CN105536879B - A kind of low-temperature denitration manganese series catalyzer load low temperature glue and preparation method thereof - Google Patents
A kind of low-temperature denitration manganese series catalyzer load low temperature glue and preparation method thereof Download PDFInfo
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- CN105536879B CN105536879B CN201510905928.9A CN201510905928A CN105536879B CN 105536879 B CN105536879 B CN 105536879B CN 201510905928 A CN201510905928 A CN 201510905928A CN 105536879 B CN105536879 B CN 105536879B
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- 239000003292 glue Substances 0.000 title claims abstract description 28
- 150000002696 manganese Chemical class 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 32
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims abstract description 26
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 9
- 230000033228 biological regulation Effects 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000084 colloidal system Substances 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 31
- 230000000694 effects Effects 0.000 abstract description 9
- 210000002381 plasma Anatomy 0.000 abstract description 4
- 239000007767 bonding agent Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 14
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 8
- 230000008569 process Effects 0.000 description 6
- 229910052878 cordierite Inorganic materials 0.000 description 4
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 108010010803 Gelatin Proteins 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000001186 cumulative effect Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 description 3
- 239000008273 gelatin Substances 0.000 description 3
- 229920000159 gelatin Polymers 0.000 description 3
- 235000019322 gelatine Nutrition 0.000 description 3
- 235000011852 gelatine desserts Nutrition 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 239000011149 active material Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 238000001802 infusion Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000009938 salting Methods 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002803 maceration Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
-
- 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
-
- B01J35/23—
Abstract
The invention discloses a kind of low-temperature denitration manganese series catalyzer load low temperature glue, its preparation method comprises the following steps:1) absolute ethyl alcohol, water, isopropanol and tetraethyl orthosilicate, catechol and formaldehyde are added into three-necked flask successively, are stirred continuously and ultrasonic disperse, obtain uniform mixed liquor I;2) it is slowly added to strong acid into gained mixed liquor I, regulation pH value obtains mixed liquor I I, while is stirred and ultrasonic disperse;3) mixed liquor I I is heated and carries out constant temperature stirring reaction, be described low-temperature denitration manganese series catalyzer load low temperature glue to sticky transparent colloid is obtained.Low-temperature denitration manganese series catalyzer load low temperature glue of the present invention can solve to contain K in existing bonding agent, Na plasmas, or the reaction acid position of catalyst surface is covered, the problems such as causing catalyst activity greatly to reduce, and the low-temperature denitration manganese series catalyzer load low temperature glue prepared can effectively improve carrier and the binding strength of catalyst activity component, it is adapted to popularization and application.
Description
Technical field
The invention belongs to chemical technology field, is related to a kind of adhesive, and in particular to a kind of low-temperature denitration manganese series catalyzer
Load low temperature glue and preparation method thereof.
Background technology
Nitrogen oxides (NOx) essentially from the fossil fuel in cement plant, glass factory, thermal power plant etc. burning, not only
Only it is the major reason for causing acid rain, additionally it is possible to cause the environmental problems such as depletion of the ozone layer, photochemical fog, haze, serious shadow
Ring ecological environment and human health.With becoming increasingly conspicuous for environmental problem, countries in the world have all started the improvement to environmental problem.
In the technology of control nitrogen oxides, selective catalysis reduction technique (SCR) is due to efficient feature, being weight with low cost
The denitration technology wanted.
In the preparation of low temperature catalyst, catalyst be supported on the mechanical strength of catalyst, service life and
Catalytic activity etc. has a major impact.Therefore, infusion process, ion-exchange, sol-gal process, cladding process etc. can typically be used
Method loads to catalyst.Infusion process is made carrier impregnation in the salting liquid of active material by high-temperature calcination processing
The method that active material forms oxide cluster in carrier surface, is generally used for preparing fine catalyst.The method can also be used for violet green grass or young crops
Stone etc. has the load of definite shape carrier, and concrete operation method is first in one layer of Al of cordierite coating2O3、TiO2Deng increase surface
Product, after by multiple maceration obtain catalyst;Method operation is complex, and the high-temperature calcination consumption energy.Sol-gal process
Typically using metal alkoxide, acid and absolute ethyl alcohol as raw material, the salting liquid of active component is added, the molten of stabilization is made after aged
Glue.To colloidal sol dry the various catalyst of the obtained load of the processing such as calcination again.Generally powder catalyst.Ion-exchange
Make carrier with ion-exchanger, in the form of counter ion introduce active component, prepare high dispersive, large surface load type metal or
Metal ion catalyst, it is generally used for preparing the catalyst of zeolites or siliceous type as carrier.Therefore, suitable load is chosen
Mode has particularly important meaning.
Manganese series catalyzer especially has good low-temperature catalytic activity, has DEVELOPMENT PROSPECT.In actual production process, it is necessary to
Powder catalyst is loaded, carrier is generally cordierite, glass fibre etc., and powder catalyst presence is glued with carrier
The problem of knot property is bad.And contain K in general bonding agent, Na plasmas, or the reaction acid position of catalyst surface is covered,
And cause catalyst activity greatly to reduce, therefore need badly and a kind of be suitable for a nanometer low temperature glue for low-temperature denitration manganese series catalyzer.
The content of the invention
It is an object of the present invention to provide a kind of low-temperature denitration manganese series catalyzer load low temperature glue and preparation method thereof, can solve
Contain K, Na plasma in existing bonding agent, or the reaction acid position covering of catalyst surface is caused into catalyst activity pole
Big the problems such as reducing, and the low-temperature denitration manganese series catalyzer load low temperature glue prepared can effectively improve carrier and catalyst activity
The binding strength of component, it is adapted to popularization and application.
To achieve the above object, the technical solution adopted by the present invention is:
A kind of preparation method of low-temperature denitration manganese series catalyzer load low temperature glue, comprises the following steps:
1) absolute ethyl alcohol, water, isopropanol, tetraethyl orthosilicate, catechol and formalin are added into three mouthfuls of burnings successively
Bottle, is stirred continuously and ultrasonic disperse, obtains uniform mixed liquor I;
2) strong acid is slowly added into gained mixed liquor I, regulation pH value obtains mixed liquor I I, be stirred simultaneously to 2~4
And ultrasonic disperse;
3) mixed liquor I I is heated to 70~90 DEG C, and carries out constant temperature 2~8h of stirring reaction, extremely obtain sticky transparent colloid
(having wall built-up phenomenon in beaker), it is described low-temperature denitration manganese series catalyzer load low temperature glue.
In such scheme, the absolute ethyl alcohol, water, the volume ratio of tetraethyl orthosilicate and isopropanol are (3~8):1:(2~
4):(0.05~0.1).
In such scheme, the volume ratio of the catechol and formalin is (1~1.2):1.
In such scheme, the volume ratio of the tetraethyl orthosilicate and formalin is (20~60):1.
In such scheme, the strong acid is hydrochloric acid or nitric acid, and concentration is 1~3mol/L.
According to such scheme prepare low-temperature denitration manganese series catalyzer load low temperature glue, available for carrier (such as cordierite,
Glass cloth etc.) and low-temperature denitration manganese of catalyst activity component (manganese systems) the load combination preparation with greater activity and service life
Series catalysts.
The present invention using isopropanol can prevent due in gel solvent rate of volatilization it is too fast caused by face checking problem;
Simultaneously by the way of modification by copolymerization, with reference to the reaction of catechol and formaldehyde, realize that the regulation to low temperature glue adhesive property is made
With increase binding strength.
Beneficial effects of the present invention are:
1) raw material of the present invention is simple and easy to get, without K, Na plasmas, avoids catalyst poisoning;The low temperature glue of preparation
In acidity, the performance of catalytic can effectively ensure that.
2) low temperature glue prepared can effectively improve carrier (such as cordierite, glass cloth etc.) and catalyst activity component (manganese systems
Catalyst etc.) binding strength, effectively extend gained composite catalyst life-span;And first apply one layer of load compared in matrix surface
Body layer, then by active layer be coated on coating surface method, its using sol-gal process synthesis technique it is simple.
3) low temperature glue for preparing the present invention is applied to the load of low-temperature denitration catalyst carrier and catalyst activity component
With reference to obtained low-temperature denitration catalyst is not required to be sintered, energy-saving, while the inactivation of catalyst under high temperature can be avoided to show
As.
4) can be by changing control of the addition realization of ethanol to the low temperature adhesiveness and catalyst concn.
5) present invention using isopropanol and combines the reaction of catechol and formaldehyde, realizes the tune to low temperature glue adhesive property
Section acts on.
6) present invention is acted on using ultrasonic disperse, is contributed between reactant to be sufficiently mixed, is greatly reduced the reaction time.
Embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention is not
It is limited only to the following examples.
Following examples unless specific instructions, the commercially available chemical reagent of reagent or industrial products of use.
In following examples, the formalin is commercially available chemical reagent, and its mass concentration is 40%.
Embodiment 1
A kind of low-temperature denitration manganese series catalyzer load low temperature glue, its preparation method comprise the following steps:
1) successively by 30ml absolute ethyl alcohols, 10ml deionized waters, 0.5ml isopropanols, 20ml tetraethyl orthosilicates, catechol
(wherein the volume ratio of catechol and formalin is 1 with formaldehyde:1, the two cumulative volume is 1ml) add in three-necked flask,
It is stirred continuously and ultrasonic disperse, continues 30min, obtain uniform mixed liquor I;
2) hydrochloric acid solution (concentration 1mol/L) is slowly added into gained mixed liquor I, regulation pH value is 2, obtains mixed liquor
II, while be stirred and ultrasonic disperse, time 10min;
3) mixed liquor I I is heated to 70 DEG C with 3 DEG C/min speed, and carries out constant temperature stirring reaction 8h, it is sticky to obtaining
Gelatin body (has wall built-up phenomenon) in beaker, is described low-temperature denitration manganese series catalyzer load low temperature glue.
Embodiment 2
A kind of low-temperature denitration manganese series catalyzer load low temperature glue, its preparation method comprise the following steps:
1) successively by 80ml absolute ethyl alcohols, 10ml deionized waters, 0.5ml isopropanols, 27ml tetraethyl orthosilicates, catechol
(wherein the volume ratio of catechol and formalin is 1.1 with formaldehyde:1, the two cumulative volume is 1.5ml) add three-necked flask
In, it is stirred continuously and ultrasonic disperse, continues 30min, obtain uniform mixed liquor I;
2) hydrochloric acid solution (concentration 1mol/L) is slowly added into gained mixed liquor I, regulation pH value is 3, obtains mixed liquor
II, while be stirred and ultrasonic disperse, time 10min;
3) mixed liquor I I is heated to 80 DEG C with 3 DEG C/min speed, and carries out constant temperature stirring reaction 4h, it is sticky to obtaining
Gelatin body (has wall built-up phenomenon) in beaker, is described low-temperature denitration manganese series catalyzer load low temperature glue.
Embodiment 3
A kind of low-temperature denitration manganese series catalyzer load low temperature glue, its preparation method comprise the following steps:
1) successively by 50ml absolute ethyl alcohols, 10ml deionized waters, 0.5ml isopropanols, 40ml tetraethyl orthosilicates, catechol
(wherein the volume ratio of catechol and formalin is 1.2 with formaldehyde:1, the two cumulative volume is 1.5ml) add three-necked flask
In, it is stirred continuously and ultrasonic disperse, continues 30min, obtain uniform mixed liquor I;
2) hydrochloric acid solution (concentration 1mol/L) is slowly added into gained mixed liquor I, regulation pH value is 4, obtains mixed liquor
II, while be stirred and ultrasonic disperse, time 10min;
3) mixed liquor I I is heated to 90 DEG C with 3 DEG C/min speed, and carries out constant temperature stirring reaction 2h, it is sticky to obtaining
Gelatin body (has wall built-up phenomenon) in beaker, is described low-temperature denitration manganese series catalyzer load low temperature glue.
Each raw material proportioning cited by the present invention can realize the present invention, and the bound value of each raw material, interval value
The present invention can be realized, the bound value and interval value of technological parameter of the invention can realize the present invention, differ herein
One enumerates.
Claims (6)
1. a kind of preparation method of low-temperature denitration manganese series catalyzer load low temperature glue, it is characterised in that comprise the following steps:
1) absolute ethyl alcohol, water, isopropanol, tetraethyl orthosilicate, catechol and formalin are added successively, are stirred continuously
With ultrasonic disperse, uniform mixed liquor I is obtained;
2) strong acid is slowly added into gained mixed liquor I, regulation pH value obtains mixed liquor I I, while be stirred and surpass to 2~4
Sound disperses;
3) mixed liquor I I is heated to 70~90 DEG C, and carries out constant temperature 2~8h of stirring reaction, to sticky transparent colloid is obtained, be
Described low-temperature denitration manganese series catalyzer load low temperature glue.
2. preparation method according to claim 1, it is characterised in that the absolute ethyl alcohol, water, tetraethyl orthosilicate and isopropyl
The volume ratio of alcohol is (3~8):1:(2~4):(0.05~0.1).
3. preparation method according to claim 1, it is characterised in that the volume ratio of the catechol and formalin
For (1~1.2):1.
4. preparation method according to claim 1, it is characterised in that the volume of the tetraethyl orthosilicate and formalin
Than for (20~60):1.
5. preparation method according to claim 1, it is characterised in that the strong acid is hydrochloric acid or nitric acid, concentration is 1~
3mol/L。
6. according to low-temperature denitration manganese series catalyzer load low temperature glue made from any one of Claims 1 to 5 preparation method.
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CN201510905928.9A CN105536879B (en) | 2015-12-09 | 2015-12-09 | A kind of low-temperature denitration manganese series catalyzer load low temperature glue and preparation method thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101830447A (en) * | 2010-06-03 | 2010-09-15 | 北京化工大学 | Preparation method of beta-silicon nitride nanowire |
CN102151564A (en) * | 2011-01-30 | 2011-08-17 | 广州市威格林环保科技有限公司 | Preparation method and slurry of denitration integral type catalyst |
CN103194438A (en) * | 2013-04-18 | 2013-07-10 | 北京工业大学 | Preparation method of mesoporous carbon/silicon composite material |
CN104448692A (en) * | 2014-11-18 | 2015-03-25 | 北京科技大学 | Preparation method of insulation board doped with modified nanopore SiO2 |
-
2015
- 2015-12-09 CN CN201510905928.9A patent/CN105536879B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101830447A (en) * | 2010-06-03 | 2010-09-15 | 北京化工大学 | Preparation method of beta-silicon nitride nanowire |
CN102151564A (en) * | 2011-01-30 | 2011-08-17 | 广州市威格林环保科技有限公司 | Preparation method and slurry of denitration integral type catalyst |
CN103194438A (en) * | 2013-04-18 | 2013-07-10 | 北京工业大学 | Preparation method of mesoporous carbon/silicon composite material |
CN104448692A (en) * | 2014-11-18 | 2015-03-25 | 北京科技大学 | Preparation method of insulation board doped with modified nanopore SiO2 |
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