CN104857949A - Indirect regeneration denitration catalyst and preparation method thereof - Google Patents
Indirect regeneration denitration catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an indirect regeneration denitration catalyst preparation method, including the following steps: (1) crushing and sieving a deactivated denitration catalyst, ultrasonically cleaning in an n acidic or alkaline solution for 0.5-4 h in the ultrasonic frequency of 40-100 KHZ, drying, and ball milling to obtain a raw material with the particle size of d90 greater than or equal to 10 mum and less than or equal to 20 mum; (2) respectively taking 75-90 parts by weight of the raw material, 0.1-5 parts by weight of active substance ammonium metavanadate, 4-10 parts by weight of ammonium tungstate or ammonium metatungstate, 3-6 parts by weight of glass fiber, 0.5-1 parts by weight of hydroxymethyl cellulose, and 300-500 parts by weight of deionized water to put into a mixer to obtain slurry; (3) preparing the slurry into an indirect regeneration denitration catalyst wet blank body by a hydraulic extrusion mechanism; and (4) calcining and drying to obtain an indirect regeneration denitration catalyst. The indirect regeneration denitration catalyst preparation method is simple, the activity of the prepared indirect regeneration of denitration catalyst reaches more than 95% of a new catalyst, strength and wear rate are improved, the use time of the catalyst is extended, and the cost of the production and use of the catalyst is reduced.
Description
Technical field
The present invention relates to a kind of renovation process of decaying catalyst, particularly relate to a kind of preparation method of indirect regeneration denitrating catalyst, belong to catalyst preparation technical field.
Background technology
SCR (SCR) technology is the flue-gas denitration process that current domestic and international application is the widest, operation is the most stable, and denitrating catalyst is the important component part of this technique.Because denitrating catalyst is expensive, being the largest portion of denitrification apparatus investment and operating cost, for economizing on resources, reducing costs, domesticly at present first inactivation denitrating catalyst to be regenerated, cannot will reclaim wherein metallic member by chemical metallurgy method by regenerating section.It is predicted, in inactivation denitrating catalyst, remove the part of regeneration, possess that the catalyst that can not regenerate treatment conditions accounts for total amount 1/3, be that 220,000 m3 calculate by the output of " 12 " waste catalyst in latter stage, 7-8 ten thousand m3 can not be reached by regeneration catalyzing dosage.
Domestic about mainly recovery can not be concentrated on by regeneration of deactivated denitrating catalyst at present, comprise and extract vanadium, tungsten and titanium dioxide aspect.Inactivation denitrating catalyst is pulverized by existing Chinese patent 201210035019.0, sodium is filtered, regulate pH value, add carbonic hydroammonium or ammonium chloride solution, ammonium metavanadate precipitate, with rare ammonium bicarbonate soln washing 2-3 time after filtration, then with ethanol washing 1-2 time, ammonium metavanadate finished product is obtained; , by obtained for surplus solution evaporation order of ammoniumparatungstate crystal, then carry out calcining obtained tungstic acid.Patent 201310085634.7 is carried out dedusting to useless denitrating catalyst, is pulverized abrasive dust, adds nonionic emulsifier flocculation, after then press filtration hydrolysis, water rinse, add potash or phosphoric acid obtains metatitanic acid filter cake after sulfuric acid solution; Filter cake is calcined after drying at 500-800 DEG C, then pulverizes, levigately obtains finished titanium dioxide.Above method process can not regenerating section inactivation denitrating catalyst process complicated, wastewater flow rate is large, extracts metal cost higher.With can not the process of regeneration of deactivated denitrating catalyst directly as the raw material manufacturing denitrating catalyst, a kind of method as indirect regeneration denitrating catalyst is reported very few so far.Waste denitration catalyst re-uses and manufactures denitrating catalyst by patent 201210492800.0 after simply purging, weak point is that waste denitration catalyst process is simple, poisoning element K, Na etc. in catalyst micropore are also untreated, tear strength does not provide yet, inactivation denitrating catalyst utilization rate limited (the highest by 90%), and with the addition of a large amount of metal oxide and inorganic additive, add the cost of indirect regenerated catalyst.
Summary of the invention
The object of the invention is to solve in prior art complex disposal process when inactivation denitrating catalyst reclaims, wastewater flow rate is large, extracts the shortcoming that metal cost is higher, provides the preparation method that a kind of method regenerates denitrating catalyst simply indirectly.
The present invention adopts following technical scheme: a kind of preparation method of indirect regeneration denitrating catalyst, comprises the steps:
(1) preparation of pretreatment and raw material: carry out vibratory sieve after the denitrating catalyst of inactivation being placed in the broken 0.5 ~ 2min of disintegrating machine and sieve, 20 ~ 100 mesh sieves are selected to sieve, sieve 3 ~ 5min, then at room temperature condition, to the inactivation denitrating catalyst ultrasonic cleaning after sieving, supersonic frequency is 40 ~ 100KHZ, ultrasonic time is 0.5 ~ 4h, in air dry oven under 60 ~ 110 DEG C of conditions dry 2 ~ 8h, dried inactivation denitrating catalyst is carried out ball milling 8 ~ 24h on ball mill, to obtain particle size be 10 μm≤raw material of d90≤20 μm;
(2) preparation of slurry: score by weight and do not get raw material 75 ~ 90 parts, active material ammonium metavanadate 0.1 ~ 5 part, ammonium tungstate or ammonium metatungstate 4 ~ 10 parts, 3 ~ 6 parts, glass fibre, CMC 0.5 ~ 1 part, deionized water 300 ~ 500 parts, each component is added carry out in batch mixer mixing, batch mixer stirs each component 1 ~ 3h with the rotating speed of 200 ~ 1000r/min, fully mix, make slurry, for subsequent use;
(3) indirectly regeneration denitrating catalyst wets the preparation of idiosome: inserted by slurry in descaling extrusion press, the pressure of descaling extrusion press is 2 ~ 5Mpa; Extrude and indirectly regenerated denitrating catalyst and to wet idiosome;
(4) dry and calcining: wet the indirect regeneration denitrating catalyst obtained idiosome drying 25 ~ 80 DEG C of drying 100 ~ 288h, then the base substrate that wet by dried indirect regeneration denitrating catalyst calcines 10 ~ 24h under 200 ~ 650 DEG C of conditions, is indirectly regenerated denitrating catalyst.
Further, adopt acid solution cleaning during ultrasonic cleaning, described acid solution is mass percentage concentration is 0.1 ~ 10% sulfuric acid, nitric acid or hydrochloric acid solution.
Further, during described ultrasonic cleaning, adopt alkaline solution, described alkaline solution to be mass percentage concentration be 0.1 ~ 10% ammoniacal liquor, NaOH or potassium hydroxide solution.
Preparation method of the present invention is simple, first by the broken flyash eliminated in inactivation denitrating catalyst surface and duct that sieves, and then under ultrasonication, adopt acid and alkalescence cleaning decaying catalyst, its toxicity matter is leached, processing procedure is simple, and the indirect regeneration denitrating catalyst activity prepared reaches more than 95% of raw catelyst, and intensity and wear rate significantly improve, extend the service time of catalyst, reduce production and the use cost of catalyst.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1: a kind of preparation method of indirect regeneration denitrating catalyst, step is as follows:
(1) after the denitrating catalyst disintegrating machine of inactivation being carried out broken 0.5min, to be sieved 3min by 20 order vibratory sieves, then at room temperature condition, ultrasonic cleaning is carried out with in the sulfuric acid solution of 0.1%, supersonic frequency is 40KHZ scavenging period is 4h, the inactivation denitrating catalyst after cleaning is put into the dry 8h of 60 DEG C of convection oven, finally on ball mill, carry out ball milling 8h, detect at Beckman LS-100Q type laser particle size analyzer, particle diameter d
90be 19.56 μm, obtain raw material;
(2) score by weight do not get raw material 75 parts, active material ammonium metavanadate 1 part, ammonium tungstate 5 parts, 3 parts, glass fibre, CMC 0.5 part, deionized water 300 parts add carry out in batch mixer mixing, the rotating speed of batch mixer is 200r/min, mix and blend 3h, mix, make slurry, for subsequent use;
(3) insert in descaling extrusion press by material, extrusion pressure is 2Mpa; Extrude and indirectly regenerated denitrating catalyst and to wet idiosome;
(4) dry and calcining: get indirect regeneration denitrating catalyst that step (3) obtains and to wet idiosome 80 DEG C of dry 100h, then in 200 DEG C of calcining 4h, then under temperature 650 DEG C of conditions, calcine 6h, indirectly regenerated denitrating catalyst, catalyst chemical formula is expressed as 1%V
2o
5-5%WO
3/ TiO
2.
Embodiment 2: a kind of preparation method of indirect regeneration denitrating catalyst, step is as follows:
(1) after the denitrating catalyst disintegrating machine of inactivation being carried out broken 2min, to be sieved 5min by 100 order vibratory sieves, then at room temperature condition, carry out ultrasonic cleaning with in the sulfuric acid solution of 5%, supersonic frequency is 100KHZ scavenging period is 0.5h, the inactivation denitrating catalyst after ultrasonic cleaning is placed in the dry 2h of 110 DEG C of convection oven, finally on ball mill, carry out ball milling 24h, detect at Beckman LS-100Q type laser particle size analyzer, particle diameter d90 is 10.35 μm, obtains raw material;
(2) score by weight do not get raw material 90 parts, active material ammonium metavanadate 1 part, ammonium metatungstate 5 parts, 6 parts, glass fibre, CMC 1 part, deionized water 500 parts add carry out in batch mixer mixing, the rotating speed of batch mixer is 1000r/min mixing 1h, fully mix, form slurry, for subsequent use;
(3) insert in descaling extrusion press by material, extrusion pressure is 5Mpa; Extrude and indirectly regenerated denitrating catalyst and to wet idiosome;
(4) dry and calcining: get indirect regeneration denitrating catalyst that step (3) obtains and to wet idiosome, 25 DEG C of dry 288h, then in 200 DEG C of temperature lower calcination 10h, 650 DEG C of temperature lower calcination 14h, indirectly regenerated denitrating catalyst, catalyst chemical formula is expressed as 1%V
2o
5-5%WO
3/ TiO
2.
Embodiment 3: a kind of preparation method of indirect regeneration denitrating catalyst, step is as follows:
(1) after the denitrating catalyst disintegrating machine of inactivation being carried out broken 1min, to be sieved 3min by 80 order vibratory sieves, then at room temperature condition, carry out ultrasonic cleaning with in the salpeter solution of 1%, supersonic frequency is 60KHZ scavenging period is 2h, the inactivation denitrating catalyst after cleaning is placed in the dry 3h of 100 DEG C of convection oven, finally on ball mill, carry out ball milling 12h, detect at Beckman LS-100Q type laser particle size analyzer, particle diameter d90 is 15.76 μm, obtains raw material;
(2) score by weight do not get raw material 85 parts, active material ammonium metavanadate 1 part, ammonium tungstate 5 parts, 4 parts, glass fibre, CMC 0.8 part, deionized water 430 parts add carry out in batch mixer mixing, the rotating speed of batch mixer is 800r/min mixing 2h, each component is fully mixed, form slurry, for subsequent use;
(3) insert in descaling extrusion press by material, extrusion pressure is 3.5Mpa; Extrude and indirectly regenerated denitrating catalyst and to wet idiosome;
(4) dry and calcining: get indirect regeneration denitrating catalyst that step (3) obtains and to wet idiosome, 40 DEG C of dry 240h, then in 200 DEG C of temperature lower calcination 8h, 650 DEG C of temperature lower calcination 16h, indirectly regenerated denitrating catalyst, catalyst chemical formula is expressed as 1%V
2o
5-5%WO
3/ TiO
2.
Embodiment 4: a kind of preparation method of indirect regeneration denitrating catalyst, step is as follows:
(1) after the denitrating catalyst disintegrating machine of inactivation being carried out broken 1.5min, to be sieved 5min by 60 order vibratory sieves, then at room temperature condition, ultrasonic cleaning is carried out with in the salpeter solution of 1%, supersonic frequency is 60KHZ scavenging period is 3h, the inactivation denitrating catalyst after cleaning is placed in the dry 4h of 90 DEG C of convection oven, finally on ball mill, carries out ball milling 18h, detects at Beckman LS-100Q type laser particle size analyzer, particle diameter d90 is 17.53 μm, obtains raw material;
(2) score by weight do not get raw material 80 parts, active material ammonium metavanadate 1 part, ammonium tungstate or ammonium metatungstate 5 parts, 5 parts, glass fibre, CMC 1 part, deionized water 460 parts add carry out in batch mixer mixing, the rotating speed of batch mixer is 700r/min mixing 3h, each component is fully mixed, make slurry, for subsequent use;
(3) insert in descaling extrusion press by material, extrusion pressure is 2.9Mpa; Extrude and indirectly regenerated denitrating catalyst and to wet idiosome;
(4) dry and calcining: get indirect regeneration denitrating catalyst that step (3) obtains and to wet idiosome, 60 DEG C of dry 148h, then in 200 DEG C of temperature lower calcination 16h, 650 DEG C of temperature lower calcination 86h, indirectly regenerated denitrating catalyst, catalyst chemical formula is expressed as 1%V
2o
5-5%WO
3/ TiO
2.
Embodiment 5: a kind of preparation method of indirect regeneration denitrating catalyst, step is as follows:
(1) after the denitrating catalyst disintegrating machine of inactivation being carried out broken 1min, to be sieved 3min by 60 order vibratory sieves, then at room temperature condition, carry out ultrasonic cleaning with in 5% salpeter solution, supersonic frequency is 80KHZ scavenging period is 2h, the denitrating catalyst after ultrasonic cleaning is placed in the dry 3h of 100 DEG C of convection oven, finally on ball mill, carry out ball milling 24h, detect at Beckman LS-100Q type laser particle size analyzer, particle diameter d90 is 15.98 μm, obtains raw material;
(2) score by weight do not get raw material 85 parts, active material ammonium metavanadate 1 part, ammonium metatungstate 5 parts, 4 parts, glass fibre, CMC 0.8 part, deionized water 430 parts add carry out in batch mixer mixing, the rotating speed of batch mixer is that 800r/min is uniformly mixed 2h, mix, form slurry, for subsequent use;
(3) insert in descaling extrusion press by material, extrusion pressure is 3.5Mpa; Extrude and indirectly regenerated denitrating catalyst and to wet idiosome;
(4) dry and calcining: get indirect regeneration denitrating catalyst that step (3) obtains and to wet idiosome, 40 DEG C of dry 240h, then in 200 DEG C of temperature lower calcination 8h, 650 DEG C of temperature lower calcination 16h, indirectly regenerated denitrating catalyst, catalyst chemical formula is expressed as 1%V
2o
5-5%WO
3/ TiO
2.
Comparative example 1: a kind of preparation method of indirect regeneration denitrating catalyst, step is as follows:
(1) the denitrating catalyst dried compressed air of inactivation purged, then on ball mill, carry out ball milling 8h, detect at Beckman LS-100Q type laser particle size analyzer, particle diameter d90 is 28.73 μm, obtains raw material;
(2) score by weight do not get raw material 75 parts, active material ammonium metavanadate 1 part, ammonium tungstate 5 parts, 3 parts, glass fibre, CMC 0.5 part, deionized water 300 parts add carry out in batch mixer mixing, the rotating speed of 200r/min is uniformly mixed 3h, mix, until form good slurry, for subsequent use;
(3) insert in descaling extrusion press by material, extrusion pressure is 2Mpa; Extrude and indirectly regenerated denitrating catalyst and to wet idiosome;
(4) dry and calcining: get indirect regeneration denitrating catalyst that step (3) obtains and to wet idiosome 80 DEG C of dry 100h, then in 200 DEG C of temperature lower calcination 4h, then 650 DEG C of temperature lower calcination 6h, are regenerated denitrating catalyst indirectly, and catalyst chemical formula is expressed as 1%V
2o
5-5%WO
3/ TiO
2.
Comparative example 2: a kind of preparation method of indirect regeneration denitrating catalyst, step is as follows:
1) after the denitrating catalyst disintegrating machine of inactivation being carried out broken 0.5min, sieved by 20 order vibratory sieves, then on ball mill, carry out ball milling 8h, detect at Beckman LS-100Q type laser particle size analyzer, particle diameter d
90be 25.56 μm, obtain raw material;
(2) count by weight raw material 75 parts, active material ammonium metavanadate 1 part, ammonium tungstate 5 parts, 3 parts, glass fibre, CMC 0.5 part, deionized water 300 parts added carry out in batch mixer mixing, the rotating speed of 200r/min is uniformly mixed 3h, mix, until form good slurry, for subsequent use;
(3) insert in descaling extrusion press by material, extrusion pressure is 2Mpa; Extrude and indirectly regenerated denitrating catalyst and to wet idiosome;
(4) dry and calcining: get indirect regeneration denitrating catalyst that step (3) obtains and to wet idiosome 80 DEG C of dry 100h, then in 200 DEG C of temperature lower calcination 4h, then 650 calcining 6h, indirectly regenerated denitrating catalyst, catalyst chemical formula is expressed as 1%V
2o
5-5%WO
3/ TiO
2.
The denitrating catalyst of Example 1-5 and comparative example 1-2 and fresh catalyst detect >=middle requirement detection denitration activity, compression strength and wear rate according to DL/T 1286-2013≤coal steam-electric plant smoke denitrating catalyst inspection specifications.Test condition is: NO 500ppm, NH
3500ppm, O
210%, 1000ppmSO
2, N
2for Balance Air, air speed 23000h
– 1
Experimental result is as table 1.
Table 1
Drawn by table 1, the activity of the indirect regeneration denitrating catalyst that the present invention prepares is higher than the denitrating catalyst adopting commonsense method to prepare in comparative example 1-2, and compression strength and tear strength significantly improve.
Be placed in fixed bed reactors according to table 1 by the indirect regeneration denitrating catalyst of preparation in embodiment 4, METHOD FOR CONTINUOUS DETERMINATION 168 hours at 380 DEG C, denitration efficiency remains unchanged substantially, and denitration activity is more than 89%.
Claims (3)
1. indirectly regenerate a preparation method for denitrating catalyst, it is characterized in that: comprise the steps:
(1) preparation of pretreatment and raw material: carry out vibratory sieve after the denitrating catalyst of inactivation being placed in broken 0.5 ~ 2 min of disintegrating machine and sieve, 20 ~ 100 mesh sieves are selected to sieve, sieve 3 ~ 5min, then at room temperature condition, to the inactivation denitrating catalyst ultrasonic cleaning after sieving, supersonic frequency is 40 ~ 100KHZ, ultrasonic time is 0.5 ~ 4h, in air dry oven under 60 ~ 110 DEG C of conditions dry 2 ~ 8h, dried inactivation denitrating catalyst is carried out ball milling 8 ~ 24h on ball mill, to obtain particle size be 10 μm≤raw material of d90≤20 μm;
(2) preparation of slurry: score by weight and do not get raw material 75 ~ 90 parts, active material ammonium metavanadate 0.1 ~ 5 part, ammonium tungstate or ammonium metatungstate 4 ~ 10 parts, 3 ~ 6 parts, glass fibre, CMC 0.5 ~ 1 part, deionized water 300 ~ 500 parts, each component is added carry out in batch mixer mixing, batch mixer stirs each component 1 ~ 3h with the rotating speed of 200 ~ 1000r/min, fully mix, make slurry, for subsequent use;
(3) indirectly regeneration denitrating catalyst wets the preparation of idiosome: inserted by slurry in descaling extrusion press, the pressure of descaling extrusion press is 2 ~ 5Mpa; Extrude and indirectly regenerated denitrating catalyst and to wet idiosome;
(4) dry and calcining: wet the indirect regeneration denitrating catalyst obtained idiosome drying 25 ~ 80 DEG C of drying 100 ~ 288h, then the base substrate that wet by dried indirect regeneration denitrating catalyst calcines twice successively under 200 ~ 650 DEG C of conditions, calcination time 10 ~ 24h, is regenerated denitrating catalyst indirectly.
2. the preparation method of the denitrating catalyst of regeneration indirectly as claimed in claim 1, is characterized in that: adopt acid solution cleaning during ultrasonic cleaning, described acid solution is mass percentage concentration is 0.1 ~ 10% sulfuric acid, nitric acid or hydrochloric acid solution.
3. the preparation method of the denitrating catalyst of regeneration indirectly as claimed in claim 1, is characterized in that: adopt alkaline solution during described ultrasonic cleaning, described alkaline solution to be mass percentage concentration be 0.1 ~ 10% ammoniacal liquor, NaOH or potassium hydroxide solution.
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Cited By (1)
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Application publication date: 20150826 |