CN106824077A - A kind of preparation method of nitric oxide adsorbent - Google Patents
A kind of preparation method of nitric oxide adsorbent Download PDFInfo
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- CN106824077A CN106824077A CN201710106606.7A CN201710106606A CN106824077A CN 106824077 A CN106824077 A CN 106824077A CN 201710106606 A CN201710106606 A CN 201710106606A CN 106824077 A CN106824077 A CN 106824077A
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- preparation
- activated carbon
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- adsorption
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- B01D53/02—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 by adsorption, e.g. preparative gas chromatography
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/40—Nitrogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
Abstract
The present invention relates to a kind of preparation method of nitric oxide adsorbent, belong to technical field of absorbent.The present invention can be necessarily modified by method physically or chemically to the physical arrangement on the pore-size distribution of activated carbon and surface, chemical functional group, the present invention is pre-processed with salpeter solution using equi-volume impregnating to activated carbon, then in its area load cobalt nitrate and potassium nitrate, make it that there is adsorption efficiency higher at 20 DEG C~200 DEG C；Compared with existing modified activated carbon, adsorption effect is more obvious, and its NO adsorption capacity can reach 59.0649mg/g (being counted with NO) in efficiency as more than 90%, and with good regenerability.
Description
Technical field：
The present invention relates to a kind of preparation method of NO adsorbents, make it that there is adsorption efficiency higher at 20 DEG C~200 DEG C,
And regenerability is good.Belong to technical field of absorbent.
Background technology
Nitrogen oxides (NOx) it is major pollutants in air, NOxMainly by NO and NO2Composition, these pernicious gases
Ozone, photochemical fog and acid rain are not only resulted in, the health of people can be also damaged, lung can be stimulated, cause the breathing system of people
The diseases such as system, lung, liver.Controlling the main method of nitrogen oxides includes SCR, SNCR, absorption and absorption.Activated carbon is a kind of normal
Adsorbent, with larger specific surface area and pore volume, thermochemical property stabilization, wide material sources do not have secondary pollution
The advantages of, it is always a research field for hot topic.
Can be to the physical arrangement on the pore-size distribution of activated carbon and surface, chemical function by method physically or chemically
It is a focus of current activated carbon research field that group carries out certain being modified.The present invention is by cobalt nitrate and potassium nitrate to activated carbon
It is modified, cobaltosic oxide and potassium oxide is generated in activated carbon surface and hole, cobaltosic oxide promotes NO catalysis oxidations
It is NO2And adsorbed, potassium oxide can aid in absorption NO2, strengthen the adsorption effect of NO.Because activated carbon is in the shape of high temperature
The phenomenon of CO and spontaneous combustion is easily produced under state, so having the research of the NO adsorbents of greater activity also less at 200 DEG C.This hair
In bright, forming cobaltosic oxide in activated carbon surface has the characteristic of storage oxygen, can suppress to produce CO to release substantial amounts of heat.Simultaneously
Can be under conditions of high temperature and NO in the potassium oxide of activated carbon surfacexReact, further adsorb NO.
The content of the invention
For the technological difficulties and development bottleneck of NO adsorbents, the present invention provides a kind of NO and prepares formula and method, makes suction
Attached dose has adsorption activity higher in 20 DEG C -200 DEG C or so of flue gas condition, and with good regenerability.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows：
The present invention loads cobalt nitrate and potassium nitrate using equi-volume impregnating in activated carbon surface.
A kind of preparation method of nitric oxide adsorbent, it is characterised in that：
1) HNO of the cocoanut active charcoal in 0.5mol/L of 16~20 mesh will be sized to3The medium volume impregnation 12h of solution, makes
Its dipping is abundant；Incipient impregnation is that dipping solution volume is equal to activated carbon heap volume；
2) it is washed with deionized repeatedly to filter liquor in neutrality after standing 12h；
3) and then in the medium volume impregnation 12h of cobalt nitrate solution；
4) by step 3) product that obtains dries 12h in being put into baking oven in 105 DEG C；
5) and then in the medium volume impregnation 12h of potassium nitrate solution；
6) by step 5) product that obtains dries 12h in being put into baking oven in 105 DEG C；
7) by step 6) gained solid is put into tubular type fabric resistor stove, and roasting 2 is small under the conditions of 400 DEG C under nitrogen protection
When, naturally cool to room temperature.
Preferred steps 3) cobalt salt is cabaltous nitrate hexahydrate, concentration is between 0.1mol/L~0.5mol/L；
Preferred steps 5) sylvite is potassium nitrate, concentration is between 0.1mol/L~0.6mol/L；
Adsorbent of the invention can still keep absorption higher at 20 DEG C~200 DEG C by the NO absorption in flue gas after regeneration
Activity.
The advantage is that：There is excellent NO absorption properties at normal temperatures, its NO adsorption capacity can reach
59.0649mg/g (being counted with NO) is in efficiency as more than 90%.(2), at high temperature 200 DEG C still have NO adsorption activities higher.
(3) adsorption activity higher is still kept after regenerating.
Brief description of the drawings
Fig. 1 is former state and cobalt nitrate and potassium nitrate modified activated carbon the NO adsorption efficiencies figure at 100 DEG C.Wherein curve 1,2,
3rd, 4 former state, example 1, example 2, the efficiency curve of the sample of example 3 are corresponded to respectively.
Fig. 2 is gained adsorbent NO adsorption efficiency figures at 20 DEG C~200 DEG C in example 2.The wherein sample of curve corresponding instance 2
Efficiency curve of the product in different temperatures.
Fig. 3 be example 2 in gained adsorbent before regeneration with 400 DEG C regeneration after NO adsorption efficiency figures.
Specific embodiment
With reference to embodiment, the present invention will be further described, but the present invention is not limited to following examples.
Embodiment 1：
The cocoanut active charcoal that 18g is sized to 16~20 mesh is put into the 0.5mol/L HNO of 30ml3The medium volume leaching of solution
Stain, it is in neutral (pH=7) to be washed with deionized repeatedly after 12h to filter liquor；Then it is molten in the 0.3mol/L cobalt nitrates of 30ml
The medium volume impregnation 12h of liquid；It is put into baking oven and dries 12h in 105 DEG C；Then 30ml 0.1mol/L potassium nitrate solutions in
Incipient impregnation 12h；It is put into baking oven and dries 12h in 105 DEG C；Gained solid is put into tubular type fabric resistor stove, in nitrogen protection
2 hours are calcined under the conditions of lower 400 DEG C, room temperature is naturally cooled to, 1# adsorbents are obtained.
Embodiment 2：
The cocoanut active charcoal that 18g is sized to 16~20 mesh is put into the 0.5mol/L HNO of 30ml3The medium volume leaching of solution
Stain, it is in neutral (pH=7) to be washed with deionized repeatedly after 12h to filter liquor；Then it is molten in the 0.3mol/L cobalt nitrates of 30ml
The medium volume impregnation 12h of liquid；It is put into baking oven and dries 12h in 105 DEG C；Then 30ml 0.5mol/L potassium nitrate solutions in
Incipient impregnation 12h；It is put into baking oven and dries 12h in 105 DEG C；Gained solid is put into tubular type fabric resistor stove, in nitrogen protection
2 hours are calcined under the conditions of lower 400 DEG C, room temperature is naturally cooled to, 2# adsorbents are obtained.
Embodiment 3：
The cocoanut active charcoal that 18g is sized to 16~20 mesh is put into the 0.5mol/L HNO of 30ml3The medium volume leaching of solution
Stain, it is in neutral (pH=7) to be washed with deionized repeatedly after 12h to filter liquor；Then it is molten in the 0.3mol/L cobalt nitrates of 30ml
The medium volume impregnation 12h of liquid；It is put into baking oven and dries 12h in 105 DEG C；Then 30ml 0.6mol/L potassium nitrate solutions in
Incipient impregnation 12h；It is put into baking oven and dries 12h in 105 DEG C；Gained solid is put into tubular type fabric resistor stove, in nitrogen protection
2 hours are calcined under the conditions of lower 400 DEG C, room temperature is naturally cooled to, 3# adsorbents are obtained.
Test case 1
So that as former state, the 1# adsorbents of example 1, the 2# adsorbents of example 2 and the 3# adsorbents of example 3 carry out NO absorption respectively
Test.Unstripped gas composition is as follows：NO (700ppm), 10%O2, N2Used as Balance Air, tolerance is 2.7L/min, and test adsorbent exists
100 DEG C of adsorption efficiency curve, test result such as Fig. 1.By test result as can be seen that 2# adsorbents present good NO suctions
Attached activity, at 100 DEG C, efficiency holding more than 90% can maintain 105min.
Test case 2
With the adsorbent of example 2, NO absorption tests are carried out.Unstripped gas composition is as follows：NO (700ppm), 10%O2, N2As
Balance Air, tolerance is 2.7L/min, adsorption efficiency curve of the test adsorbent at 20~200 DEG C, test result such as Fig. 2.By surveying
Test result can be seen that temperature has certain influence, but the adsorbent on adsorbent effect not only at normal temperatures with good
Absorption property, and at 200 DEG C, 90min can be reached in adsorption efficiency holding more than 90%.
Test case 3
After the adsorbent of example 2 to having adsorbed NO heats 2h regeneration at 400 DEG C, NO absorption tests are carried out.Unstripped gas is constituted
It is as follows：NO (700ppm), 10%O2, N2Used as Balance Air, tolerance is 2.7L/min, suction of the adsorbent at 100 DEG C after test regeneration
Attached efficiency curve, test result such as Fig. 3.By test result as can be seen that at 100 DEG C, adsorption efficiency keeps more than 90%
In the case of adsorption time can reach 85min, activity higher is still kept, with preferable regenerability.
Claims (3)
1. a kind of preparation method of nitric oxide adsorbent, it is characterised in that：
1) HNO of the cocoanut active charcoal in 0.5mol/L of 16~20 mesh will be sized to3The medium volume impregnation 12h of solution, impregnates it
Fully；Incipient impregnation is that dipping solution volume is equal to activated carbon heap volume；
2) it is washed with deionized repeatedly to filter liquor in neutrality after standing 12h；
3) and then in the medium volume impregnation 12h of cobalt nitrate solution；
4) by step 3) product that obtains dries 12h in being put into baking oven in 105 DEG C；
5) and then in the medium volume impregnation 12h of potassium nitrate solution；
6) by step 5) product that obtains dries 12h in being put into baking oven in 105 DEG C；
7) by step 6) gained solid is put into tubular type fabric resistor stove, is calcined 2 hours under the conditions of 400 DEG C under nitrogen protection,
Naturally cool to room temperature.
2. preparation method as claimed in claim 1, it is characterised in that：The step 3) in cobalt nitrate solution concentration be
0.1mol/L~0.5mol/L.
3. preparation method as claimed in claim 1, it is characterised in that：The step 5) in nitric acid potassium concn 0.1mol/L~
Between 0.6mol/L.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108889274A (en) * | 2018-07-19 | 2018-11-27 | 深圳市环球绿地新材料有限公司 | A kind of carried active carbon and its preparation method and application |
| CN111318157A (en) * | 2020-03-13 | 2020-06-23 | 云南民族大学 | Preparation method, product and application of modified carbide slag desulfurization and denitrification agent |
| CN111578275A (en) * | 2020-04-03 | 2020-08-25 | 乐清市亿得利燃烧器有限公司 | Combustor with low emission of nitrogen oxides |
| CN114588891A (en) * | 2022-02-18 | 2022-06-07 | 国电电力发展股份有限公司 | Denitration catalyst and preparation method and application thereof |
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| CN101480603A (en) * | 2008-12-30 | 2009-07-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Nitrous oxides gas adsorbing substance and preparation method thereof |
| CN101693192A (en) * | 2009-10-23 | 2010-04-14 | 中国科学院过程工程研究所 | Process for preparing nitric oxide adsorbent with high adsorption capacity |
| CN101879435A (en) * | 2010-06-08 | 2010-11-10 | 华东理工大学 | High-adsorption-capacity room-temperature nitrogen oxide adsorbent and preparation method thereof |
| CN101884906A (en) * | 2010-07-06 | 2010-11-17 | 上海纳米技术及应用国家工程研究中心有限公司 | Modified honeycomb activated carbon with nitric oxide adsorption function and preparation method thereof |
| CN103736458A (en) * | 2014-01-08 | 2014-04-23 | 中国科学院过程工程研究所 | Preparation method of NOx adsorbent operated at room temperature |
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2017
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Patent Citations (5)
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|---|---|---|---|---|
| CN101480603A (en) * | 2008-12-30 | 2009-07-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Nitrous oxides gas adsorbing substance and preparation method thereof |
| CN101693192A (en) * | 2009-10-23 | 2010-04-14 | 中国科学院过程工程研究所 | Process for preparing nitric oxide adsorbent with high adsorption capacity |
| CN101879435A (en) * | 2010-06-08 | 2010-11-10 | 华东理工大学 | High-adsorption-capacity room-temperature nitrogen oxide adsorbent and preparation method thereof |
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| CN103736458A (en) * | 2014-01-08 | 2014-04-23 | 中国科学院过程工程研究所 | Preparation method of NOx adsorbent operated at room temperature |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108889274A (en) * | 2018-07-19 | 2018-11-27 | 深圳市环球绿地新材料有限公司 | A kind of carried active carbon and its preparation method and application |
| CN111318157A (en) * | 2020-03-13 | 2020-06-23 | 云南民族大学 | Preparation method, product and application of modified carbide slag desulfurization and denitrification agent |
| CN111578275A (en) * | 2020-04-03 | 2020-08-25 | 乐清市亿得利燃烧器有限公司 | Combustor with low emission of nitrogen oxides |
| CN114588891A (en) * | 2022-02-18 | 2022-06-07 | 国电电力发展股份有限公司 | Denitration catalyst and preparation method and application thereof |
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Application publication date: 20170613 |