CN106563439A - La-modified La-V2O5/TiO2 desulfurization catalyst - Google Patents
La-modified La-V2O5/TiO2 desulfurization catalyst Download PDFInfo
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- CN106563439A CN106563439A CN201610954409.6A CN201610954409A CN106563439A CN 106563439 A CN106563439 A CN 106563439A CN 201610954409 A CN201610954409 A CN 201610954409A CN 106563439 A CN106563439 A CN 106563439A
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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
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8603—Removing sulfur compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/206—Rare earth metals
- B01D2255/2063—Lanthanum
Abstract
The invention discloses a La-modified La-V2O5/TiO2 desulfurization catalyst, wherein metatitanic acid slurry, ammonium metavanadate, oxalic acid and lanthanum chloride are adopted as main synthesis raw materials. The raw materials are subjected to magnetization reaction to synthesize a novel modified desulfurization and denitration catalyst. The catalyst is high in desulfurization efficiency.
Description
Technical field
The present invention relates to a kind of modified La-V of La2O5/TiO2Catalyst, with metatitanic acid slurry, ammonium metavanadate, oxalic acid, chlorination
Lanthanum is main synthesis material, belongs to catalyst technical field.
Background technology
It is various harmful containing sulfur dioxide, nitrogen oxides and dust etc. in coal-burning boiler and the flue gas of thermal power plant discharge
Composition, the natural resources, the ecosystem, material, visibility and public health to China constitutes serious threat, while
Socio-economic development and the normal life of the people are affected, SO is controlled2, NO discharges have become China quite over a long time
One of vital task.Dry fume is while desulfurization (SO2) denitration (NO) because can be prevented effectively from equipment repeat configure, running cost
It is simple to operate with low, it is considered as a very promising flue gases purification the features such as without secondarily polluted water.
V2O5/TiO2As desulphurization denitration catalyst, his desulphurization denitration rate is not especially high, and catalyst regeneration is also to perplex its one
Problem, now we are using the modified obtained La-V of rare element La2O5/TiO2Catalyst effectively improves V2O5/TiO2Urge
The two defects of agent.
The content of the invention
The technical solution used in the present invention is:A kind of La modified La-V2O5/TiO2Catalyst, with metatitanic acid slurry, inclined vanadium
Sour ammonium, oxalic acid, lanthanum chloride is main synthesis material
Comprise the following steps:
Step 1, first by metatitanic acid starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4, a certain amount of ammonium metavanadate and oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8, lanthanum chloride is dissolved in in deionized water the removal of impurities under ultrasonic oscillation;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Beneficial effect of the present invention:V2O5/TiO2Catalyst desulfurizing denitration rate is general, and the present invention passes through to introduce La rare elements,
By magnetic agitation in preparation process, calcine under atmosphere under sufficient air, these method of modifying make obtained catalyst
Effect is greatly promoted and greatly improves desulphurization denitration rate, is 1 in lanthanum chloride and ammonium metavanadate mass ratio:6, lanthanum chloride
5g, meta-aluminic acid ammonium 30g, metatitanic acid slurry 10ml, oxalic acid 10ml, deionized water 150ml, obtained La-V2O5/TiO2Catalyst takes off
Sulphur denitration effect is best.
Specific embodiment
Embodiment 1
Produce lanthanum chloride and ammonium metavanadate mass ratio 1:1 sample.Lanthanum chloride 5g, meta-aluminic acid ammonium 5g, metatitanic acid slurry 10ml, oxalic acid
10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,5g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Sheetmolding is pushed after stain 6h in certain power;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,5g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Embodiment 2
Produce lanthanum chloride and ammonium metavanadate mass ratio 1:2 sample.Lanthanum chloride 5g, meta-aluminic acid ammonium 10g, metatitanic acid slurry 10ml, oxalic acid
10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,10g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,5g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Embodiment 3
Produce lanthanum chloride and ammonium metavanadate mass ratio 1:3 sample.Lanthanum chloride 5g, meta-aluminic acid ammonium 15g, metatitanic acid slurry 10ml, oxalic acid
10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,15g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,5g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Embodiment 4
Produce lanthanum chloride and ammonium metavanadate mass ratio 1:4 sample.Lanthanum chloride 5g, meta-aluminic acid ammonium 20g, metatitanic acid slurry 10ml, oxalic acid
10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,20g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,5g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Embodiment 5
Produce lanthanum chloride and ammonium metavanadate mass ratio 1:5 sample.Lanthanum chloride 5g, meta-aluminic acid ammonium 25g, metatitanic acid slurry 10ml, oxalic acid
10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,25g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,5g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Embodiment 6
Produce lanthanum chloride and ammonium metavanadate mass ratio 1:6 sample.Lanthanum chloride 5g, meta-aluminic acid ammonium 30g, metatitanic acid slurry 10ml, oxalic acid
10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,30g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,5g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Embodiment 7
Produce lanthanum chloride and ammonium metavanadate mass ratio 1:7 sample.Lanthanum chloride 5g, meta-aluminic acid ammonium 35g, metatitanic acid slurry 10ml, oxalic acid
10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,35g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,5g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Embodiment 8
Produce lanthanum chloride and ammonium metavanadate mass ratio 1:8 sample.Lanthanum chloride 5g, meta-aluminic acid ammonium 40g, metatitanic acid slurry 10ml, oxalic acid
10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,40g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,5g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Embodiment 9
Produce lanthanum chloride and ammonium metavanadate mass ratio 1.2:1 sample.Lanthanum chloride 6g, meta-aluminic acid ammonium 5g, metatitanic acid slurry 10ml, grass
Sour 10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,5g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,6g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Embodiment 10
Produce lanthanum chloride and ammonium metavanadate mass ratio 1.3:1 sample.Lanthanum chloride 6.5g, meta-aluminic acid ammonium 5g, metatitanic acid slurry 10ml, grass
Sour 10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,5g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid point 20 drop speed per minute is then added dropwise the magnetic force when being added dropwise is added dropwise and stir
Mix 80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,6.5g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Embodiment 11
Produce lanthanum chloride and ammonium metavanadate mass ratio 1.4:1 sample.Lanthanum chloride 7g, meta-aluminic acid ammonium 5g, metatitanic acid slurry 10ml, grass
Sour 10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,5g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,7g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Embodiment 12
Produce lanthanum chloride and ammonium metavanadate mass ratio 1.5:1 sample.Lanthanum chloride 7.5g, meta-aluminic acid ammonium 5g, metatitanic acid slurry 10ml,
Oxalic acid 10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,5g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,7.5g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Embodiment 13
Produce lanthanum chloride and ammonium metavanadate mass ratio 1.6:1 sample.Lanthanum chloride 8g, meta-aluminic acid ammonium 5g, metatitanic acid slurry 10ml, oxalic acid
10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,5g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid point 20 drop speed per minute is then added dropwise the magnetic force when being added dropwise is added dropwise and stir
Mix 80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,8g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Embodiment 14
Produce lanthanum chloride and ammonium metavanadate mass ratio 1.7:1 sample.Lanthanum chloride 8.5g, meta-aluminic acid ammonium 5g, metatitanic acid slurry 10ml, grass
Sour 10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,5g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid point 20 drop speed per minute is then added dropwise the magnetic force when being added dropwise is added dropwise and stir
Mix 80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,8.5g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Embodiment 15
Produce lanthanum chloride and ammonium metavanadate mass ratio 1.8:1 sample.Lanthanum chloride 9g, meta-aluminic acid ammonium 5g, metatitanic acid slurry 10ml, oxalic acid
10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,5g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,9g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Reference examples 1
Produce lanthanum chloride and ammonium metavanadate mass ratio 1:6 sample.Lanthanum chloride 5g, meta-aluminic acid ammonium 30g, metatitanic acid slurry 10ml, oxalic acid
10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,30g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise is added dropwise and stir oil bath when being added dropwise
80 DEG C of heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, 100 DEG C of dipping 6h of stirring oil bath heating
Compression molding under pressure afterwards;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8,5g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of stirring, Ran Hou in lanthanum chloride solution
Be centrifuged under centrifugal separator, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La-V are obtained2O5/
TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Reference examples 2
Produce lanthanum chloride and ammonium metavanadate mass ratio 1:6 sample.Lanthanum chloride 5g, meta-aluminic acid ammonium 30g, metatitanic acid slurry 10ml, oxalic acid
10ml, deionized water 150ml.
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
The lower 800 DEG C of calcinings 12h of air, is obtained anatase titanium dioxide TiO in step 3 and then Muffle furnace2Carrier;
Step 4,5g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace air2O5/TiO2Urge
Agent;
Step 8,5g lanthanum chlorides are dissolved in into the removal of impurities under ultrasonic oscillation in 150ml deionized waters;
Step 9, by obtained V2O5/TiO2Catalyst is immersed in 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2Catalyst;
Step 10, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
Reference examples 3 are added without the modified samples of La.Meta-aluminic acid ammonium 30g, metatitanic acid slurry 10ml, oxalic acid 10ml, deionized water
150ml。
Step 1, first by 10ml metatitanic acids starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO is obtained2Carrier;
Step 4,30g ammonium metavanadates and 10ml oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, will obtained TiO as stated above2 Carrier is immersed in the mixed liquor, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V in 500 DEG C of Muffle furnace abundance air2O5/
TiO2Catalyst;
Step 8, by prepared La-V2O5/TiO2Catalyst makes 20-30 mesh under sampling machine.
The activity rating of catalyst
The evaluation of simultaneous SO_2 and NO removal catalyst activity is carried out in the fixed bed reactors that internal diameter is 19 mm.Temperature is fixed on 200
DEG C, reaction gas volume consists of 0. 137%SO2、0. 039% NO、0. 043% N H3、2. 5% H2O、3. 9%O2 , Ar is
Balance Air.Total gas flow rate is 430 mL/min.At 200 °C, apparent air speed is 1 850 h for reaction temperature control- 1.Before reaction
Gas afterwards produces Dra ger gas alloying apparatus on-line analyses using Germany, while continuously detecting the concentration of SO2, NO and O2.Inhale
Sulphur reaches the catalyst of saturation in N H3(air speed is 850 h to (h=0. 05)/Ar- 1 ) 330 DEG C of 70 min of regeneration in atmosphere.
As a result the desulphurization denitration of embodiment 6 is shown preferably, because now La metallic elements and V2O5And carrier TiO2Synergy reaches
To best.Basic what change of the modified catalyst of La desulfurization off sulfide effect after regeneration is added, does not add La to be modified
Catalyst regeneration after desulfurization off sulfide effect can reduce much.It can be found that comparative example 1,2,3,4,5,6,7,8 is when each
When kind operation is identical, lanthanum chloride is 1 with ammonium metavanadate mass ratio:When 6, obtained La-V2O5/TiO2Catalyst is imitated
Fruit is preferably that desulfurization off sulfide effect is good, obtained La-V under other ratios2O5/TiO2Catalyst La elements and V2O5And carrier
TiO2Between synergistic action effect be not fine.Contrast implements row 1,9,10,11,12,13,14,15 it is found that lanthanum chloride
It is 1.2 with ammonium metavanadate mass ratio:Obtained La-V when 12O5/TiO2Catalyst effect is best, with the increasing of La elements
Plus or reduction La elements and V2O5And carrier TiO2Synergy can all decline catalytic effect all can be reduced.Implement row 6, with
The control contrast of row 1 is it can be found that in La-V obtained in magnetic agitation2O5/TiO2Catalyst desulfurizing denitration effect will be significantly better than not
It is obtained under magnetic stirring.Embodiment 6, with the contrast of reference examples 2 it can be found that the La-V calcined under sufficient air2O5/TiO2
Catalyst desulfurizing denitration effect will be significantly better than in the or not obtained catalyst of calcining under sufficient air.Embodiment 6, and compares
The contrast of example 3 is it can be found that poor without the element modified catalyst denitration effects of La.
Claims (3)
1. the La-V2O5/TiO2 desulphurization catalysts that a kind of La is modified, it is characterised in that starched with metatitanic acid, ammonium metavanadate, oxalic acid,
Lanthanum chloride is main synthesis material, and by the new modified desulphurization denitration catalyst of magnetization synthesis.
2. the La-V2O5/TiO2 desulphurization catalysts that a kind of La according to claim 1 is modified, it is characterised in that concrete system
Preparation Method is as follows:
Step 1, first metatitanic acid is starched into removal of impurities;
Step 2 then by after removal of impurities metatitanic acid slurry drying;
Calcine in step 3 and then Muffle furnace and anatase titanium dioxide TiO2 carriers are obtained;
Step 4, weigh a certain amount of ammonium metavanadate and oxalic acid, removal of impurities;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid heating is then added dropwise;
Step 6, obtained TiO2 carriers will immerse in the mixed liquor as stated above, under pressure compression molding;
Step 7, again Jing vavuum pumps are filtered, and are dried, and roasting in Muffle furnace abundance air is obtained V2O5/TiO2 catalyst;
Step 8, lanthanum chloride is dissolved in in deionized water the removal of impurities under ultrasonic oscillation;
Step 9, obtained V2O5/TiO2 catalyst is immersed in into oil bath heating in lanthanum chloride solution, then in centrifugal separator
Lower centrifugation, moisture evaporation under rotary evaporator, is then dried prepared La-V2O5/TiO2 catalyst;
Step 10, prepared La-V2O5/TiO2 catalyst is made into 20-30 mesh under sampling machine.
3. the La-V2O5/TiO2 desulphurization catalysts that a kind of La according to claim 1 is modified, it is characterised in that more have
The step of body, includes as follows:
Step 1, first by metatitanic acid starch 90 DEG C of oil bath ultrasound 4h removal of impurities under ultrasonic oscillation;
Step 2 then by after removal of impurities metatitanic acid starch 140 DEG C be air-dried 15h;
Lower 800 DEG C of sufficient air calcines 12h in step 3 and then Muffle furnace, and anatase titanium dioxide TiO2 carriers are obtained;
Step 4, a certain amount of ammonium metavanadate and oxalic acid are weighed, the lower 90 DEG C of oil bath removal of impurities of ultrasonic oscillation;
Step 5, ammonium metavanadate is poured in beaker, oxalic acid 20 drop speed per minute is then added dropwise the magnetic agitation when being added dropwise is added dropwise
80 DEG C of oil bath heating;
Step 6, obtained TiO2 carriers will immerse in the mixed liquor as stated above, the 100 DEG C of leachings of magnetic agitation oil bath heating
Compression molding under pressure after stain 6h;
Step 7, again Jing vavuum pumps are filtered, and 140 DEG C are dried 15h, and roasting 6h is obtained V2O5/ in 500 DEG C of Muffle furnace abundance air
TiO2 catalyst;
Step 8, lanthanum chloride is dissolved in in deionized water the removal of impurities under ultrasonic oscillation;
Step 9, obtained V2O5/TiO2 catalyst is immersed in into 100 DEG C of oil bath heatings 8h of magnetic agitation in lanthanum chloride solution, so
Be centrifuged under centrifugal separator afterwards, under rotary evaporator 180 DEG C moisture evaporation, then 120 DEG C are dried 10h La- are obtained
V2O5/TiO2 catalyst;
Step 10, prepared La-V2O5/TiO2 catalyst is made into 20-30 mesh under sampling machine.
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任飞等: "《普通化学》", 31 August 2014 * |
刘世越: "《常用分析试剂与标准溶液配制标定实用手册 第1卷》", 30 November 2004 * |
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