CN106732526A - The method of the denitrating catalyst regeneration duties vanadic anhydride based on curve matching - Google Patents
The method of the denitrating catalyst regeneration duties vanadic anhydride based on curve matching Download PDFInfo
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- CN106732526A CN106732526A CN201611181435.6A CN201611181435A CN106732526A CN 106732526 A CN106732526 A CN 106732526A CN 201611181435 A CN201611181435 A CN 201611181435A CN 106732526 A CN106732526 A CN 106732526A
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- catalyst
- ammonium metavanadate
- vanadic anhydride
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- metavanadate solution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
Abstract
The present invention relates to a kind of method of the denitrating catalyst regeneration duties vanadic anhydride based on curve matching, comprise the following steps:(1)Determine fit line;(2)During continuous dipping, ammonium metavanadate solution is added.Step(2)Comprise the following steps:(2‑1)Obtain the net load quality of vanadic anhydride in catalyst;(2‑2)Ammonium metavanadate solution is taken, is calculated after a catalyst dipping is completed, the ammonium metavanadate solution volume for needing to add when catalyst impregnates is carried out again;(2‑3)Addition ammonium metavanadate solution, and deionized water is added to meet ammonium metavanadate solution and catalyst geometric volume ratio.The present invention can effectively control vanadic anhydride net load amount in the catalyst of diverse location using above-mentioned dipping method, and the Mathematical Fitting obtained using the method for above-mentioned fit line can be effectively adapted to the actual production of above-mentioned dipping method.
Description
Technical field
The present invention relates to a kind of method for loading vanadic anhydride, it is specifically related to a kind of denitration based on curve matching and urges
The method of agent regeneration duties vanadic anhydride.
Background technology
Vanadium is a kind of non-ferrous metal, and vanadic anhydride is widely used in the industries such as metallurgy, chemical industry, is mainly used in smelting ferrovanadium.
As alloy addition, more than the 80% of vanadic anhydride total flow is accounted for, next to that the catalyst as organic chemical industry, that is, touch
Matchmaker, accounts for the 10% of total amount, elsewhere accounts for the 10% of total amount as inorganic chemical, chemical reagent, enamel and magnetic material etc..But
It is that may be caused to be lost in as the vanadic anhydride of catalyst active component according to different regeneration technologies, it is therefore desirable to pass through
Load vanadic anhydride causes that the activity of catalyst is recovered again.
The content of the invention
For the above-mentioned technical problem of prior art, the invention provides a kind of denitrating catalyst based on curve matching again
The method of raw load vanadic anhydride, vanadic anhydride net load amount is uniformly distributed in can meeting single catalyst.While root
The net load amount of vanadic anhydride in catalyst can be effectively controlled according to Mathematical Fitting formula.
To reach above-mentioned purpose, the present invention is achieved by the following technical solutions:
A kind of method of the denitrating catalyst regeneration duties vanadic anhydride based on curve matching, comprises the following steps:
(1)Determine fit line;
(2)During continuous dipping, ammonium metavanadate solution is added.
As preferred, the step(1)Comprise the following steps:
(1-1)Tested by XRF and obtain pentoxide content K% in catalyst sample;
(1-2)Sizeable acid-resistant container is chosen, the volume ratio for designing ammonium metavanadate solution and catalyst geometric volume is V1;
(1-3)Catalyst sample quality is weighed for M g;
(1-4)Catalyst is put into container, and needs are calculated with above-mentioned volume ratio V1 according to catalyst geometric volume
Addition ammonium metavanadate concentration is the volume of X g/L, then ultrasonically treated 2 hours under normal temperature condition;
(1-5)Catalyst after dipping is calcined 5 hours for 650 DEG C in Muffle furnace;
(1-6)Catalyst after calcining is detected into pentoxide content H% by XRF again;
(1-7)Fitting formula is set up under the conditions of volume ratio is V1:Y%=A+B×X %;Y=H-K
Wherein A is constant, and B is coefficient, and X is ammonium metavanadate solution concentration, and Y% is that vanadic anhydride is born only in impregnating rear catalyst
Carry content.
(1-8)Under the conditions of same volume is than V1, using in the ammonium metavanadate solution and dipping rear catalyst of various concentrations
Vanadic anhydride net load content carries out curve fitting, and obtains fitting formula.
The step(2)Comprise the following steps:
(2-1)The net load quality N g of vanadic anhydride in catalyst are obtained, then N=Y% × M;
(2-2)The solution that ammonium metavanadate concentration is C g/L is taken, is calculated by T=1.3 × N/C and is completed a catalyst dipping
Afterwards, the ammonium metavanadate solution volume T for needing to add when catalyst impregnates is carried out again;
(2-3)Addition volume is the ammonium metavanadate solution of C g/L for the concentration of T, and adds deionized water to meet metavanadic acid
Ammonium salt solution is V1 with catalyst geometric volume ratio.
Beneficial effects of the present invention are as follows:
The method of denitrating catalyst regeneration duties vanadic anhydride of the present invention based on curve matching, can using above-mentioned dipping method
With vanadic anhydride net load amount, the number obtained using the method for above-mentioned fit line in the catalyst for effectively controlling diverse location
Learning fitting can be effectively adapted to the actual production of above-mentioned dipping method.
Brief description of the drawings
Fig. 1 is basic flow sheet of the invention;
Fig. 2 is fitted figure of the invention;
Fig. 3 is catalyst schematic diagram of the invention.
Specific embodiment
With reference to specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to
This.
As shown in figure 1, the method for denitrating catalyst regeneration duties vanadic anhydride of the present invention based on curve matching, including
Following steps:
(1)Determine fit line:
(1-1)Tested by XRF and obtain pentoxide content K% in catalyst sample;
(1-2)Sizeable acid-resistant container is chosen, the volume ratio for designing ammonium metavanadate solution and catalyst geometric volume is V1;
(1-3)Catalyst sample quality is weighed for M g;
(1-4)Catalyst is put into container, and needs are calculated with above-mentioned volume ratio V1 according to catalyst geometric volume
Addition ammonium metavanadate concentration is the volume of X g/L, then ultrasonically treated 2 hours under normal temperature condition;
(1-5)Catalyst after dipping is calcined 5 hours for 650 DEG C in Muffle furnace;
(1-6)Catalyst after calcining is detected into pentoxide content H% by XRF again;
(1-7)Fitting formula is set up under the conditions of volume ratio is V1:Y%=A+B×X %;Y=H-K
Wherein A is constant, and B is coefficient, and X is ammonium metavanadate solution concentration, and Y% is that vanadic anhydride is born only in impregnating rear catalyst
Carry content.
(1-8)Under the conditions of same volume is than V1, using in the ammonium metavanadate solution and dipping rear catalyst of various concentrations
Vanadic anhydride net load content carries out curve fitting, and obtains fitting formula, as shown in Figure 2.
(2)During continuous dipping, ammonium metavanadate solution is added:
(2-1)The net load quality N g of vanadic anhydride in catalyst are obtained, then N=Y% × M;
(2-2)The solution that ammonium metavanadate concentration is C g/L is taken, can be calculated by T=1.3 × N/C and be completed a catalyst dipping
Afterwards, the ammonium metavanadate solution volume T for needing to add when catalyst impregnates is carried out again;
(2-3)Addition volume is the ammonium metavanadate solution of C g/L for the concentration of T, and adds deionized water to meet metavanadic acid
Ammonium salt solution is V1 with catalyst geometric volume ratio.
Embodiment 1
Single catalyst carries out dipping pilot experiment checking
Volume ratio:Volume and catalyst geometric volume according to addition ammonium metavanadate solution determine volume ratio.
Fit line:Under the volume ratio, as needed for the mathematical formulae calculating catalyst of fitting reaches default net load amount
Ammonium metavanadate solution concentration, and the volume of ammonium metavanadate solution is calculated according to the geometric volume of catalyst.
Pretreatment:Catalyst is carried out into deashing through hole, and wash, each 30 minutes of pickling.
Dipping:The ammonium metavanadate solution of known volume and concentration is added, and is impregnated 30 minutes under conditions of bubbling.
Dry:After catalyst is taken out using air blower drying 1 hour, end, middle-end and lower end are sampled on a catalyst,
And calcining 5 hours at 650 DEG C are put into Muffle furnace.
Fluid infusion:Added ammonium metavanadate solution and be put into unregenerated catalyst by ammonium metavanadate solution replenishment method and continuously soaked
Stain.
Result such as table 1 below:
Table 1
Using above-mentioned dipping method, vanadic anhydride net load amount is uniformly distributed in can meeting single catalyst.While basis
Mathematical Fitting formula can effectively control the net load amount of vanadic anhydride in catalyst.
Table 2
By adding ammonium metavanadate solution, can be with the single catalyst of the dipping of continuous-stable.
Embodiment 2
FCL catalyst carries out dipping trial production experimental verification
Volume ratio:Volume and catalyst geometric volume according to ammonium metavanadate solution determine volume ratio.
Fit line:Under the volume ratio, as needed for the mathematical formulae calculating catalyst of fitting reaches default net load amount
Ammonium metavanadate solution concentration, and the volume of ammonium metavanadate solution is calculated according to the geometric volume of catalyst.
Pretreatment:Catalyst is carried out into deashing through hole;Wash again, each 30 minutes of pickling, carry out dipping preparation.
Dipping:The ammonium metavanadate solution of known volume and concentration is added, and is impregnated 30 minutes under conditions of bubbling.
Dry:After catalyst is taken out using air blower drying 1 hour, the catalyst sample that numbering is 2,4,6,7,8,10 is taken
Product, and calcining 5 hours at 650 DEG C are put into Muffle furnace.
Fluid infusion:Added ammonium metavanadate solution and be put into unregenerated catalyst by ammonium metavanadate solution replenishment method and continuously soaked
Stain.Catalyst schematic diagram is as shown in Figure 3.
The catalyst detection for taking Fig. 3 obtains data such as table 3 below:
Table 3
Vanadic anhydride net load amount in the catalyst of diverse location can be effectively controlled using above-mentioned dipping method, using upper
Stating the Mathematical Fitting that the method for fit line obtains can be effectively adapted to the actual production of above-mentioned dipping method.
Form 4
The continuous dipping FCL catalyst that can be effectively stablized using dipping liquid replenishing method, is produced a desired effect.
Above-described embodiment is only used for illustrating inventive concept of the invention, rather than the restriction to rights protection of the present invention,
All changes for carrying out unsubstantiality to the present invention using this design, all should fall into protection scope of the present invention.
Claims (3)
1. a kind of method of the denitrating catalyst regeneration duties vanadic anhydride based on curve matching, it is characterised in that including following
Step:
(1)Determine fit line;
(2)During continuous dipping, ammonium metavanadate solution is added.
2. the method for the denitrating catalyst regeneration duties vanadic anhydride of curve matching, its feature are based on as claimed in claim 1
It is the step(1)Comprise the following steps:
(1-1)Tested by XRF and obtain pentoxide content K% in catalyst sample;
(1-2)Sizeable acid-resistant container is chosen, the volume ratio for designing ammonium metavanadate solution and catalyst geometric volume is V1;
(1-3)Catalyst sample quality is weighed for M g;
(1-4)Catalyst is put into container, and needs are calculated with above-mentioned volume ratio V1 according to catalyst geometric volume
Addition ammonium metavanadate concentration is the volume of X g/L, then ultrasonically treated 2 hours under normal temperature condition;
Catalyst after dipping is calcined 5 hours for 650 DEG C in Muffle furnace;
Catalyst after calcining is detected into pentoxide content H% by XRF again;
(1-7)Fitting formula is set up under the conditions of volume ratio is V1:Y%=A+B×X %;Y=H-K
Wherein A is constant, and B is coefficient, and X is ammonium metavanadate solution concentration, and Y% is that vanadic anhydride is born only in impregnating rear catalyst
Carry content;
(1-8)Under the conditions of same volume is than V1, using ammonium metavanadate solution and five oxygen in dipping rear catalyst of various concentrations
Change two vanadium net load contents to carry out curve fitting, obtain fitting formula.
3. the method for the denitrating catalyst regeneration duties vanadic anhydride of curve matching, its feature are based on as claimed in claim 1
It is the step(2)Comprise the following steps:
(2-1)The net load quality N g of vanadic anhydride in catalyst are obtained, then N=Y% × M;
(2-2)The solution that ammonium metavanadate concentration is C g/L is taken, is calculated by T=1.3 × N/C and is completed a catalyst dipping
Afterwards, the ammonium metavanadate solution volume T for needing to add when catalyst impregnates is carried out again;
(2-3)Addition volume is the ammonium metavanadate solution of C g/L for the concentration of T, and adds deionized water to meet metavanadic acid
Ammonium salt solution is V1 with catalyst geometric volume ratio.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109507365A (en) * | 2019-01-08 | 2019-03-22 | 苏州西热节能环保技术有限公司 | A method of measurement SCR catalyst regeneration content of vanadium in load liquid |
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CN101259417A (en) * | 2008-04-15 | 2008-09-10 | 中国科学院山西煤炭化学研究所 | Regeneration method of sulphur absorption V2O5/AC catalytic adsorption agent |
CN103920503A (en) * | 2013-12-03 | 2014-07-16 | 华南理工大学 | Modified regenerated SCR (selective catalytic reduction) denitration catalyst and its preparation method |
CN105536884A (en) * | 2016-01-18 | 2016-05-04 | 北京国电龙源环保工程有限公司 | Method for regenerating waste denitration catalyst by selectively implanting active ingredients |
CN105561781A (en) * | 2015-12-14 | 2016-05-11 | 重庆大学 | Method for removing NOx in sintering flue gas through low-temperature SCR (Selective Catalytic Reduction) catalyst |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101259417A (en) * | 2008-04-15 | 2008-09-10 | 中国科学院山西煤炭化学研究所 | Regeneration method of sulphur absorption V2O5/AC catalytic adsorption agent |
CN103920503A (en) * | 2013-12-03 | 2014-07-16 | 华南理工大学 | Modified regenerated SCR (selective catalytic reduction) denitration catalyst and its preparation method |
CN105561781A (en) * | 2015-12-14 | 2016-05-11 | 重庆大学 | Method for removing NOx in sintering flue gas through low-temperature SCR (Selective Catalytic Reduction) catalyst |
CN105536884A (en) * | 2016-01-18 | 2016-05-04 | 北京国电龙源环保工程有限公司 | Method for regenerating waste denitration catalyst by selectively implanting active ingredients |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109507365A (en) * | 2019-01-08 | 2019-03-22 | 苏州西热节能环保技术有限公司 | A method of measurement SCR catalyst regeneration content of vanadium in load liquid |
CN109507365B (en) * | 2019-01-08 | 2022-02-22 | 苏州西热节能环保技术有限公司 | Method for measuring vanadium content in negative carrier liquid for SCR catalyst regeneration |
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Application publication date: 20170531 |