3) is obtained be deposited in 110 ℃ lower dry;
5) dried be deposited in 550 ℃ of lower calcinings after, pulverize and namely obtain denitration titanium dioxide.
Embodiment 6
1) according to mass ratio WO
3/ TiO
2=1:9, V
2O
5/ TiO
2=1:200 takes by weighing ammonium tungstate and ammonium metavanadate, takes by weighing the oxalic acid that equates with ammonium tungstate and ammonium metavanadate gross mass, with ammonium tungstate, ammonium metavanadate, the water-soluble wiring solution-forming of oxalic acid;
2) solution with step 1) joins in the titanium tetrachloride liquid, mixes and obtains material liquid;
3) with ammoniacal liquor regulating step 2) the material liquid pH to 5.5 that obtains, behind the sedimentation and filtration that obtains, washing;
4) step 3) is obtained be deposited in 130 ℃ lower dry;
5) dried be deposited in 600 ℃ of lower calcinings after, pulverize and namely obtain denitration titanium dioxide.
All in the situation that do not break away from the simple distortion that core of the present invention makes or revise and all fall into protection scope of the present invention.
Claims (6)
1. one kind prepares denitration with the method for titanium dioxide with titanium tetrachloride, it is characterized in that, in the intermediate product titanium tetrachloride liquid of chloridising production titanium dioxide, add the compound of vanadium and the compound of tungsten, neutralize with alkaline matter after stirring, the precipitation that obtains after the filtration namely obtains denitration titanium dioxide after washing, oven dry, calcining.
2. a kind of method for preparing denitration usefulness titanium dioxide with titanium tetrachloride according to claim 1 is characterized in that, the compound of described vanadium is ammonium metavanadate.
3. a kind of method for preparing denitration usefulness titanium dioxide with titanium tetrachloride according to claim 1 is characterized in that, the compound of described tungsten is ammonium tungstate.
4. according to claim 1ly a kind ofly prepare denitration with the method for titanium dioxide with titanium tetrachloride, it is characterized in that, add oxalic acid when adding the compound of the compound of vanadium and tungsten in the titanium liquid.
5. a kind of method for preparing denitration usefulness titanium dioxide with titanium tetrachloride according to claim 1 is characterized in that, described alkaline matter is NaOH or ammoniacal liquor.
6. according to claim 1 to 5 each described a kind of methods that prepare denitration usefulness titanium dioxide with titanium tetrachloride, it is characterized in that, the method may further comprise the steps successively:
1) according to mass ratio WO
3/ TiO
2=1:8 ~ 1:10, V
2O
5/ TiO
2=1:100 ~ 1:200 takes by weighing ammonium tungstate and ammonium metavanadate, takes by weighing the oxalic acid that equates with ammonium tungstate and ammonium metavanadate gross mass, with ammonium tungstate, ammonium metavanadate, the water-soluble wiring solution-forming of oxalic acid;
2) solution with step 1) joins in the titanium tetrachloride liquid, mixes and obtains material liquid;
3) with sodium hydroxide solution or ammoniacal liquor regulating step 2) the material liquid pH to 5 that obtains ~ 6, behind the sedimentation and filtration that obtains, washing;
4) step 3) is obtained be deposited in 80 ~ 130 ℃ lower dry;
5) dried be deposited in 450 ~ 600 ℃ of lower calcinings after, pulverize and namely obtain denitration titanium dioxide.
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|---|---|---|---|
| CN2011103030842A CN103028392A (en) | 2011-10-10 | 2011-10-10 | Preparation method of titanium dioxide for denitration through use of titanium tetrachloride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109012566A (en) * | 2018-09-18 | 2018-12-18 | 渤海大学 | The preparation method of secondary chlorine white clay foundation stone oil Organic Pollutants in Wastewater removal material |
Citations (3)
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| CN101396656A (en) * | 2008-10-23 | 2009-04-01 | 清华大学 | Power plant flue-gas SCR denitration catalyst capable of preventing sulfur trioxide poisoning and preparation method thereof |
| CN101513620A (en) * | 2009-04-07 | 2009-08-26 | 南京大学 | Preparation method for titanium dioxide group catalyst carrier |
| CN101695656A (en) * | 2009-10-21 | 2010-04-21 | 东南大学 | Method for preparing powdery selective catalytic reduction denitration catalyst by using sol impregnation method |
-
2011
- 2011-10-10 CN CN2011103030842A patent/CN103028392A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101396656A (en) * | 2008-10-23 | 2009-04-01 | 清华大学 | Power plant flue-gas SCR denitration catalyst capable of preventing sulfur trioxide poisoning and preparation method thereof |
| CN101513620A (en) * | 2009-04-07 | 2009-08-26 | 南京大学 | Preparation method for titanium dioxide group catalyst carrier |
| CN101695656A (en) * | 2009-10-21 | 2010-04-21 | 东南大学 | Method for preparing powdery selective catalytic reduction denitration catalyst by using sol impregnation method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109012566A (en) * | 2018-09-18 | 2018-12-18 | 渤海大学 | The preparation method of secondary chlorine white clay foundation stone oil Organic Pollutants in Wastewater removal material |
| CN109012566B (en) * | 2018-09-18 | 2021-08-06 | 渤海大学 | Preparation method of material for removing organic pollutants in hypochlorous white mud-based petroleum wastewater |
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Application publication date: 20130410 |