CN103143396B - Honeycomb flue gas denitrification catalyst and preparation method thereof - Google Patents
Honeycomb flue gas denitrification catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a honeycomb flue gas denitrification catalyst and a preparation method thereof, belonging to the technical field of inorganic new materials. The honeycomb flue gas denitrification catalyst is mainly prepared by carrying out extrusion molding and sintering on the following raw materials in parts by weight: 68-92.8 parts of nano TiO2, 3-10 parts of nano SiO2, 2-10 parts of glass fiber, 0.1-0.5 part of extrusion aid, 0.1-0.2 part of carboxymethyl cellulose, 0.1-0.3 part of polyoxyethylene and 0.1-0.2 part of sesbania powder. The preparation method comprises the following steps: (1) weighing the nano TiO2 and nano SiO2 powder, adding the extrusion aid, adding water while stirring to obtain paste, and adding ammonia water to regulate the pH value to 7-11; (2) adding the rest of raw materials, evenly mixing, and extruding with an extruding machine to obtain a honeycomb blank; (3) drying the blank at 30-70 DEG C under the relative humidity of 20-100% for 7-15 days; and (4) calcining the dried blank at 250-300 DEG C for 8-15 hours, calcining at 380-420 DEG C for 5-10 hours, and calcining at 580-620 DEG C for 8-12 hours to obtain the finished product.
Description
Technical field
The invention belongs to New Inorganic Materials technical field, be specifically related to a kind of cellular catalyst for denitrating flue gas, also relate to the preparation method going back catalyst simultaneously.
Background technology
Nitrogen oxide (NO
x) be the main reason forming acid rain and photochemical fog, serious harm natural environment and human health.Power plants is the discharge rich and influential family of nitrogen oxide, and discharge capacity accounts for 50% of national total release.On September 21st, 2011, national environmental protection portion has issued " fossil-fuel power plant atmospheric pollutant emission standard ", is defined as 100mg/m by unified for the concentration of emission limit value of domestic nitrogen oxide
3, the new-built unit time of implementation, the old unit time of implementation was from July, 2014 from 2012.This concentration of emission limit value requires for national all regions.
At present, for denitrating flue gas, SCR (SCR) method remains international mainstream technology, and its technological core is SCR catalyst.As far back as the seventies in last century, developed country has just started the situation such as emission level, coal characteristics, boiler type according to this country as Japan, Germany, the U.S. etc., have developed a series of SCR catalyst.The advanced experience of many R&D institutions of China or individual foreign, (flue-gas temperature is high, and at 280 DEG C ~ 450 DEG C, dustiness is high, can reach 50 ~ 60g/Nm for the rear boiler smoke condition difference of, burning complicated for Coal Combustion in China ature of coal
3) etc. situation carried out a series of research, and develop some denitrating catalysts.
But, current with TiO
2removal of nitrogen oxide catalyst for nucleus also has the shortcomings such as mechanical strength is low, wear strength is poor, non-refractory, and the phenomenon such as excessive wear, efflorescence easily appears in catalyst in running, and then affects the normal operation of power plant units.Therefore, the denitrating catalyst developing applicable domestic flue gas condition will be an important breakthrough in the industry.
Summary of the invention
Object of the present invention aims to provide the preparation method of a kind of honeycomb type flue gas denitration catalyst and this catalyst.
Based on above-mentioned purpose, technical scheme provided by the invention is: a kind of honeycomb type flue gas denitration catalyst, and the raw material primarily of following weight portion forms through extrusion molding, sintering: nano-TiO
268 ~ 92.8 parts, Nano-meter SiO_2
23 ~ 10 parts, 2 ~ 10 parts, glass fibre, extrusion aid 0.1 ~ 0.5 part, carboxymethyl cellulose 0.1 ~ 0.2 part, polyethylene glycol oxide 0.1 ~ 0.3 part, 0.1 ~ 0.2 part, sesbania powder.
Described raw material also comprises partially/ammonium paratungstate with WO
3meter 2 ~ 10 weight portions, ammonium metavanadate are with V
2o
5meter 0.2 ~ 2 weight portion.
Described nano-TiO
2particle diameter be 1 ~ 10 μm, described Nano-meter SiO_2
2particle diameter be 1 ~ 10nm.
Described extrusion aid is stearic acid or glycerine.
Described honeycomb fashion denitrating flue gas takes off the preparation method of agent, comprises the following steps:
(1) nano-TiO is taken
2, Nano-meter SiO_2
2powder, adds extrusion aid, adds water while stirring and lives into paste, and adds ammoniacal liquor instrumentality material pH value to 7 ~ 11;
(2) add all the other raw materials to mix, utilize extruder to extrude honeycomb fashion idiosome;
(3) make idiosome 30 ~ 70 DEG C, relative humidity under being the condition of 20 ~ 100% dry 7 ~ 15 days;
(4) calcine 8 ~ 15 hours under dried idiosome being first placed in 250 ~ 300 DEG C of conditions, and then in 380 ~ 420 DEG C of calcinings 5 ~ 10 hours, calcine 8 ~ 12 hours, get product for 580 ~ 620 DEG C.
Step (1), before adding ammoniacal liquor instrumentality material pH value, is also added with partially/ammonium paratungstate with WO
3meter 2 ~ 10 weight portions, ammonium metavanadate is with V
2o
5meter 0.2 ~ 2 weight portion.
In described preparation method, nano-TiO
2particle diameter be 1 ~ 10 μm, described Nano-meter SiO_2
2particle diameter be 1 ~ 10nm.
In described preparation method, extrusion aid is stearic acid or glycerine.
The present invention is with TiO
2, SiO
2for main body, the honeycombed catalyst coordinating the raw material such as glass fibre, stearic acid/glycerine, polyethylene glycol oxide, carboxymethyl cellulose and sesbania powder to make has that mechanical strength is high, the advantage such as to resistance to wear.Add WO further on this basis
3presoma partially/ammonium paratungstate and V
2o
5presoma ammonium metavanadate can promote the catalytic activity of this catalyst further, improves its resistance to elevated temperatures.Comprehensively it seems, compared with existing catalyst, catalyst provided by the invention has following advantage:
1. mechanical strength is high, can run at a higher pressure;
2. wear strength is strong, can adapt to the flue gas that dustiness is high, long service life;
3. there is excellent pore structure and specific surface pore volume: > 0.25 cc/g, average pore size: 12 ~ 20nm; Specific area: > 55m
2/ g;
4. stability is strong, can run under different flue-gas temperature conditions;
5. high temperature resistant, at 450 DEG C, 10 hours more than can be run continuously;
6. catalytic activity high (denitration efficiency is high), oxidation rate of sulfur dioxide is low.
Preparation method provided by the invention adopts special drying program and calcination procedure, and obtained catalyst ratio of defects is low, and using strength is secure; Yield rate is high, is suitable for extensive popularization.
Accompanying drawing explanation
Fig. 1 is the radial crushing strength test schematic diagram of test block;
Fig. 2 is the axial compression strength test schematic diagram of test block.
Detailed description of the invention
According to specific embodiment, the invention will be further described below.
embodiment 1
A kind of honeycomb type flue gas denitration catalyst, is formed through extrusion molding, sintering by the raw material of following weight portion: nano-TiO
2(1 ~ 10 μm) 83 parts, Nano-meter SiO_2
2(1 ~ 10nm) 8.3 parts, ammonium metatungstate are with WO
3count 10 weight portions, ammonium metavanadate with V
2o
5count 1 weight, 6.7 parts, glass fibre, extrusion aid (stearic acid) 0.42 part, carboxymethyl cellulose 0.17 part, polyethylene glycol oxide 0.25 part, 0.17 part, sesbania powder.
Its preparation method comprises the following steps:
(1) nano-TiO is taken
2, Nano-meter SiO_2
2powder, ammonium metatungstate and ammonium metavanadate, add extrusion aid, adds water while stirring and live into paste, and add ammoniacal liquor instrumentality material pH value to 7.5;
(2) add all the other raw materials to mix, utilize vacuum-extruder to extrude cross section is 150mm × 150mm, hole count is 15 × 15, length is 1000mm honeycomb fashion idiosome;
(3) make idiosome 30 DEG C, relative humidity under being the condition of 100% dry 5 days, then 40 DEG C, relative humidity under being the condition of 80% dry 4 days, 50 DEG C, relative humidity is under the condition of 50% dry 3 days, 60 DEG C, relative humidity is under the condition of 30% dry 2 days, 70 DEG C, relative humidity is under the condition of 20% dry 1 day.
(4) calcine 15 hours under dried idiosome being first placed in 250 DEG C of conditions, and then in 420 DEG C of calcinings 5 hours, calcine 10 hours, get product for 580 DEG C.
embodiment 2
A kind of honeycomb type flue gas denitration catalyst, is formed through extrusion molding, sintering by the raw material of following weight portion: nano-TiO
2(1 ~ 10 μm) 92.8 parts, Nano-meter SiO_2
2(1 ~ 10nm) 7.4 parts, ammonium metatungstate are with WO
3count 7.4 weight portions, ammonium metavanadate with V
2o
5count 0.8 weight, 9.3 parts, glass fibre, extrusion aid (stearic acid) 0.46 part, carboxymethyl cellulose 0.19 part, polyethylene glycol oxide 0.28 part, 0.19 part, sesbania powder.
Its preparation method comprises the following steps:
(1) nano-TiO is taken
2, Nano-meter SiO_2
2powder, partially/ammonium paratungstate and ammonium metavanadate, add extrusion aid, add water while stirring and live into paste, and add ammoniacal liquor instrumentality material pH value to 8;
(2) add all the other raw materials to mix, utilize vacuum-extruder to extrude cross section is 150mm × 150mm, hole count is 15 × 15, length is 1000mm honeycomb fashion idiosome; With extruder, above-mentioned material is extruded honeycomb fashion idiosome;
(3) make idiosome 30 DEG C, relative humidity under being the condition of 90% dry 4 days, then 40 DEG C, relative humidity under being the condition of 70% dry 3 days, 50 DEG C, relative humidity is under the condition of 40% dry 2 days, 65 DEG C, relative humidity is under the condition of 20% dry 2 days.
(4) calcine 8 hours under dried idiosome being first placed in 300 DEG C of conditions, and then in 380 DEG C of calcinings 10 hours, calcine 12 hours, get product for 580 DEG C.
embodiment 3
A kind of honeycomb type flue gas denitration catalyst, is formed through extrusion molding, sintering by the raw material of following weight portion: nano-TiO
2(1 ~ 10 μm) 68 parts, Nano-meter SiO_2
2(1 ~ 10nm) 3.4 parts, ammonium paratungstate are with WO
3count 2.7 weight portions, ammonium metavanadate with V
2o
5count 0.48 weight, 3.4 parts, glass fibre, extrusion aid (glycerine) 0.14 part, carboxymethyl cellulose 0.14 part, polyethylene glycol oxide 0.2 part, 0.14 part, sesbania powder.
Its preparation method comprises the following steps:
(1) nano-TiO is taken
2, Nano-meter SiO_2
2powder, ammonium paratungstate and ammonium metavanadate, add extrusion aid, adds water while stirring and live into paste, and to add ammoniacal liquor instrumentality material pH value be 7;
(2) add all the other raw materials to mix, utilize vacuum-extruder to extrude cross section is 150mm × 150mm, hole count is 20 × 20, length is 1000mm honeycomb fashion idiosome;
(3) make idiosome 30 DEG C, relative humidity under being the condition of 80% dry 2 days, then 40 DEG C, relative humidity under being the condition of 80% dry 2 days, 50 DEG C, relative humidity is under the condition of 50% dry 1 day, 60 DEG C, relative humidity is under the condition of 30% dry 1 day, 70 DEG C, relative humidity is under the condition of 20% dry 1 day.
(4) calcine 10 hours under dried idiosome being first placed in 280 DEG C of conditions, and then in 390 DEG C of calcinings 9 hours, calcine 9 hours, get product for 610 DEG C.
embodiment 4
A kind of honeycomb type flue gas denitration catalyst, is formed through extrusion molding, sintering by the raw material of following weight portion: nano-TiO
2(1 ~ 10 μm) 80 parts, Nano-meter SiO_2
2(1 ~ 10nm) 3 parts, ammonium metatungstate are with WO
3count 5 weight portions, ammonium metavanadate with V
2o
5count 0.2 weight, 2 parts, glass fibre, extrusion aid (glycerine) 0.1 part, carboxymethyl cellulose 0.2 part, polyethylene glycol oxide 0.1 part, 0.2 part, sesbania powder.
Its preparation method comprises the following steps:
(1) nano-TiO is taken
2, Nano-meter SiO_2
2powder, ammonium paratungstate and ammonium metavanadate, add extrusion aid, adds water while stirring and live into paste, and add ammoniacal liquor instrumentality material pH value to 11;
(2) add all the other raw materials to mix, utilize vacuum-extruder to extrude cross section is 150mm × 150mm, hole count is 20 × 20, length is 1000mm honeycomb fashion idiosome;
(3) make idiosome 30 DEG C, relative humidity under being the condition of 90% dry 3 days, then 40 DEG C, relative humidity under being the condition of 70% dry 3 days, 50 DEG C, relative humidity is under the condition of 40% dry 2 days, 60 DEG C, relative humidity is under the condition of 30% dry 1 day.
(4) calcine 10 hours under dried idiosome being first placed in 270 DEG C of conditions, and then in 410 DEG C of calcinings 6 hours, calcine 11 hours, get product for 590 DEG C.
embodiment 5
A kind of honeycomb type flue gas denitration catalyst, is formed through extrusion molding, sintering by the raw material of following weight portion: nano-TiO
2(1 ~ 10 μm) 70 parts, Nano-meter SiO_2
2(1 ~ 10nm) 10 parts, ammonium metatungstate are with WO
3count 2 weight portions, ammonium metavanadate with V
2o
5count 2 weight, 10 parts, glass fibre, extrusion aid (stearic acid) 0.5 part, carboxymethyl cellulose 0.1 part, polyethylene glycol oxide 0.3 part, 0.1 part, sesbania powder.
Its preparation method comprises the following steps:
(1) nano-TiO is taken
2, Nano-meter SiO_2
2powder, ammonium paratungstate and ammonium metavanadate, add extrusion aid, adds water while stirring and live into paste, and add ammoniacal liquor instrumentality material pH value to 9;
(2) add all the other raw materials to mix, utilize vacuum-extruder to extrude cross section is 150mm × 150mm, hole count is 15 × 15, length is 1000mm honeycomb fashion idiosome;
(3) make idiosome 30 DEG C, relative humidity under being the condition of 95% dry 2 days, then 40 DEG C, relative humidity under being the condition of 70% dry 3 days, 50 DEG C, relative humidity is under the condition of 45% dry 3 days, 60 DEG C, relative humidity is under the condition of 30% dry 1 day, 65 DEG C, relative humidity is under the condition of 20% dry 1 day.
(4) calcine 120 hours under dried idiosome being first placed in 260 DEG C of conditions, and then in 400 DEG C of calcinings 6 hours, calcine 10 hours, get product for 600 DEG C.
embodiment 6 test experiments
1, method of testing
Respectively the honeycomb type flue gas denitration catalyst of embodiment 1,2,3 is tested as follows:
1.1 intensity test
Often kind of catalyst intercepts two test blocks, is of a size of 150 mm × 150, mm × 150 mm; Axial and the horizontal compression strength (range of forcing press is 300KN, compression rate 250N/s) with pressure testing machine test.Fig. 1 and Fig. 2 be shown in by resistance to compression schematic diagram.
tear strength detects
Intercepting appearance and size is the test block of 70mm × 70mm × 70mm, is placed in abrasion test device; By air (the dustiness 50g/m containing wearing and tearing agent (quartz sand particle size 400 ~ 500 μm)
3) pass through sample with 14.5 ± 1 m/s flow velocitys, after running 3h, sample is taken out the tear strength of counting yield.
Wear rate by following formulae discovery every kilogram quartz sand:
Wear rate (%/kg)=(1-W
2/ W
1)/W
3× 100;
Wherein, W
1: example weight (g) before wear testing;
W
2: example weight (g) after wear testing;
W
3: the quartz sand weight (kg) collected.
catalytic performance is tested
From the test test specimen that cellular catalyst cuts 3 × 3 holes, length is 300mm, be filled in reactor, measured denitration efficiency and SO under the following conditions
2oxygenation efficiency.
Test condition:
Specimen size: 3 × 3 holes, length 300mm;
Reaction temperature: 380 DEG C, SV=10,000hr
-1;
Gas composition: NO
x=180ppm, NH
3=180ppm, SO
2=500ppm, O
2=2%, H
2o=10%, N
2=surplus.
test result
As can be seen from the test result that upper table provides, it is large that cellular catalyst provided by the invention has compression strength, and wear rate is low, and denitration rate is high, SO
2the advantages such as oxygenation efficiency is low.
Claims (4)
1. a honeycomb type flue gas denitration catalyst, the raw material primarily of following weight portion forms through extrusion molding, sintering: nano-TiO
268 ~ 92.8 parts, Nano-meter SiO_2
23 ~ 10 parts, 2 ~ 10 parts, glass fibre, extrusion aid 0.1 ~ 0.5 part, carboxymethyl cellulose 0.1 ~ 0.2 part, polyethylene glycol oxide 0.1 ~ 0.3 part, 0.1 ~ 0.2 part, sesbania powder, partially/ammonium paratungstate is with WO
3meter 2 ~ 10 weight portions, ammonium metavanadate are with V
2o
5meter 0.2 ~ 2 weight portion; Described extrusion aid is stearic acid or glycerine;
This honeycomb type flue gas denitration catalyst comprises the following steps when preparing:
(1) nano-TiO is taken
2, Nano-meter SiO_2
2powder, partially/ammonium paratungstate, ammonium metavanadate, add extrusion aid, add water while stirring and live into paste, and add ammoniacal liquor instrumentality material pH value to 7 ~ 11;
(2) add all the other raw materials to mix, utilize extruder to extrude honeycomb fashion idiosome;
(3) make idiosome 30 ~ 70 DEG C, relative humidity under being the condition of 20 ~ 100% dry 7 ~ 15 days;
(4) calcine 8 ~ 15 hours under dried idiosome being first placed in 250 ~ 300 DEG C of conditions, and then in 380 ~ 420 DEG C of calcinings 5 ~ 10 hours, calcine 8 ~ 12 hours, get product for 580 ~ 620 DEG C.
2. honeycomb type flue gas denitration catalyst as claimed in claim 1, is characterized in that, described nano-TiO
2particle diameter be 1 ~ 10 μm, described Nano-meter SiO_2
2particle diameter be 1 ~ 10nm.
3. described in claim 1, honeycomb fashion denitrating flue gas takes off the preparation method of agent, it is characterized in that, comprises the following steps:
(1) nano-TiO is taken
2, Nano-meter SiO_2
2powder, partially/ammonium paratungstate, ammonium metavanadate, add extrusion aid, add water while stirring and live into paste, and add ammoniacal liquor instrumentality material pH value to 7 ~ 11;
(2) add all the other raw materials to mix, utilize extruder to extrude honeycomb fashion idiosome;
(3) make idiosome 30 ~ 70 DEG C, relative humidity under being the condition of 20 ~ 100% dry 7 ~ 15 days;
(4) calcine 8 ~ 15 hours under dried idiosome being first placed in 250 ~ 300 DEG C of conditions, and then in 380 ~ 420 DEG C of calcinings 5 ~ 10 hours, calcine 8 ~ 12 hours, get product for 580 ~ 620 DEG C.
4. honeycomb fashion denitrating flue gas takes off the preparation method of agent as claimed in claim 3, it is characterized in that, described nano-TiO
2particle diameter be 1 ~ 10 μm, described Nano-meter SiO_2
2particle diameter be 1 ~ 10nm.
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| CN107213890A (en) * | 2017-06-09 | 2017-09-29 | 中国石油天然气股份有限公司 | One kind reduction SO2Oxygenation efficiency is without vanadium denitration catalyst and preparation method thereof |
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