CN102614866A - Honeycomb SCR smoke denitration catalyst embryoid body and preparation method thereof - Google Patents
Honeycomb SCR smoke denitration catalyst embryoid body and preparation method thereof Download PDFInfo
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- CN102614866A CN102614866A CN2012100519936A CN201210051993A CN102614866A CN 102614866 A CN102614866 A CN 102614866A CN 2012100519936 A CN2012100519936 A CN 2012100519936A CN 201210051993 A CN201210051993 A CN 201210051993A CN 102614866 A CN102614866 A CN 102614866A
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Abstract
The invention discloses a honeycomb SCR (Selective Catalytive Redution) smoke denitration catalyst embryoid body and a preparation method thereof. The honeycomb SCR smoke denitration catalyst body consists of the following raw materials as per percentage by weight: 40 to 60 percent of titanium dioxide, 1 to 10 percent of white clay, 0.1 to 1 percent of ammonium metavanadate, 1 to 8 percent of ammonium meta-tungstate, 0.1 to 3 percent of niobium oxalate, 0.5 to 3 percent of lactic acid aqueous solution, 1 to 5 percent of oxalic acid aqueous solution, 25 to 35 percent of deionized water, 1 to 10 percent of ceramic fiber, 0.1 to 3 percent of fluff pulp, 0.1 to 1 percent of stearic acid, 0.1 to 1 percent of hydroxypropyl methyl cellulose and 1 to 5 percent of glycerol. The honeycomb SCR smoke denitration catalyst embryoid body has high plasticity, caking property and mechanical strength. The method is simple and convenient in operation and low in cost. Each component of the prepared catalyst body is dispersed uniformly; the catalyst body is easy in forming and demolding in the extrusion process and has high finished product rate; and the catalyst prepared by the embryoid body has high denitration efficiency.
Description
Technical field
The present invention relates to technical field of waste gas treatment, be specifically related to a kind of honeycomb-shaped SCR catalyst for denitrating flue gas idiosome and preparation method thereof.
Background technology
Along with " thermal power plant's atmosphere pollutants emission standards " promulgation (GB13223-2011), it is strict that the discharge standard of nitrogen oxide more becomes.SCR (SCR) has denitration efficiency efficiently, and the discharging of ability better controlled thermal power plant nitrogen oxide is a method of controlling nitrogen oxide at present the most efficiently, also will become the mainstream technology of denitrating flue gas gradually.Catalyst is the core of SCR technology, because SCR technology is arranged in the high ash section between economizer and the air preheater mostly, catalyst is in the flue gas of high dust; If adopt granular catalyst can cause the obstruction of bed, resistance increases, and makes pressure drop increase; Reaction continous-stable operation for a long time, so commercial catalysts adopts integral catalyzer usually, like honeycombed catalyst; Its ceramic honey comb percent opening is big, and surface area is big, and catalyst volume is little; Help passing through smoothly of dust, have and advantage such as be difficult for to stop up, wear-resistant, easy to loading and unloading.
The ceramic honeycomb catalyst idiosome has decisive action to the activity of ceramic honeycomb catalyst, thereby ceramic honeycomb catalyst idiosome and preparation thereof are one of keys of ceramic honeycomb catalyst.But shortcomings such as it is inhomogeneous that the ceramic honeycomb catalyst idiosome that existing denitrating flue gas is used exists component to mix, and intensity is low, it is not high to be difficult for the demoulding, yield rate during extrusion molding in its preparation process.Therefore, develop a kind of low cost, high performance ceramic honeycomb catalyst idiosome has a good application prospect.
Granted publication number discloses a kind of aluminium titanates-mullite ceramic honey comb and preparation method thereof for the Chinese patent of CN101074161B; Earlier aluminium titanates and mullite are compounded to form composite diphase material according to performance requirement; The mould that adds the compound plasticized modifier of configuration and design voluntarily again; Obtain idiosome through mixing, pugging, after extruding, carry out obtaining cellular structure after drying, the roasting again, this preparation method's operation is complicated; Narrow application range, the honeycomb molded body that obtains can't satisfy the performance requirement of the required catalyst in present denitrating flue gas field.
Granted publication is number for the Chinese patent of CN101502796B discloses integral honeycomb selective catalytic reduction catalyst for flue gas denitration and preparation method, and catalyst is carrier and skeleton with the nano titanium oxide, and the denitration activity component is evenly distributed in the skeleton; And the bond of adding proper proportion; Its percentage by weight is: nano titanium oxide 60～85%, and active component 4～25%, bond is 5～20%; This catalyst is applicable to the improvement of large-sized station boiler tail gas, but denitration efficiency is lower.
Summary of the invention
The invention provides a kind of honeycomb-shaped SCR catalyst for denitrating flue gas idiosome, plasticity is excellent, and caking property is strong, and mechanical strength is high.
A kind of honeycomb-shaped SCR catalyst for denitrating flue gas idiosome, the mass percent of its raw material consists of:
The mass percent concentration of described oxalic acid aqueous solution is 40～60%; The mass percent concentration of described lactic acid aqueous solution is 50～60%.
Described ceramic fibre, Time of Fluff Slurry are commercially available finished product, and ceramic fibre is a kind of fibrous light refractory material, the F-1260 type ceramic fibre that can select for use Deqing, the Zhejiang refined crystal fibre of indigo plant Co., Ltd to produce; Described Time of Fluff Slurry is through bleaching, extracts wood pulp, straw pulp after the operation such as organic solvent out, the optional Time of Fluff Slurry of using from the prosperous civilian fibrous material in Daye City, Hubei processing factory, and its width is 20～25 μ m, length is 0.5～1mm.
The present invention also provides a kind of preparation method of honeycomb-shaped SCR catalyst for denitrating flue gas idiosome, may further comprise the steps:
(1) get the raw materials ready by following mass percent:
The mass percent concentration of described oxalic acid aqueous solution is 40～60%; The mass percent concentration of described lactic acid aqueous solution is 50～60%.
(2) ammonium metavanadate, ammonium metatungstate, niobium oxalate are mixed with oxalic acid aqueous solution, obtain mixed solution;
(3) mixed solution that obtains in titanium white powder, white clay, lactic acid aqueous solution, stearic acid, deionized water, the step (2) is carried out once mixing, once mixing end adds ceramic fibre, Time of Fluff Slurry, hydroxypropyl methylcellulose, glycerine, deionized water again and carries out the mixing mud embryo that obtains of secondary;
(3) successively the mud embryo is carried out old processing, filtering and impurity removing, extrusion molding and obtain honeycomb-shaped SCR catalyst for denitrating flue gas idiosome.
Described temperature once mixing, that secondary is mixing is 75 ℃～85 ℃, and the once mixing time is 30～60min, and the mixing time of secondary is 10～20min, and each component is uniformly dispersed, and helps the extrusion molding of postorder.
Described old temperature is 15 ℃～25 ℃, and the old time is 6～12h, and each component is uniformly dispersed, and to improve the plasticity of idiosome, helps the extrusion molding of postorder.
The filter screen order number that adopts in the described filtering and impurity removing is 14～20 orders.
What described extrusion molding was adopted is vacuum-extruder, the negative pressure of described vacuum-extruder is-and 0.085MPa～-0.095MPa.
In the preparation process of honeycomb-shaped SCR catalyst for denitrating flue gas idiosome of the present invention, for obtaining good extrusion molding effect, be beneficial to the shaping and demoulding of catalyst idiosome, can before carrying out extrusion molding, extrude processing in advance as required to the mud embryo.
The present invention compared with prior art has following advantage:
Catalyst idiosome of the present invention has good plasticity, strong cohesive property, high mechanical properties; Catalyst idiosome preparation method of the present invention is easy and simple to handle, cost is low, and each component is uniformly dispersed in the catalyst idiosome for preparing, the easy shaping and demoulding of extrusion, and yield rate is high; The catalyst denitration efficiency that is made by catalyst idiosome of the present invention is high.
Description of drawings
Fig. 1 is the process flow diagram of honeycomb-shaped SCR catalyst for denitrating flue gas idiosome preparation of the present invention.
The specific embodiment
The preparation of embodiment 1 honeycomb-shaped SCR catalyst for denitrating flue gas idiosome
With ammonium metavanadate 10g, ammonium metatungstate 20g, niobium oxalate 25g and 20ml mass percent concentration is that 60% oxalic acid aqueous solution stirs under 50 ℃ of temperature, mixes, and obtains mixed solution;
With titanium white powder 412g, white clay 80g, mass percent concentration is that 50% lactic acid aqueous solution 10ml, stearic acid 3g, deionized water 275ml, above-mentioned mixed solution are put into mixer and under 80 ℃, carried out once mixing; Add ceramic fibre 80g (F-1260 type ceramic fibre behind the mixing 42min again; Deqing, Zhejiang blue refined crystal fibre Co., Ltd), Time of Fluff Slurry 3g (Daye City, Hubei prosperous civilian fibrous material processing factory), hydroxypropyl methylcellulose 2g, glycerine 20ml, that deionized water 40ml carries out secondary is mixing, obtains the mud embryo behind the mixing 15min;
The mud embryo is encased with plastic foil, be placed on shady and cool moist place (temperature is about 23 ℃) and carry out old processing, old time 12h;
It is that 16 purpose filters filter removal impurity that idiosome after old is put into filter screen order number, puts into preparatory extruder again and is extruded into block idiosome;
Block idiosome is put into vacuum-extruder, and extrusion molding obtains honeycomb-shaped SCR catalyst for denitrating flue gas idiosome, wherein the vacuum chamber negative pressure remain-0.085MPa～-0.095MPa.
The preparation of embodiment 2 honeycomb-shaped SCR catalyst for denitrating flue gas idiosomes
With ammonium metavanadate 2g, ammonium metatungstate 40g, niobium oxalate 5g and 35ml mass percent concentration is that 60% oxalic acid aqueous solution stirs under 50 ℃ of temperature, mixes, and obtains mixed solution;
With titanium white powder 590g, white clay 11g, mass percent concentration is that 50% lactic acid aqueous solution 15ml, stearic acid 8g, deionized water 210ml, mixed solution are put into mixer and under 80 ℃, carried out once mixing; Add ceramic fibre 30g, Time of Fluff Slurry 20g, hydroxypropyl methylcellulose 10g, glycerine 25ml behind the mixing 60min again, that deionized water 50ml carries out secondary is mixing, obtains the mud embryo behind the mixing 10min;
The mud embryo is encased with plastic foil, be placed on shady and cool moist place (temperature is about 15 ℃) and carry out old processing, old time 6h;
It is that 20 purpose filters filter removal impurity that idiosome after old is put into filter screen order number, puts into preparatory extruder again and is extruded into block idiosome;
Block idiosome is put into vacuum-extruder, and extrusion molding obtains honeycomb-shaped SCR catalyst for denitrating flue gas idiosome, wherein the vacuum chamber negative pressure remain-0.085MPa～-0.095MPa.
The preparation of embodiment 3 honeycomb-shaped SCR catalyst for denitrating flue gas idiosomes
With ammonium metavanadate 5g, ammonium metatungstate 20g, niobium oxalate 3g and 30ml mass percent concentration is that 60% oxalic acid aqueous solution stirs under 50 ℃ of temperature, mixes, and obtains mixed solution;
With titanium white powder 525g, white clay 30g, mass percent concentration is that 50% lactic acid aqueous solution 12ml, stearic acid 10g, deionized water 230ml, mixed solution are put into mixer and under 80 ℃, carried out once mixing; Add ceramic fibre 50g, Time of Fluff Slurry 10g, hydroxypropyl methylcellulose 5g, glycerine 20ml behind the mixing 55min again, that deionized water 50ml carries out secondary is mixing, obtains the mud embryo behind the mixing 15min;
The mud embryo is encased with plastic foil, be placed on shady and cool moist place (temperature is about 20 ℃) and carry out old processing, the old time is 8h;
It is that 18 purpose filters filter removal impurity that idiosome after old is put into filter screen order number, puts into preparatory extruder again and is extruded into block idiosome;
Block idiosome is put into vacuum-extruder, and extrusion molding obtains honeycomb-shaped SCR catalyst for denitrating flue gas idiosome, wherein the vacuum chamber negative pressure remain-0.085MPa～-0.095MPa.
The preparation of embodiment 4 honeycomb-shaped SCR catalyst for denitrating flue gas idiosomes
With ammonium metavanadate 8g, ammonium metatungstate 15g, niobium oxalate 15g and 50ml mass percent concentration is that 60% oxalic acid aqueous solution stirs under 50 ℃ of temperature, mixes, and obtains mixed solution;
With titanium white powder 455g, white clay 60g, mass percentage concentration is that 50% lactic acid aqueous solution 12ml, stearic acid 5g, deionized water 230ml, above-mentioned mixed solution are put into mixer and under 80 ℃, carried out once mixing; Add ceramic fibre 60g, Time of Fluff Slurry 15g, hydroxypropyl methylcellulose 5g, glycerine 20ml behind the mixing 30min again, that deionized water 50ml carries out secondary is mixing, obtains the mud embryo behind the mixing 20min;
The mud embryo is encased with plastic foil, be placed on shady and cool moist place (temperature is about 23 ℃) and carry out old processing, old time 6h;
It is that 20 purpose filters filter removal impurity that idiosome after old is put into filter screen order number, puts into preparatory extruder again and is extruded into block idiosome;
Block idiosome is put into vacuum-extruder, and extrusion molding obtains honeycomb-shaped SCR catalyst for denitrating flue gas idiosome, wherein the vacuum chamber negative pressure remain-0.085MPa～-0.095MPa.
Embodiment 5 honeycomb-shaped SCR catalyst for denitrating flue gas mechanical strengths and specific area test
The honeycomb-shaped SCR catalyst for denitrating flue gas idiosome that obtains in the embodiment of the invention 1 in 20～50 ℃ of dryings 7 days, behind 600 ℃ of roasting 5h, is obtained honeycomb-shaped SCR catalyst for denitrating flue gas coupon.Coupon is cut into the square coupon, put into universal testing machine and test, obtaining the vertical compression strength of honeycomb-shaped SCR catalyst for denitrating flue gas is 360N/cm
2, under the equal conditions, the vertical compression strength that records existing certain commercially available honeycomb denitrating catalyst is 310N/cm
2With square coupon crushing screening; Obtaining particle diameter is the catalyst granules between 40 order to 60 orders; Get the part particle and put into the Autosorb-1-c instrument that U.S. Kang Ta company produces and carry out the specific area test, recording honeycomb-shaped SCR catalyst for denitrating flue gas specific area is 71.6m
2/ g, under the equal conditions, the specific area that records existing certain commercially available honeycomb denitrating catalyst is 62m
2/ g.
Embodiment 6 honeycomb-shaped SCR catalyst for denitrating flue gas mechanical strengths and specific area test
The honeycomb-shaped SCR catalyst for denitrating flue gas idiosome for preparing in the embodiment of the invention 2 in 20～50 ℃ of dryings 7 days, behind 600 ℃ of roasting 5h, is obtained honeycomb-shaped SCR catalyst for denitrating flue gas coupon.Coupon is cut into the square coupon, put into universal testing machine and test, obtaining the vertical compression strength of honeycomb-shaped SCR catalyst for denitrating flue gas is 325N/cm
2With square coupon crushing screening; Obtaining particle diameter is the catalyst granules between 40 order to 60 orders; Get the part particle and put into the Autosorb-1-c instrument that U.S. Kang Ta company produces and carry out the specific area test, recording honeycomb-shaped SCR catalyst for denitrating flue gas specific area is 65.6m
2/ g.
Embodiment 7 honeycomb-shaped SCR catalyst for denitrating flue gas mechanical strengths and specific area test
The honeycomb-shaped SCR catalyst for denitrating flue gas idiosome for preparing in the embodiment of the invention 3 in 20～50 ℃ of dryings 7 days, behind 600 ℃ of roasting 5h, is obtained honeycomb-shaped SCR catalyst for denitrating flue gas coupon.Coupon is cut into the square coupon, put into universal testing machine and test, obtaining the vertical compression strength of honeycomb-shaped SCR catalyst for denitrating flue gas is 335N/cm
2With square coupon crushing screening; Obtaining particle diameter is the catalyst granules between 40 order to 60 orders; Get the part particle and put into the Autosorb-1-c instrument that U.S. Kang Ta company produces and carry out the specific area test, recording honeycomb-shaped SCR catalyst for denitrating flue gas specific area is 67.6m
2/ g.
Embodiment 8 honeycomb-shaped SCR catalyst for denitrating flue gas mechanical strengths and specific area test
The honeycomb-shaped SCR catalyst for denitrating flue gas idiosome for preparing in the embodiment of the invention 4 in 20～50 ℃ of dryings 7 days, behind 600 ℃ of roasting 5h, is obtained honeycomb-shaped SCR catalyst for denitrating flue gas coupon.Coupon is cut into the square coupon, put into universal testing machine and test, obtaining the vertical compression strength of honeycomb-shaped SCR catalyst for denitrating flue gas is 340N/cm
2With square coupon crushing screening; Obtaining particle diameter is the catalyst granules between 40 order to 60 orders; Get the part particle and put into the Autosorb-1-c instrument that U.S. Kang Ta company produces and carry out the specific area test, recording honeycomb-shaped SCR catalyst for denitrating flue gas specific area is 69.1m
2/ g.
Embodiment 9 honeycomb-shaped SCR catalyst for denitrating flue gas activity ratings
The honeycomb-shaped SCR catalyst for denitrating flue gas idiosome for preparing in the embodiment of the invention 1 in 20～50 ℃ of dryings 7 days, behind 600 ℃ of roasting 5h, is obtained honeycomb-shaped SCR catalyst for denitrating flue gas coupon.Honeycomb-shaped SCR catalyst for denitrating flue gas coupon is cut into 50mm * 50mm * 300mm coupon, this coupon is put into homemade catalyst activity evaluating apparatus carry out active testing, smoke components is 300ppm NO, 300ppm NH
3, 500ppm SO
2, 10vol%H
2O, 5vol%O
2, all the other are N
2Area speed is 20m/h, and reaction temperature is 360 ℃, and after stablizing, recording the catalyst denitration efficiency is 97.2%.
Embodiment 10 honeycomb-shaped SCR catalyst for denitrating flue gas activity ratings
The honeycomb-shaped SCR catalyst for denitrating flue gas idiosome for preparing in the embodiment of the invention 4 in 20～50 ℃ of dryings 7 days, behind 600 ℃ of roasting 5h, is obtained honeycomb-shaped SCR catalyst for denitrating flue gas coupon.Honeycomb-shaped SCR catalyst for denitrating flue gas coupon is cut into 50mm * 50mm * 300mm coupon, this coupon is put into homemade catalyst activity evaluating apparatus carry out active testing, smoke components is 300ppm NO, 300ppm NH
3, 500ppm SO
2, 10vol%H
2O, 5vol%O
2, all the other are N
2Area speed is 20m/h, and reaction temperature is 320 ℃, and after stablizing, recording the catalyst denitration efficiency is 92.9%.
Claims (8)
1. honeycomb-shaped SCR catalyst for denitrating flue gas idiosome is characterized in that the mass percent of its raw material consists of:
2. honeycomb-shaped SCR catalyst for denitrating flue gas idiosome as claimed in claim 1 is characterized in that the mass percent concentration of described oxalic acid aqueous solution is 40～60%.
3. honeycomb-shaped SCR catalyst for denitrating flue gas idiosome as claimed in claim 1 is characterized in that the mass percent concentration of described lactic acid aqueous solution is 50～60%.
4. the preparation method of a honeycomb-shaped SCR catalyst for denitrating flue gas idiosome is characterized in that, may further comprise the steps:
(1) get the raw materials ready by following mass percent:
The mass percent concentration of described oxalic acid aqueous solution is 40～60%; The mass percent concentration of described lactic acid aqueous solution is 50～60%;
(2) ammonium metavanadate, ammonium metatungstate, niobium oxalate are mixed with oxalic acid aqueous solution, obtain mixed solution;
(3) mixed solution that obtains in titanium white powder, white clay, lactic acid aqueous solution, stearic acid, deionized water and the step (2) is carried out once mixing, add ceramic fibre, Time of Fluff Slurry, hydroxypropyl methylcellulose, glycerine, deionized water after the mixing end again and carry out the mixing mud embryo that obtains of secondary;
(4) successively the mud embryo is carried out old processing, filtering and impurity removing, extrusion modling and obtain honeycomb-shaped SCR catalyst for denitrating flue gas idiosome.
5. the preparation method of honeycomb-shaped SCR catalyst for denitrating flue gas idiosome as claimed in claim 4; It is characterized in that; Described temperature once mixing, that secondary is mixing is 75 ℃～85 ℃, and the once mixing time is 30～60min, and the mixing time of secondary is 10～20min.
6. the preparation method of honeycomb-shaped SCR catalyst for denitrating flue gas idiosome as claimed in claim 4 is characterized in that, described old temperature is 15 ℃～25 ℃, and the old time is 6～12h.
7. the preparation method of honeycomb-shaped SCR catalyst for denitrating flue gas idiosome as claimed in claim 4 is characterized in that, the filter screen order number that adopts in the described filtering and impurity removing is 14～20 orders.
8. the preparation method of honeycomb-shaped SCR catalyst for denitrating flue gas idiosome as claimed in claim 4 is characterized in that, what described extrusion molding was adopted is vacuum-extruder, the negative pressure of described vacuum-extruder is-and 0.085MPa～-0.095MPa.
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| CN103586016A (en) * | 2013-11-14 | 2014-02-19 | 索平 | Honeycomb type selective catalytic reduction denitration catalyst and preparation method thereof |
| CN103623806A (en) * | 2013-09-24 | 2014-03-12 | 无锡华光新动力环保科技股份有限公司 | SCR (Selective Catalytic Reduction) honeycombed denitration catalyst production technology |
| CN103878032A (en) * | 2014-03-25 | 2014-06-25 | 浙江海亮环境材料有限公司 | SCR denitration catalyst with clay |
| CN104307508A (en) * | 2014-10-17 | 2015-01-28 | 辽宁科隆精细化工股份有限公司 | Preparation method of SCR denitration catalyst capable of being rapidly dried |
| CN105148904A (en) * | 2015-08-28 | 2015-12-16 | 武汉京运通环保工程有限公司 | Flue gas denitration catalyst applied at a low temperature and preparation method thereof |
| CN105964239A (en) * | 2016-05-23 | 2016-09-28 | 石河子大学 | Method for preparing spherical denitration catalyst |
| CN107321176A (en) * | 2017-06-27 | 2017-11-07 | 中国第汽车股份有限公司 | A kind of preparation method of the compound monoblock type SCR catalytic reactors of inorganic oxide |
| CN113509924A (en) * | 2021-05-22 | 2021-10-19 | 山东博霖环保科技发展有限公司 | Denitration catalyst and production process thereof |
| CN113600179A (en) * | 2021-09-16 | 2021-11-05 | 山东博霖环保科技发展有限公司 | Denitration catalyst and preparation method thereof |
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| CN105964239A (en) * | 2016-05-23 | 2016-09-28 | 石河子大学 | Method for preparing spherical denitration catalyst |
| CN105964239B (en) * | 2016-05-23 | 2018-09-11 | 石河子大学 | The preparation method of spherical denitrating catalyst |
| CN107321176A (en) * | 2017-06-27 | 2017-11-07 | 中国第汽车股份有限公司 | A kind of preparation method of the compound monoblock type SCR catalytic reactors of inorganic oxide |
| CN113509924A (en) * | 2021-05-22 | 2021-10-19 | 山东博霖环保科技发展有限公司 | Denitration catalyst and production process thereof |
| CN113600179A (en) * | 2021-09-16 | 2021-11-05 | 山东博霖环保科技发展有限公司 | Denitration catalyst and preparation method thereof |
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