CN103691476B - A kind of low-temperature synchronous denitration desulphurization catalyst and preparation method - Google Patents
A kind of low-temperature synchronous denitration desulphurization catalyst and preparation method Download PDFInfo
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Abstract
The invention belongs to the preparing technical field of catalyst, disclose a kind of low-temperature synchronous desulphurization denitration catalyst and preparation method.A kind of low-temperature synchronous desulphurization denitration catalyst proposed, the composition of catalyst and percentage by weight are: granular catalyst initial material 83.33%, surfactant and heat stabilizer 3.33%, crosslinking agent 2.50%, reinforcing agent 4.17%, pure ammoniacal liquor 3.34% and deionized water 3.33%; The composition of granular catalyst initial material and percentage by weight are: mesoporous SBA-15 molecular sieve 65.22% ~ 72.28%, nano-TiO
2?10.84% ~ 19.57%, metal oxide auxiliary agent 6.52% ~ 7.23%, oxalic acid 8.69% ~ 9.65%.The present invention can for catalysis S below 300 DEG C
xo
y, NO
xsimultaneous removing, there is good water-resistance, high mechanical properties, specific area is large, heat endurance is high and reactivity is strong feature.
Description
Technical field
The invention belongs to the preparing technical field of catalyst, disclose a kind of low-temperature synchronous desulphurization denitration catalyst and preparation method.
Background technology
Along with a large amount of consumption of industrial development and the energy, SO
2grow with each passing day with NOx discharge, severe contamination environment, brings serious harm to the health of human body, so control SO
2china's main task quite over a long time has been become with the discharge of NOx.At present, the catalyst synchronously carrying out desulphurization denitration in prior art mainly contains active carbon, Cu/Mg/Al, CuO/Al
2o
3; Activated-carbon catalyst comprises traditional activated Pd/carbon catalyst and patent No. Alveolate activated carbon capable (ACH) catalyst disclosed in 03145680.4; Active carbon, Cu/Mg/Al, CuO/Al
2o
3deposit and be middle temperature or high temperature catalyst, there is temperature window high, general effective catalytic temperature is more than 300 DEG C, and below 300 DEG C of temperature, catalytic efficiency obviously declines.
Summary of the invention
For solving the problems of the technologies described above, the object of the invention is to propose a kind of low-temperature synchronous desulphurization denitration catalyst and preparation method.
The present invention adopts following technical scheme for completing above-mentioned purpose:
A kind of low-temperature synchronous desulphurization denitration catalyst, the composition of described catalyst and percentage by weight are: granular catalyst initial material 83.33%, surfactant and heat stabilizer 3.33%, crosslinking agent 2.50%, reinforcing agent 4.17%, pure ammoniacal liquor 3.34% and deionized water 3.33%; The composition of described granular catalyst initial material and percentage by weight are: mesoporous SBA-15 molecular sieve 65.22% ~ 72.28%, nano-TiO
210.84% ~ 19.57%, metal oxide auxiliary agent 6.52% ~ 7.23%, oxalic acid 8.69% ~ 9.65%; Wherein said nano-TiO
2form composite oxides activity with mesoporous SBA-15 molecular sieve and carry base; Described metal oxide auxiliary agent load is carried on base in composite oxides activity and is formed granular catalyst initial material.
Described surfactant and heat stabilizer are one or both the mixing in stearic acid, glycerine.
Described crosslinking agent is methacrylic acid-2-carboxylic ethyl ester.
Described reinforcing agent is glass fibre, plays physics humidification to catalyst.
Described nanoscale TiO
2for Detitanium-ore-type TiO
2; There is two profiles state in titanium oxide: Detitanium-ore-type TiO
2, rutile TiO
2, due to Detitanium-ore-type TiO
2have and compare rutile TiO
2higher catalytic activity, nanoscale TiO
2as a kind of important hydrodesulfurization and NO hydrogenation co-catalyst, the catalytic activity of its existence on active component has larger impact, therefore, selects Detitanium-ore-type TiO
2.
Described composite oxides activity carries base using mesoporous SBA-15 molecular sieve as carrier, by nanoscale TiO
2load on carrier and form composite oxides activity year base, greatly prevent Detitanium-ore-type TiO
2to rutile TiO
2transformation, improve Detitanium-ore-type TiO
2mechanical strength, specific area, heat endurance and reactivity; The binary oxide that this method is formed is that composite reactive carries base, and the main purpose of Kaolinite Preparation of Catalyst is in order to both advantages integrated are in one, seeks the more high catalytic performance after interacting; At nanoscale TiO
2introduce mesoporous SBA-15 molecular sieve and can significantly improve nanoscale TiO
2the transition temperature of crystal formation, improves nanoscale TiO
2heat endurance and reactivity; Mesoporous SBA-15 molecular sieve has texture stable in order and large specific area, the TiO of Detitanium-ore-type simultaneously
2load can increase the TiO of Detitanium-ore-type on the molecular sieve supported base of mesoporous SBA-15
2stability; The TiO2 of Detitanium-ore-type is loaded to and mesoporous SBA-15 molecular sieve is formed composite oxides activity and carry a base and can be used for catalysis S
xo
y, NO
xsimultaneous removing, there is good water-resistance, high mechanical properties, specific area is large, heat endurance is high and reactivity is strong feature.
Composite oxides activity carries base can the activity and selectivity catalytic of the further regulating catalyst of other active components of load; Carry metal oxide-loaded auxiliary agent on base in composite oxides activity and, as catalyst aid, catalytic reaction activity can be improved further.
Described metal oxide auxiliary agent is amphoteric oxide, and object is amphoteric oxide, carries in base activated in high activity, shows the exclusive high catalytic oxidation type of amphoteric oxide or high catalytic reduction, greatly improves the overall catalytic performance of catalyst; And, active activity of carrying basic body can also be improved further by the amphoteric oxide activated, thus again improve the overall catalytic activity of catalyst; Described amphoteric oxide is one or more in Mn oxide, V oxide, Cr oxide, Ce oxide, W oxide, Mo oxide.
Cr oxide in metal oxide auxiliary agent, Mn oxide, Ce oxide are prepared by corresponding nitrate solution pyrolysis respectively; W oxide in metal oxide auxiliary agent and Mo oxide are prepared by ammonium tungstate and the pyrolysis of key acid ammonium respectively, and V oxide is prepared by positive ammonium vanadate, ammonium metavanadate or ammonium poly-vanadate or vanadic sulfate pyrolysis.
A preparation method for low-temperature synchronous desulphurization denitration catalyst, adopts by mesoporous SBA-15 molecular sieve and nano-TiO
2the composite oxides activity formed carries base as first material, granular catalyst is prepared again through mixing procedure, granular catalyst is again through moulding process, namely through rerolling, shaping and calcination, the synchronous denitration desulphurization catalyst of a kind of cellular low-temperature flue gas of final formation, its concrete steps are as follows:
1) mesoporous SBA-15 molecular sieve, nanoscale TiO is prepared
2and metal oxide auxiliary agent;
2) mixing procedure: in a kettle., adds the deionized water of 10 ~ 15mL and is heated to 600-800 DEG C, and the deionized water under high temperature has high locomotor activity as a kind of solvent, contributes to nanoscale TiO
2spread in mesoporous SBA-15 molecular sieve, not containing other metal ion in deionized water, thus avoid the nanoscale TiO caused thus
2reunion; By mesoporous SBA-15 molecular sieve, nano-TiO in step 1
2, metal oxide auxiliary agent and oxalic acid joins in reactor, mesoporous SBA-15 molecular sieve, nano-TiO
2, metal oxide auxiliary agent and oxalic acid addition be respectively: 65.2% ~ 72.28%, 10.84% ~ 19.57%, 6.5% ~ 7.2%, 8.7% ~ 9.6%, reaction 1h, in question response still, material is muddy, after 160 DEG C ~ 200 DEG C drying 50 ~ 60min, transfers in calcination kiln be crushed into granular catalyst initial material after calcination 50 ~ 60min at the temperature of 250 ~ 450 DEG C;
3) moulding process: the granular catalyst initial material taking mixing procedure gained, adds surfactant and heat stabilizer, crosslinking agent, reinforcing agent, and adds pure ammoniacal liquor and deionized water in granular catalyst initial material; The addition of granular catalyst initial material, surfactant and heat stabilizer, crosslinking agent, reinforcing agent, pure ammoniacal liquor and deionized water is respectively: 83.33%, 3.33%, 2.50%, 4.17%, 3.34%, 3.33%; Again through mud refining, vacuum mud refining, under constant temperature and humidity condition old 24h ~ 48h, shaping, under the condition of 60 ~ 80 DEG C dry 60 ~ 90h, in tunnel cave with 180-450 DEG C of sintering 2h ~ 5h, until fully dry, become Faveolate denitration desulphurization catalyst.
Step 2) effect of mesoxalic acid is: oxalic acid at high temperature volatilizees, and for catalyst provides better porosity, is convenient to catalyst with the flue gas and the reaction that need to react and contact;
The object adding pure ammoniacal liquor in step 3) utilizes its alkalescence and strong volatility, after shaping of catalyst, strongly volatilizees in heating process, for catalyst provides more duct, and itself can further improve NO as alkali
xcatalyst adsorb efficiency.
The object adding deionized water in step 3) is the hardness regulating catalyst mud refining, is convenient to shaping, must uses deionized water herein, to prevent other ion of also having in light water, causes the reunion of effective ingredient in catalyst, causes catalytic efficiency to reduce.
A kind of low-temperature synchronous desulphurization denitration catalyst that the present invention proposes and preparation method, adopt mesoporous SBA-15 molecular sieve as carrier, by nanoscale TiO
2load on carrier and form composite oxides activity year base, and add amphoteric oxide as metal oxide oxidation catalyst auxiliary agent on composite oxides activity year base, can for catalysis S below 300 DEG C
xo
y, NO
xsimultaneous removing, there is good water-resistance, high mechanical properties, specific area is large, heat endurance is high and reactivity is strong feature.140-250 DEG C of reaction, during using ammonia steam as absorbent, catalyzing N O
x, SO
2removal efficiency be respectively 90%, more than 95% and there is good life-span and mechanical strength.
Detailed description of the invention
Carry out detailed preparation technology below in conjunction with specific experiment example to the present invention to describe, the present invention is not limited to following instance;
experimental example one:
(1) mixing procedure:
In a kettle., add 10ml deionized water and be heated to 800 DEG C, mesoporous SBA-15 molecular sieve, nano-TiO
2, metal oxide auxiliary agent and oxalic acid joins in reactor by quality 300g:45g:30g:40g, reaction 1h, in question response still, material is muddy, at 160 DEG C of drying 50 ~ 60min, transfers in calcination kiln and is crushed into granular catalyst initial material after 250 ~ 450 DEG C of calcination 50 ~ 60min;
(2) moulding process:
Take the granular catalyst initial material 200g of mixing procedure gained, add stearic acid 8g, add methacrylic acid-2-carboxylic ethyl ester 6g, add glass fibre l0g, add pure ammoniacal liquor 8g, add deionized water 8g through mud refining, vacuum mud refining, under constant temperature and humidity condition old 24h, shaping, under the condition of 60 DEG C dry 60 ~ 90h, in tunnel cave, become Faveolate denitration desulphurization catalyst with 180-450 DEG C of sintering 2h.
experimental example two:
(1) mixing procedure:
In a kettle., add the deionized water of 10mL and be heated to 800 DEG C, mesoporous SBA-15 molecular sieve, nano-TiO
2, provide the salt of oxides additive and oxalic acid to join in reactor by quality 300g:62.5g:30g:40g, reaction 1h, in question response still, material is muddy, at 160 DEG C of drying 50 ~ 60min, transfers in calcination kiln and is crushed into granular catalyst initial material after 250 ~ 450 DEG C of calcination 50 ~ 60min;
(2) moulding process is identical with example one.
experimental example three:
(1) mixing procedure:
In a kettle., add the deionized water of 15ml and be heated to 800 DEG C, mesoporous SBA-15 molecular sieve, nano-TiO
2, provide the salt of oxides additive and oxalic acid to join in reactor by quality 300g:90g:30g:40g, reaction 1h, in question response still, material is muddy, at 160 DEG C of drying 50 ~ 60min, transfers in calcination kiln and is crushed into granular catalyst initial material after 250 ~ 450 DEG C of calcination 50 ~ 60min;
(2) moulding process is identical with example one.
experimental example four:
(1) mixing procedure:
In a kettle., add a certain amount of deionized water and be heated to 800 DEG C, mesoporous SBA-15 molecular sieve, nano-TiO
2, provide the salt of oxides additive and oxalic acid to join in reactor by quality 300g:90g:30g:40g, reaction 1h, in question response still, material is muddy, at 160 DEG C of drying 50 ~ 60min, transfers in calcination kiln and is crushed into granular catalyst initial material after 250 ~ 450 DEG C of calcination 50 ~ 60min;
(2) moulding process:
Take the pellet type catalyst 200g of mixing procedure gained, add glycerine 8g, add methacrylic acid-2-carboxylic ethyl ester 6g, add glass fibre l0g, add pure ammoniacal liquor 8g, add deionized water 8g through mud refining, vacuum mud refining, under constant temperature and humidity condition old 24h, shaping, under the condition of 60 DEG C dry 60 ~ 90h, in tunnel cave, become Faveolate denitration desulphurization catalyst with 180-450 DEG C of sintering 2h.
experimental example five:
(1) mixing procedure is identical with example four
(2) moulding process:
Take the granular catalyst initial material 200g of mixing procedure gained, add glycerine 4g, add stearic acid 4g and add methacrylic acid-2-carboxylic ethyl ester 6g, add glass fibre l0g, add pure ammoniacal liquor 8g, add deionized water 8g through mud refining, vacuum mud refining, under constant temperature and humidity condition old 24h, shaping, under the condition of 60 DEG C dry 60 ~ 90h, in tunnel cave, become Faveolate denitration desulphurization catalyst with 180-450 DEG C of sintering 2h.
Mud refining described in above-described embodiment, vacuum mud refining are all the maturation process of tunnel cave technique, in this not explanation.
laboratory sample test result and calculating
Catalyst activity is tested: utilize simulated experiment to test prepared catalyst.
Experimental simulation device and condition as follows: prepared 5 kinds of catalyst are put into fixing tubular type heater platform respectively, pass into simulated flue gas (SO
2=1000ppm, NO=1000ppm, O
2=13%, steam 8%, N
2for balanced protection gas), air speed ratio=10000h
-1.With NO
xanalyzer detecting catalyst imports and exports the concentration of NO, because the NO in kiln gas
xmore than 90% is NO, thus this to sentence NO more convincing as estimation conditions.The desulfurization of flue gas is comparatively easy, under catalyzed dose and absorbent effect, comparatively easily can realize desulfuration efficiency.
Denitration efficiency computational methods:
=× 100%
In formula
for denitration efficiency,
,
be respectively and import and export NO concentration, unit ppm
Desulfuration efficiency computational methods:
=× 100%
In formula
for desulfuration efficiency,
,
be respectively and import and export SO
2concentration, unit ppm
Table 1: catalyst sample denitration efficiency is tested
Table 2: catalyst sample desulfuration efficiency is tested
Claims (6)
1. a preparation method for low-temperature synchronous desulphurization denitration catalyst, is characterized in that: adopt by mesoporous SBA-15 molecular sieve and anatase type nano TiO
2the composite oxides activity formed carries base as first material, granular catalyst is prepared again through mixing procedure, granular catalyst is again through moulding process, namely through rerolling, shaping and calcination, the synchronous denitration desulphurization catalyst of a kind of cellular low-temperature flue gas of final formation, its concrete steps are as follows:
1) mesoporous SBA-15 molecular sieve, anatase type nano TiO is prepared
2and metal oxide auxiliary agent;
2) mixing procedure: in a kettle., adds the deionized water of 10 ~ 15mL and is heated to 600-800 DEG C, and the deionized water under high temperature has high locomotor activity as a kind of solvent, contributes to anatase type nano TiO
2spread in mesoporous SBA-15 molecular sieve, not containing other metal ion in deionized water, thus avoid the anatase type nano TiO caused thus
2reunion; By the mesoporous SBA-15 molecular sieve in step 1, anatase type nano TiO
2, metal oxide auxiliary agent and oxalic acid joins in reactor, mesoporous SBA-15 molecular sieve, anatase type nano TiO
2, metal oxide auxiliary agent and oxalic acid addition be respectively: 65.22% ~ 72.28%, 10.84% ~ 19.57%, 6.52% ~ 7.23%, 8.69% ~ 9.65%, reaction 1h, in question response still, material is muddy, after 160 DEG C ~ 200 DEG C drying 50 ~ 60min, transfers in calcination kiln be crushed into granular catalyst initial material after calcination 50 ~ 60min at the temperature of 250 ~ 450 DEG C;
3) moulding process: the granular catalyst initial material taking mixing procedure gained, adds surfactant and heat stabilizer, crosslinking agent, reinforcing agent, and adds pure ammoniacal liquor and deionized water in granular catalyst initial material; The addition of granular catalyst initial material, surfactant and heat stabilizer, crosslinking agent, reinforcing agent, pure ammoniacal liquor and deionized water is respectively: 83.33%, 3.33%, 2.50%, 4.17%, 3.34%, 3.33%; Again through mud refining, vacuum mud refining, under constant temperature and humidity condition old 24h ~ 48h, shaping, under the condition of 60 ~ 80 DEG C dry 60 ~ 90h, in tunnel cave with 180-450 DEG C of sintering 2h ~ 5h, until fully dry, become Faveolate denitration desulphurization catalyst.
2. the preparation method of a kind of low-temperature synchronous desulphurization denitration catalyst according to claim 1, is characterized in that: described surfactant and heat stabilizer are one or both the mixing in stearic acid, glycerine.
3. the preparation method of a kind of low-temperature synchronous desulphurization denitration catalyst according to claim 1, is characterized in that: described crosslinking agent is methacrylic acid-2-carboxylic ethyl ester.
4. the preparation method of a kind of low-temperature synchronous desulphurization denitration catalyst according to claim 1, is characterized in that: described reinforcing agent is glass fibre.
5. the preparation method of a kind of low-temperature synchronous desulphurization denitration catalyst according to claim 1, it is characterized in that: described metal oxide auxiliary agent is amphoteric oxide, described amphoteric oxide is one or more in Mn oxide, V oxide, Cr oxide, Ce oxide, Mo oxide.
6. the preparation method of a kind of low-temperature synchronous desulphurization denitration catalyst according to claim 5, is characterized in that: the Cr oxide in metal oxide auxiliary agent, Mn oxide, Ce oxide are prepared by corresponding nitrate solution pyrolysis respectively; Mo oxide in metal oxide auxiliary agent is prepared by ammonium molybdate pyrolysis, and V oxide is prepared by positive ammonium vanadate, ammonium metavanadate or ammonium poly-vanadate or vanadic sulfate pyrolysis.
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CN104174442B (en) * | 2014-08-27 | 2016-04-13 | 清华大学 | A kind of shaping of catalyst technique of low-temperature denitration of flue gas |
CN104437653A (en) * | 2014-12-12 | 2015-03-25 | 海南中航特玻材料有限公司 | Bio-based rubble paper-like catalyst for low-temperature synchronous denitration and desulfurization and preparation method thereof |
CN105195171A (en) * | 2015-11-03 | 2015-12-30 | 海南中航特玻科技有限公司 | Honeycombed catalyst for low-temperature denitration and preparation method |
CN105688974B (en) * | 2016-01-11 | 2019-03-19 | 大唐南京环保科技有限责任公司 | One kind is with SBA-15/TiO2For the denitrating catalyst and preparation method thereof of carrier |
CN108671750A (en) * | 2018-06-04 | 2018-10-19 | 常州宝电节能环保科技有限公司 | A kind of preparation method of width temperature operating window dedusting denitration double functional ceramics column |
CN109046324B (en) * | 2018-06-22 | 2021-07-20 | 清华大学盐城环境工程技术研发中心 | Medium-low temperature denitration catalyst with mesoporous cerium oxide as carrier and preparation method thereof |
CN111659367A (en) * | 2020-06-16 | 2020-09-15 | 福建龙净环保股份有限公司 | Nano-grade anatase titanium dioxide dispersion liquid, SCR denitration catalyst suspension liquid, preparation method of SCR denitration catalyst suspension liquid and catalytic ceramic filter cylinder |
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