CN105214678A - A kind of without vanadium rare earth based titanium tungsten powder and preparation method thereof - Google Patents
A kind of without vanadium rare earth based titanium tungsten powder and preparation method thereof Download PDFInfo
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- CN105214678A CN105214678A CN201510590915.7A CN201510590915A CN105214678A CN 105214678 A CN105214678 A CN 105214678A CN 201510590915 A CN201510590915 A CN 201510590915A CN 105214678 A CN105214678 A CN 105214678A
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Abstract
The invention provides a kind of without vanadium rare earth based titanium tungsten powder and preparation method thereof, solve the difficult problem that the characteristic of catalyst high-temperature aging resisting, catalyst activity element or activated centre decentralization improve, and the problem that catalyst chemical is poisoning.The present invention is without vanadium rare earth based titanium tungsten powder, composition comprises: titanium dioxide 750-900 part, compound 10-60 part of tungsten, one or more the 30-60 parts in the compound of the compound of cerium, the compound of lanthanum, rhenium, manganese molybdenum nickel composite metal oxide (Mn-Mo-Ni-OX) 10-15 part.Catalyst of the present invention has the feature of high-temperature aging resisting and long service life.Not adding active element vanadium, is real environmentally friendly catalyst.
Description
Technical field
The invention belongs to environmental catalysis, environmentally conscious materials and technical field of air pollution control, relate to a kind of without vanadium rare earth based titanium tungsten powder and preparation method thereof.
Background technology
Along with the growth of energy-consuming, a large amount of fossil fuel is consumed, and causes the discharge capacity of nitrogen oxide constantly to increase, causes very big destruction to environment.Therefore, under excess oxygen, the emission control of NOx has become a study hotspot in current environmental catalysis and technical field of air pollution control.Ammonia SCR (Selectivecatalyticreduction, SCR) is considered to one of most effective method that stationary source NOx eliminates, and its key problem is the development of catalyst.At present, the NH of industrial applications
3-SCR catalyst, mainly V
2o
5-TiO
2or V
2o
5-WO
3(MoO
3)-TiO
2.Such catalyst shows higher NOx clearance and good sulfur resistance at 350 ~ 400 DEG C.But still there are some problems in actual use in this catalyst: mainly active component V
2o
5predecessor toxicity general very large, all there is toxic action to human body and environment.Vanadic anhydride is amphoteric oxide, based on acidity.More than 700 DEG C significantly volatilizations.700-1125 DEG C is decomposed into oxygen and vanadium tetraoxide.For strong oxidizer, be easily reduced into multiple low oxide.Be slightly soluble in water, easily form stable colloidal solution.Very easily be dissolved in alkali, vanadate (VO3 can be generated under weak basic condition
-).Be dissolved in strong acid (rising molten about general pH=2) and do not generate vanadic acid radical ion, and generate the oxygen base vanadium ion (VO3 with valence state
+).For noxious material, in air, maximum magnitude is less than 0.5mg/m
3.
Secondly the high temperature ageing characteristic of catalyst is bad, and active element or activated centre decentralization difficulty improve; Operating temperature window is narrower, and controls strict, is not suitable for existing power-plant flue gas denitration of China etc.; Therefore, need a kind of have within the scope of wider temperature window excellent NOx removal effect and sulfur poisoning resistance without vanadium catalyst.
The patent No. be 200910087773.7 patent document disclose a kind of low-vanadium denitration catalyst, this catalyst has the conversion rate of NOx higher than 90% within the scope of 200 ~ 450 DEG C, but this catalyst contains a small amount of v element, to environment and human body, still there is certain damaging effect.Application number be 200910145015.6 patent document disclose a kind of low temperature Selective catalytic reduction denitrating catalyst, this catalyst adopts nano manganese oxide to be active component, within the scope of wider temperature window, (200 ~ 350 DEG C) its conversion rate of NOx remains on more than 80%, but this patent do not investigate its in sulfur-bearing atmosphere denitration performance.Application number be 200910219534.2 patent document disclose a kind of ceria-based denitration catalyst, this catalyst is with CeO
2-WO
3for active component, within the scope of 250 ~ 450 DEG C, show good denitration activity and sulfur resistance, but the sulfur dioxide concentration that this patent is investigated (being only 100ppm) on the low side, limit the range of application of this catalyst.The patent document of the patent No. 201110344341.7 disclose a kind of for denitrating flue gas without vanadium denitration catalyst and preparation method thereof, this invention is with CeO
2-Fe
2o
3for active component, do not adopt toxic active component V
2o
5, this catalyst carries out denitration test under fixed bed simulated flue gas condition, and result shows when air speed is 30000h
-1, NO volumetric concentration is 1000ppm, SO
2when volumetric concentration is 500ppm, in the temperature range of 250 ~ 500 DEG C, denitration efficiency reaches more than 80%.But the high-temperature aging resisting performance of this catalyst and catalytic conversion all have much room for improvement.
As can be seen here, how while the operating temperature window keeping catalyst wider and higher anti-sulfur poisonous performance, improving the security in catalyst preparing and use procedure, is that can above-mentioned denitration technology the key issue of extensive use.
Summary of the invention
Object of the present invention, overcome the deficiencies in the prior art to provide a kind of without vanadium rare earth based titanium tungsten powder and preparation method thereof, solve the difficult problem that the characteristic of catalyst high-temperature aging resisting, catalyst activity element or activated centre decentralization improve, and the problem that catalyst chemical is poisoning.
The object of the invention is to be achieved through the following technical solutions: a kind of without vanadium rare earth based titanium tungsten powder, it is characterized in that, composition comprises: titanium dioxide 750-900 part, compound 10-60 part of tungsten, one or more 30-60 parts in the compound of the compound of cerium, the compound of lanthanum, rhenium, manganese molybdenum nickel composite metal oxide (Mn-Mo-Ni-O
x) 10-15 part.
Also comprise MEA 5-15 part, citric acid 5-25 part.
The compound of described tungsten be ammonium metatungstate and or ammonium paratungstate; The compound of cerium is one or more in cerous nitrate, cerium oxalate, cerous sulfate or cerium oxide.The compound of lanthanum is one or more in lanthanum nitrate, lanthanum oxalate, lanthanum sulfate or lanthana.The compound of rhenium is one or more in nitric acid rhenium, oxalic acid rhenium, sulfuric acid rhenium or rheium oxide.In described Mn-Mo-Ni-Ox composite metal oxide active component, Mn/Mo/Ni elemental mole ratios is 1:(0.1 ~ 1): (0.1 ~ 1).Titanium dioxide is anatase-type nanometer titanium dioxide.
Preparation method is:
(1) anatase-type nanometer titanium dioxide is added the suspension that enough water is made into 15% concentration;
(2) 10-30 part water and MEA are uniformly mixed dissolving, when temperature arrives 80-100 DEG C, add the compound uniform stirring of tungsten, for subsequent use after all dissolving;
(3) water of 40-60 part and citric acid are uniformly mixed dissolving, add the compound of cerium, until completely dissolved, then add the compound of lanthanum, it is for subsequent use that the compound adding rhenium until completely dissolved again makes mixed liquor;
(4) under agitation, the solution of the suspension of step (1) and step (2) is stirred to mix for 2-3 hour obtain slurry;
(5) slurry that step (4) obtains is put in ultrasonic device, ultrasonic immersing 2-4 hour, then add the solution of step (3) under agitation, continue ultrasonic immersing 2-4 hour; Then manganese molybdenum nickel composite metal oxide (Mn-Mo-Ni-O is added under agitation
x), continue ultrasonic immersing 2-4 hour;
(6) take out drying after ultrasonic end, then 400-700 DEG C of roasting temperature 1-2 hour in net belt type continuous drying kiln, finally grinds to form 80-100 object powder, obtained catalyst.
Catalyst of the present invention is compared with existing typical catalyst, and have better characteristic, it is as shown in the table:
Table 1 catalyst feature of the present invention
The present invention has following beneficial aspects:
(1) catalyst of the present invention has the feature of high-temperature aging resisting and long service life.Tradition SCR catalyst is when temperature reaches 550 DEG C, just there will be the characteristic that active layer specific area starts to reduce, and catalyst of the present invention is under 650 DEG C of conditions, active layer specific area also can remain relatively stable, thus maintains the life-span of catalyst activity and extending catalyst.The tradition SCR catalyst life-span only has 15000 hours, catalyst of the present invention, brings up to more than 25000 hours service life.
(2) not adding active element vanadium, is real environmentally friendly catalyst.The present invention's rare earth replaces the effect of vanadic anhydride, and traditional SCR catalyst pentoxide content is 3% effect, and to environment, and catalyst of the present invention is containing vanadic anhydride, realize catalyst without vanadium Non-toxic, environmental protection.
(3) process route is succinct, with short production cycle, production capacity and high efficiency.The inventive method improves the adsorption of material, maintains the crystalline substance picture of material under a high position and stablizes, improve the high-temperature aging resisting of catalyst.The present invention introduces the auxiliary agent such as manganese, molybdenum, improves the sulfur resistive of catalyst, anti-arsenic poisoning characteristic, inhibits catalyst poisoning, improve the service life of catalyst.
Detailed description of the invention
Embodiment 1, one are without vanadium rare earth based titanium tungsten powder, composition comprises: titanium dioxide 750kg, ammonium metatungstate 10kg, cerous nitrate 15kg, lanthanum nitrate 15kg, nitric acid rhenium 10kg, manganese molybdenum nickel composite metal oxide (Mn-Mo-Ni-OX) 10kg, MEA 5kg, citric acid 5kg.
Wherein, in Mn-Mo-Ni-Ox composite metal oxide active component, Mn/Mo/Ni elemental mole ratios is 1:0.5:0.5.Titanium dioxide is anatase-type nanometer titanium dioxide
Preparation method is:
(1) anatase-type nanometer titanium dioxide is added the suspension that enough water is made into 15% concentration;
(2) 20 premium on currency are joined in dissolving tank, then MEA is joined in dissolving tank, when temperature arrives 90 DEG C, add ammonium metatungstate uniform stirring, for subsequent use after all dissolving;
(3) joined in dissolving tank by 50 premium on currency, then join in dissolving tank by citric acid, stir, then add cerous nitrate, until completely dissolved, then add lanthanum nitrate, adding nitric acid rhenium until completely dissolved again, to make mixed liquor for subsequent use;
(4) under agitation, the solution mix and blend of the suspension of step (1) and step (2) is mixed for 2 hours obtain slurry;
(5) put in ultrasonic device by the slurry that step (4) obtains, ultrasonic immersing 2.5 hours, then adds the solution of step (3) under agitation, continues ultrasonic immersing 2.5 hours; Then manganese molybdenum nickel composite metal oxide (Mn-Mo-Ni-O is added under agitation
x), continue ultrasonic immersing 2.5 hours;
(6) take out drying after ultrasonic end, then 400 ~ 700 DEG C of roasting temperatures 1 hour in net belt type continuous drying kiln, finally grind to form 100 object powder, obtained catalyst.
Embodiment 2, one are without vanadium rare earth based titanium tungsten powder, and composition comprises: titanium dioxide 900kg, ammonium paratungstate 60kg, cerous sulfate 20kg part, lanthanum sulfate 40kg, manganese molybdenum nickel composite metal oxide (Mn-Mo-Ni-O
x) 15kg, MEA 15kg, citric acid 25kg.
Wherein, manganese molybdenum nickel composite metal oxide (Mn-Mo-Ni-O
x) in Mn/Mo/Ni elemental mole ratios be 1:1:1.Titanium dioxide is anatase-type nanometer titanium dioxide.
Preparation method is:
(1) anatase-type nanometer titanium dioxide is added the suspension that enough water is made into 15% concentration;
(2) 30 premium on currency are joined in dissolving tank, then MEA is joined mixed dissolution in dissolving tank, when temperature arrives 100 DEG C, add ammonium paratungstate uniform stirring, for subsequent use after all dissolving;
(3) joined in dissolving tank by the water of 60 liters, then add citric acid and stir, add cerous sulfate, until completely dissolved, then adding lanthanum sulfate, to make mixed liquor for subsequent use;
(4) under agitation, the solution of the suspension of step (1) and step (2) is stirred to mix for 3 hours obtain slurry;
(5) put in ultrasonic device by the slurry that step (4) obtains, ultrasonic immersing 4 hours, then adds the solution of step (3) under agitation, continues ultrasonic immersing 4 hours; Then manganese molybdenum nickel composite metal oxide (Mn-Mo-Ni-O is added under agitation
x), continue ultrasonic immersing 4 hours;
(6) take out drying after ultrasonic end, then 400 ~ 700 DEG C of roasting temperatures 2 hours in net belt type continuous drying kiln, finally grind to form 100 object powder, obtained catalyst.
Embodiment 3, one are without vanadium rare earth based titanium tungsten powder, and composition comprises: titanium dioxide 800kg, ammonium metatungstate 50kg, nitric acid rhenium 50kg, manganese molybdenum nickel composite metal oxide (Mn-Mo-Ni-O
x) 12kg, MEA 10kg, citric acid 20kg.
Wherein, manganese molybdenum nickel composite metal oxide (Mn-Mo-Ni-O
x) in Mn/Mo/Ni elemental mole ratios be 1:0.8:0.8.Titanium dioxide is anatase-type nanometer titanium dioxide.
Preparation method is:
(1) anatase-type nanometer titanium dioxide is added the suspension that enough water is made into 15% concentration;
(2) 20 premium on currency are joined in dissolving tank, then MEA is joined mixed dissolution in dissolving tank, when temperature arrives 88 DEG C, add ammonium metatungstate uniform stirring, for subsequent use after all dissolving;
(3) water of 50 liters is joined in dissolving tank, then add citric acid stirring, add nitric acid rhenium, make mixed liquor until completely dissolved for subsequent use;
(4) under agitation, the solution of the suspension of step (1) and step (2) is stirred to mix for 3 hours obtain slurry;
(5) put in ultrasonic device by the slurry that step (4) obtains, ultrasonic immersing 3 hours, then adds the solution of step (3) under agitation, continues ultrasonic immersing 3 hours; Then manganese molybdenum nickel composite metal oxide (Mn-Mo-Ni-O is added under agitation
x), continue ultrasonic immersing 3 hours;
(6) take out drying after ultrasonic end, then 400 ~ 700 DEG C of roasting temperatures 1.5 hours in net belt type continuous drying kiln, finally grind to form 100 object powder, obtained catalyst.
Embodiment 4, one are without vanadium rare earth based titanium tungsten powder, and composition comprises: titanium dioxide 850kg part, ammonium paratungstate 40kg, cerium oxide 15kg, nitric acid rhenium 40kg, manganese molybdenum nickel composite metal oxide (Mn-Mo-Ni-O
x) 14kg, MEA 11kg, citric acid 22kg
Wherein, manganese molybdenum nickel composite metal oxide (Mn-Mo-Ni-O
x) in active component, Mn/Mo/Ni elemental mole ratios is 1:0.7:1.Titanium dioxide is anatase-type nanometer titanium dioxide.
Preparation method is:
(1) anatase-type nanometer titanium dioxide is added the suspension that enough water is made into 15% concentration;
(2) 30 premium on currency are joined in dissolving tank, then MEA is joined mixed dissolution in dissolving tank, when temperature arrives 80-100 DEG C, add ammonium paratungstate uniform stirring, for subsequent use after all dissolving;
(3) joined in dissolving tank by the water of 45 liters, then join in dissolving tank by citric acid, stir, add cerium oxide, until completely dissolved, then adding nitric acid rhenium, to make mixed liquor for subsequent use;
(4) under agitation, the solution of the suspension of step (1) and step (2) is stirred to mix for 3 hours obtain slurry;
(5) put in ultrasonic device by the slurry that step (4) obtains, ultrasonic immersing 4 hours, then adds the solution of step (3) under agitation, continues ultrasonic immersing 4 hours; Then manganese molybdenum nickel composite metal oxide (Mn-Mo-Ni-O is added under agitation
x), continue ultrasonic immersing 4 hours;
(6) take out drying after ultrasonic end, then 400 ~ 700 DEG C of roasting temperatures 2 hours in net belt type continuous drying kiln, finally grind to form 100 object powder, obtained catalyst.
Claims (3)
1. one kind without vanadium rare earth based titanium tungsten powder, it is characterized in that, composition comprises: titanium dioxide 750-900 part, compound 10-60 part of tungsten, one or more 30-60 parts in the compound of the compound of cerium, the compound of lanthanum, rhenium, manganese molybdenum nickel composite metal oxide 10-15 part;
The compound of described tungsten be ammonium metatungstate and or ammonium paratungstate; The compound of cerium is one or more in cerous nitrate, cerium oxalate, cerous sulfate or cerium oxide; The compound of lanthanum is one or more in lanthanum nitrate, lanthanum oxalate, lanthanum sulfate or lanthana; The compound of rhenium is one or more in nitric acid rhenium, oxalic acid rhenium, sulfuric acid rhenium or rheium oxide; In described Mn-Mo-Ni-Ox composite metal oxide active component, Mn/Mo/Ni elemental mole ratios is 1:(0.1 ~ 1): (0.1 ~ 1).
2. as claimed in claim 1 without vanadium rare earth based titanium tungsten powder, it is characterized in that, also comprise MEA 5-15 part, citric acid 5-25 part.
3. described in claim 1 or 2 without vanadium rare earth based titanium tungsten powder, it is characterized in that, preparation method is:
(1) anatase-type nanometer titanium dioxide is added the suspension that enough water is made into 15% concentration;
(2) 10-30 part water and MEA are uniformly mixed dissolving, when temperature arrives 80-100 DEG C, add the compound uniform stirring of tungsten, for subsequent use after all dissolving;
(3) water of 40-60 part and citric acid are uniformly mixed dissolving, add the compound of cerium, until completely dissolved, then add the compound of lanthanum, it is for subsequent use that the compound adding rhenium until completely dissolved again makes mixed liquor;
(4) under agitation, the solution of the suspension of step (1) and step (2) is stirred to mix for 2-3 hour obtain slurry;
(5) slurry that step (4) obtains is put in ultrasonic device, ultrasonic immersing 2-4 hour, then add the solution of step (3) under agitation, continue ultrasonic immersing 2-4 hour; Then add manganese molybdenum nickel composite metal oxide under agitation, continue ultrasonic immersing 2-4 hour;
(6) take out drying after ultrasonic end, then 400-700 DEG C of roasting temperature 1-2 hour in net belt type continuous drying kiln, finally grinds to form 80-100 object powder, obtained catalyst.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115521644A (en) * | 2022-10-14 | 2022-12-27 | 潮州市索力德机电设备有限公司 | Degradable oxynitride coating and preparation method and application thereof |
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| US20100303697A1 (en) * | 2008-05-16 | 2010-12-02 | Anatoly Sobolevskiy | Selective Catalytic Reduction System and Process for Treating NOx Emissions Using a Zinc or Titanium Promoted Palladium-Zirconium Catalyst |
| CN102950008A (en) * | 2011-08-29 | 2013-03-06 | 中国石油化工股份有限公司 | Composite smoke SCR (selective catalytic reduction) denitrification catalyst and preparation method thereof |
| CN103586017A (en) * | 2013-11-22 | 2014-02-19 | 西南化工研究设计院有限公司 | Preparation method of titanium and tungsten powder for flue gas denitration catalyst and product prepared through preparation method |
| CN104415747A (en) * | 2013-08-22 | 2015-03-18 | 上海郎特汽车净化器有限公司 | Titanium tungsten powder and preparation method thereof |
-
2015
- 2015-09-16 CN CN201510590915.7A patent/CN105214678A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20100303697A1 (en) * | 2008-05-16 | 2010-12-02 | Anatoly Sobolevskiy | Selective Catalytic Reduction System and Process for Treating NOx Emissions Using a Zinc or Titanium Promoted Palladium-Zirconium Catalyst |
| CN102950008A (en) * | 2011-08-29 | 2013-03-06 | 中国石油化工股份有限公司 | Composite smoke SCR (selective catalytic reduction) denitrification catalyst and preparation method thereof |
| CN104415747A (en) * | 2013-08-22 | 2015-03-18 | 上海郎特汽车净化器有限公司 | Titanium tungsten powder and preparation method thereof |
| CN103586017A (en) * | 2013-11-22 | 2014-02-19 | 西南化工研究设计院有限公司 | Preparation method of titanium and tungsten powder for flue gas denitration catalyst and product prepared through preparation method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115521644A (en) * | 2022-10-14 | 2022-12-27 | 潮州市索力德机电设备有限公司 | Degradable oxynitride coating and preparation method and application thereof |
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