CN108057437A - Active ingredient passes through SCR catalyst of 3D printing straight forming and preparation method thereof - Google Patents
Active ingredient passes through SCR catalyst of 3D printing straight forming and preparation method thereof Download PDFInfo
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- CN108057437A CN108057437A CN201711210597.2A CN201711210597A CN108057437A CN 108057437 A CN108057437 A CN 108057437A CN 201711210597 A CN201711210597 A CN 201711210597A CN 108057437 A CN108057437 A CN 108057437A
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- 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
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
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- 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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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/2073—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The present invention relates to catalyst more particularly to a kind of active ingredient to pass through SCR catalyst of 3D printing straight forming and preparation method thereof.Include the raw material of following mass parts：100 parts of graphite oxide；20~50 parts of manganese salt；200~400 parts of reactive oligomers；30~100 parts of reactive diluent；5~10 parts of photoinitiator.The present invention has low-temperature SCR active window using graphene manganese oxide composite material as the active ingredient of catalyst, reduces absorption of the water in catalyst surface, reduces sulfate in the deposition of catalyst surface, improves the ability that its water resistant sulfur resistive poisons；Using the method for a step 3D printing, by the active ingredient straight forming of catalyst, compared with traditional honeycomb-shaped SCR catalyst, specific surface area with bigger, the pore passage structure being more suitable for so as to effectively reduce flue gas resistance, reduce pressure drop, improves the service life of catalyst；The present invention effectively improves the load capacity of catalyst, been significantly enhanced the denitration efficiency of catalyst without ceramic monolith.
Description
Technical field
The present invention relates to catalyst more particularly to a kind of active ingredient by the SCR catalyst of 3D printing straight forming and
Its preparation method.
Background technology
China is in the world using the most country of Coal Energy Source, and the serious pollution environment of utilization of coal simultaneously endangers people
The health of class.Since the burning of coal can largely give off sulfur dioxide (SO2) and nitrogen oxides (NOx), so as to cause acid rain,
The a series of environmental problems such as photochemical fog, secondary aerosol species pollution.More than 90% NO according to statisticsxDischarge comes from electricity
The exhaust gas generated in factory, cement plant, steel mill using the burning of fossil fuel.Country is for NO in recent yearsxDischarge carried out sternly
The limitation of lattice, and formulated relevant regulation.Therefore to the NO of dischargexIt is handled very necessary.
Selective catalytic reduction (SCR) method is to handle NO so farxMaximally efficient means.So far, business
The SCR catalyst for changing application is V2O5-WO3-TiO2System, active temperature windows are at 400 DEG C or so.But SCR denitration system
It is arranged in after Industrial Stoves, exhaust temperature usually only has 250 DEG C or so.If by flue gas heat up if can greatly increase operation into
This.In addition, the flying dust in flue gas is accumulated and causes catalyst blockage on the surface of catalyst；Vapor and SO2It can make in catalyst
Poison causes catalyst inactivation.Chinese invention patent CN201610545189.1 discloses low temperature manganese base SCR denitration, low
Warm denitration performance is preferable, however its water resistant, sulfur poisoning ability are not evaluated.Chinese invention patent
CN201611069102.4 discloses a kind of low temperature vanadium-tungsten-titanium denitrating catalyst, has preferable low temperature active, however vanadium is simultaneously
It is not a kind of environmentally friendly material, it is also necessary to a series of problems, such as considering catalyst inactivation post processing.
Traditional cellular SCR catalyst is generally using ceramic material, such as cordierite, mullite, TiO2Wait materials
As carrier, certain pore passage structure is obtained by being machined, then will by coprecipitation, infusion process, sol-gel method etc.
Catalyst activity component loads thereon.But its gas-flow resistance is larger, geometric proportion finite surface area damages in practical application in industry
Consumption is higher；Regeneration and recycling after also failing simultaneously to catalyst active component cause difficulty.
The content of the invention
To overcome above-mentioned the deficiencies in the prior art, the present invention provides a kind of active ingredients to pass through 3D printing straight forming
SCR catalyst and preparation method thereof.There is the present invention low-temperature SCR active window, higher sulfur resistive water resistant to poison ability；The present invention
Production cost is low, environmental-friendly.
In order to achieve the above object, the present invention is realized using following technical scheme：
A kind of active ingredient includes the raw material of following mass parts by the SCR catalyst of 3D printing straight forming：
The manganese salt is one or more of manganese acetate, manganese chloride, manganese sulfate, manganese nitrate.
The reactive oligomers are unsaturated polyester (UP), acrylic resin, polyester acrylate, poly-methyl methacrylate
One or more of ester, polyether acrylate, epoxy acrylate, polyurethane acrylate.
The reactive diluent is senecioate-hydroxyl ethyl ester, diallyphthalate acid esters, triethylene-glycol dipropyl
One or several kinds in olefin(e) acid ester, isobomyl acrylate fat.
The photoinitiator be a, a '-dimethyl benzil ketals, a, a '-diethoxy acetophenone, 2- methyl-1s (4 first
Sulfenyl) phenyl -2- morpholine -1- acetone, 2,4,6- tri-methyl benzophenones, isopropyl thioxanthone, Omnicat550,
One or more of Omnicat650.
A kind of active ingredient is specifically comprised the following steps by the preparation method of the SCR catalyst of 3D printing straight forming：
(1) will graphite oxide be prepared using Hummer ' s methods, and will take graphite oxide, 20~50 mass parts of 100 mass parts
Four acetate hydrate manganese, 200~400 mass parts polymethyl methacrylates be placed in ball mill with 400~800r/min turn
Scattered 2~the 6h of speed, is made dispersion liquid；
(2) the diallyphthalate acid fat of 30~100 mass parts and the Omnicat650 of 5~10 mass parts are weighed,
It adds it in above-mentioned dispersion liquid, 1~2h of mechanical agitation, 1~2h of sonic oscillation；
(3) honeycombed catalyst model is established by computer software AutoCAD, by model be arranged to the length of side for 100~
300mm is highly 100~300mm, and inside is the hexahedron knot of 0.5~2mm diametric holes, and threedimensional model is resolved into thickness
For 30~100 μm of section, and input in SLA 3D printers；
(4) it is 0.1~0.3m/s to set printer operating speed, and print resolution is 70~100 μm, and powder sending quantity is
0.2mm2/S；The intensity, angle, shape of printer light beam are regulated and controled, the slurry is successively printed and photocuring, is obtained
To honeycombed catalyst idiosome；
(5) by idiosome under protection of argon gas, 500~700 DEG C of 2~4h of calcining, remove the wherein impurity such as organic matter, and urging
Agent is activated.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) using graphene-manganese oxide composite material as the active ingredient of catalyst, there is low-temperature SCR active window；
(2) graphene can effectively reduce absorption of the water in catalyst surface as a kind of hydrophobic material, while
Deposition of the sulfate in catalyst surface can be reduced, improves the ability that its water resistant sulfur resistive poisons；
(3) method for using a step 3D printing, by the active ingredient straight forming of catalyst, with traditional honeycomb-shaped SCR
Catalyst is compared, and has the specific surface area of bigger, the pore passage structure being more suitable for, so as to effectively reduce flue gas resistance, subtract
Small pressure drop further improves the service life of catalyst；
(4) load capacity of catalyst is effectively improved, makes the de- of catalyst without ceramic monolith in catalyst of the present invention
Nitre efficiency is been significantly enhanced.
Description of the drawings
The water resistant sulfur resistive that Fig. 1 is the present invention poisons analysis of experimental results figure.
Specific embodiment
Following instance is for the more detailed description present invention, but the present invention is not limited thereto.Join for the technique being not specified
Number can refer to routine techniques progress.
Embodiment 1
A kind of active ingredient includes the raw material of following mass parts by the SCR catalyst of 3D printing straight forming：
A kind of active ingredient is specifically comprised the following steps by the preparation method of the SCR catalyst of 3D printing straight forming：
(1) 100 mass parts of graphite oxide that Hummer ' s methods will be used to prepare, four acetate hydrate manganese, 20 mass parts and polymethyl
Sour 200 mass parts of methyl esters are placed in ball mill with the rotating speed of 800r/min, disperse 2h；
(2) 30 mass parts diallyphthalate acid fat are weighed, 5 mass parts Omnicat650 are added to above-mentioned dispersion liquid
In, mechanical agitation 1h, sonic oscillation 1h；
(3) honeycombed catalyst model is established by computer software AutoCAD, model is arranged to the length of side as 200mm,
It is highly 200mm, inside is the hexahedron knot of 0.5mm diametric holes, and threedimensional model is resolved into the section that thickness is 30 μm, and
It inputs in SLA 3D printers；
(4) it is 0.2m/s to set printer operating speed, and print resolution is 70~100 μm, powder sending quantity 0.2mm2/S；
The intensity, angle, shape of printer light beam are regulated and controled, the slurry is successively printed and photocuring, is obtained cellular
Catalyst idiosome
(5) by idiosome under protection of argon gas, 500 DEG C of calcining 2h, remove the wherein impurity such as organic matter, and catalyst is carried out
Activation.
Embodiment 2
A kind of active ingredient includes the raw material of following mass parts by the SCR catalyst of 3D printing straight forming：
A kind of active ingredient is specifically comprised the following steps by the preparation method of the SCR catalyst of 3D printing straight forming：
(1) 100 mass parts of graphite oxide that Hummer ' s methods will be used to prepare, four acetate hydrate manganese, 30 mass parts and polymethyl
Sour 200 mass parts of methyl esters are placed in ball mill with the rotating speed of 400r/min, disperse 2h；
(2) 50 mass parts diallyphthalate acid fat are weighed, 7 mass parts Omnicat650 are added to above-mentioned dispersion liquid
In, mechanical agitation 1h, ultrasonic 1h；
(3) honeycombed catalyst model is established by computer software AutoCAD, model is arranged to the length of side as 100mm,
It is highly 100mm, inside is the hexahedron knot of 1mm diametric holes, and threedimensional model is resolved into the section that thickness is 50 μm, and defeated
Enter in SLA 3D printers；
(4) it is 0.1m/s to set printer operating speed, and print resolution is 70 μm, powder sending quantity 0.2mm2/S；Air exercise
Intensity, angle, the shape of print machine light beam are regulated and controled, and the slurry is successively printed and photocuring, obtains honeycomb catalyst
Agent idiosome
(5) by idiosome under protection of argon gas, 600 DEG C of calcining 2h, remove the wherein impurity such as organic matter, and catalyst is carried out
Activation
Embodiment 3
A kind of active ingredient includes the raw material of following mass parts by the SCR catalyst of 3D printing straight forming：
A kind of active ingredient is specifically comprised the following steps by the preparation method of the SCR catalyst of 3D printing straight forming：
(1) 100 mass parts of graphite oxide that Hummer ' s methods will be used to prepare, four acetate hydrate manganese, 40 mass parts and polymethyl
Sour 300 mass parts of methyl esters are placed in ball mill with the rotating speed of 800r/min, disperse 2h；
(2) 70 mass parts diallyphthalate acid fat are weighed, 8 mass parts Omnicat650 are added to above-mentioned dispersion liquid
In, mechanical agitation 1h, sonic oscillation 1h；
(3) honeycombed catalyst model is established by computer software AutoCAD, model is arranged to the length of side as 150mm,
It is highly 150mm, inside is the hexahedron knot of 1.5mm diametric holes, and threedimensional model is resolved into the section that thickness is 50 μm, and
It inputs in SLA 3D printers；
(4) it is 0.2m/s to set printer operating speed, and print resolution is 70 μm, powder sending quantity 0.2mm2/S；Air exercise
Intensity, angle, the shape of print machine light beam are regulated and controled, and the slurry is successively printed and photocuring, obtains honeycomb catalyst
Agent idiosome
(5) by idiosome under protection of argon gas, 600 DEG C of calcining 2h, remove the wherein impurity such as organic matter, and catalyst is carried out
Activation
Embodiment 4
A kind of active ingredient includes the raw material of following mass parts by the SCR catalyst of 3D printing straight forming：
A kind of active ingredient is specifically comprised the following steps by the preparation method of the SCR catalyst of 3D printing straight forming：
(1) 100 mass parts of graphite oxide that Hummer ' s methods will be used to prepare, four acetate hydrate manganese, 40 mass parts and polymethyl
Sour 400 mass parts of methyl esters are placed in ball mill with the rotating speed of 800r/min, disperse 6h；
(2) 80 mass parts diallyphthalate acid fat are claimed, 10 mass parts Omnicat650 are added to above-mentioned dispersion liquid
In, mechanical agitation 2h, sonic oscillation 2h；
(3) honeycombed catalyst model is established by computer software AutoCAD, model is arranged to the length of side as 250mm,
It is highly 250mm, inside is the hexahedron knot of 2mm diametric holes, and threedimensional model is resolved into the section that thickness is 100 μm, and
It inputs in SLA 3D printers；
(4) it is 0.3m/s to set printer operating speed, and print resolution is 100 μm, powder sending quantity 0.2mm2/S；Air exercise
The intensity of print machine light beam, angle, shape are regulated and controled, and the slurry is successively printed and photocuring, obtains honeycomb catalyst
Agent idiosome
(5) by idiosome under protection of argon gas, 700 DEG C of calcining 4h, remove the wherein impurity such as organic matter, and catalyst is carried out
Activation
Embodiment 5
A kind of active ingredient includes the raw material of following mass parts by the SCR catalyst of 3D printing straight forming：
A kind of active ingredient is specifically comprised the following steps by the preparation method of the SCR catalyst of 3D printing straight forming：
(1) 100 mass parts of graphite oxide that Hummer ' s methods will be used to prepare, four acetate hydrate manganese, 50 mass parts and polymethyl
Sour 400 mass parts of methyl esters are placed in ball mill with the rotating speed of 800r/min, disperse 6h；
(2) 100 mass parts diallyphthalate acid fat are weighed, 10 mass parts Omnicat650 are added to above-mentioned scattered
In liquid, mechanical agitation 2h, sonic oscillation 2h；
(3) honeycombed catalyst model is established by computer software AutoCAD, model is arranged to the length of side as 300mm,
It is highly 300mm, inside is the hexahedron knot of 2mm diametric holes, and threedimensional model is resolved into the section that thickness is 100 μm, and
It inputs in SLA 3D printers；
(4) it is 0.3m/s to set printer operating speed, and print resolution is 100 μm, powder sending quantity 0.2mm2/S；Air exercise
The intensity of print machine light beam, angle, shape are regulated and controled, and the slurry is successively printed and photocuring, obtains honeycomb catalyst
Agent idiosome
(5) by idiosome under protection of argon gas, 700 DEG C of calcining 4h, remove the wherein impurity such as organic matter, and catalyst is carried out
Activation
Catalyst prepared by Examples 1 to 5 is reacted for low-temperature selective catalytic reduction denitration, reaction condition and work
Property is as shown in table 1.
The catalyst denitration activity at different temperatures of 1 Examples 1 to 5 of table
Catalyst performance evaluation：Catalyst prepared by Examples 1 to 5, which is placed in quartz ampoule fixed bed reactors, carries out activity
Evaluation.Flue gas uses laboratory simulation flue gas condition, NH3It is for also Primordial Qi, test condition：NO1000ppm, NH31000ppm,
5%O2, Ar is Balance Air, air speed (GHSV)=10000h-1, loaded catalyst 5ml.Gas analysis is auspicious using Qingdao crowd
ZR-3200 flue gas analyzers.In addition, the catalyst chosen prepared by embodiment 5 carries out the experiment of water resistant and sulfur resistance.Herein
In experiment, simulated flue gas ingredient has also been passed through 200ppm SO in addition to the flue gas of above-mentioned concentration in mixed gas2Gas.
Its denitration effect is as shown in Figure 1.
As shown in Table 1, the catalyst prepared by Examples 1 to 5 is respectively provided with preferable low-temperature denitration activity, at 200 DEG C
More than 90%, and embodiment 5 has best denitration effect.
As shown in Figure 1, in the water resistant sulfur resistive using sample prepared by embodiment 5 as denitrating catalyst poisons experiment, anti-
H is passed through when answering 60 minutes2O and SO2Afterwards, denitration efficiency drops to 82% or so, stops being passed through H at 210 minutes2O and SO-2Afterwards
Denitration efficiency is slightly promoted, but initial effect is not achieved.
The present invention has low-temperature SCR active window using graphene-manganese oxide composite material as the active ingredient of catalyst；
Graphene can effectively reduce absorption of the water in catalyst surface, while can also reduce sulphur as a kind of hydrophobic material
Hydrochlorate improves the ability that its water resistant sulfur resistive poisons in the deposition of catalyst surface；Using the method for a step 3D printing, by catalyst
Active ingredient straight forming, compared with traditional honeycomb-shaped SCR catalyst, have bigger specific surface area, be more suitable for
Pore passage structure so as to effectively reduce flue gas resistance, reduce pressure drop, further improves the service life of catalyst；This hair
Without ceramic monolith in bright catalyst, the load capacity of catalyst is effectively improved, the denitration efficiency of catalyst is made to obtain significantly
Enhancing.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of active ingredient passes through the SCR catalyst of 3D printing straight forming, which is characterized in that includes the original of following mass parts
Material：
2. a kind of active ingredient according to claim 1 is existed by the SCR catalyst of 3D printing straight forming, feature
In the manganese salt is one or more of manganese acetate, manganese chloride, manganese sulfate, manganese nitrate.
3. a kind of active ingredient according to claim 1 is existed by the SCR catalyst of 3D printing straight forming, feature
In the reactive oligomers are unsaturated polyester (UP), acrylic resin, polyester acrylate, polymethyl methacrylate, polyethers
One or more of acrylate, epoxy acrylate, polyurethane acrylate.
4. a kind of active ingredient according to claim 1 is existed by the SCR catalyst of 3D printing straight forming, feature
In the reactive diluent is senecioate-hydroxyl ethyl ester, diallyphthalate acid esters, triethylene-glycol diacrylate
One or several kinds in ester, isobomyl acrylate fat.
5. a kind of active ingredient according to claim 1 is existed by the SCR catalyst of 3D printing straight forming, feature
In, the photoinitiator be a, a '-dimethyl benzil ketals, a, a '-diethoxy acetophenone, 2,4,6- trimethyl hexichol first
One or more of ketone, isopropyl thioxanthone, Omnicat550, Omnicat650.
6. a kind of active ingredient according to claim 1 is by the preparation method of the SCR catalyst of 3D printing straight forming,
It is characterized in that, specifically comprise the following steps：
(1) will graphite oxide be prepared using Hummer ' s methods, take 100 mass parts graphite oxide, the four of 20~50 mass parts
Acetate hydrate manganese, 200~400 mass parts polymethyl methacrylates are placed in ball mill with the rotating speed of 400~800r/min point
2~6h is dissipated, dispersion liquid is made；
(2) the diallyphthalate acid fat of 30~100 mass parts and the Omnicat650 of 5~10 mass parts are weighed, by it
It is added in above-mentioned dispersion liquid, 1~2h of mechanical agitation, 1~2h of sonic oscillation；
(3) honeycombed catalyst model is established by computer software AutoCAD, by model be arranged to the length of side for 100~
300mm is highly 100~300mm, and inside is the hexahedron knot of 0.5~2mm diametric holes, and threedimensional model is resolved into thickness
For 30~100 μm of section, and input in SLA 3D printers；
(4) it is 0.1~0.3m/s to set printer operating speed, and print resolution is 70~100 μm, powder sending quantity 0.2mm2/
S；The intensity, angle, shape of printer light beam are regulated and controled, the slurry is successively printed and photocuring, obtains honeycomb
Shape catalyst idiosome；
(5) by idiosome under protection of argon gas, 500~700 DEG C of 2~4h of calcining, remove wherein impurity, and catalyst is lived
Change.
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| CN109095912A (en) * | 2018-09-06 | 2018-12-28 | 深圳大学 | A kind of method that 3D printing is integrated cordierite honeycomb ceramic carrier |
| CN109499349A (en) * | 2018-11-21 | 2019-03-22 | 江苏瑞洁环境工程科技有限责任公司 | For reducing the desulfurization particle of CFB recirculating fluidized bed discharge |
| CN110433770A (en) * | 2019-07-17 | 2019-11-12 | 天津大学 | Photocatalysis honeycomb C-base composte material and preparation method |
| CN111167429A (en) * | 2020-02-27 | 2020-05-19 | 辽宁科技大学 | Preparation method of 3D printing aluminum-silicon metallurgy flue gas denitration catalyst carrier |
| CN113289626A (en) * | 2021-04-25 | 2021-08-24 | 南京师范大学 | Preparation method and application of 3D printing monolithic catalyst applied to Fenton-like/persulfate system |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109095912A (en) * | 2018-09-06 | 2018-12-28 | 深圳大学 | A kind of method that 3D printing is integrated cordierite honeycomb ceramic carrier |
| CN109499349A (en) * | 2018-11-21 | 2019-03-22 | 江苏瑞洁环境工程科技有限责任公司 | For reducing the desulfurization particle of CFB recirculating fluidized bed discharge |
| CN110433770A (en) * | 2019-07-17 | 2019-11-12 | 天津大学 | Photocatalysis honeycomb C-base composte material and preparation method |
| CN110433770B (en) * | 2019-07-17 | 2022-03-18 | 天津大学 | Photocatalytic honeycomb carbon-based composite material and preparation method thereof |
| CN111167429A (en) * | 2020-02-27 | 2020-05-19 | 辽宁科技大学 | Preparation method of 3D printing aluminum-silicon metallurgy flue gas denitration catalyst carrier |
| CN113289626A (en) * | 2021-04-25 | 2021-08-24 | 南京师范大学 | Preparation method and application of 3D printing monolithic catalyst applied to Fenton-like/persulfate system |
| CN113289626B (en) * | 2021-04-25 | 2023-04-21 | 南京师范大学 | Preparation method and application of 3D printing monolithic catalyst applied to Fenton/persulfate-like system |
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