CN105944665A - Preparation method of molecular sieve concentration rotating wheel adsorption packing for treating VOCs - Google Patents
Preparation method of molecular sieve concentration rotating wheel adsorption packing for treating VOCs Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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Abstract
The invention discloses a preparation method of molecular sieve concentration wheel adsorption packing for treating VOCs. A ceramic honeycomb carrier is prepared through the steps that 60 wt%-90 wt% of aggregates prepared by processing cordierite and 10 wt%-40 wt% of raw materials are mixed to prepare a basic material, an adhesive accounting for 2 wt%-5 wt% of the basic material, a pore forming agent accounting for 5 wt%-10 wt% of the basic material and a lubricating agent accounting for 0.1 wt%-3 wt% of the basic material are added, the materials are mixed and subjected to extrusion forming, then the honeycomb ceramic body is obtained, molecular sieves are treated, molecular sieve slurry is prepared, the ceramic honeycomb carrier is soaked into the molecular sieve slurry, the surplus slurry is blown away, drying is conducted, and firing under heat preservation is conducted to obtain molecular sieve concentration rotating wheel adsorption packing; the molecular sieve concentration rotating wheel adsorption packing is soaked into a solution containing an organosilicone surfactant or fluorocarbon surfactant, then drying is conducted at the temperature 60 DEG C-200 DEG C, and the modified hydrophobic molecular sieve concentration rotating wheel adsorption packing is obtained. The molecular sieve concentration rotating wheel adsorption packing is simple in preparation method and process, low in requirements for equipment and plants, capable of easily achieving industrialization, high in strength, good in corrosion resistance and film formation property and high in adsorption capacity.
Description
Technical field
The present invention relates to the preparation method of a kind of molecular sieve concentration runner filler processing VOC (being called for short VOCs), belong to environmental protection, energy-conservation technical field.
Background technology
VOCs refers to that saturated vapor pressure is more than 70Pa, boiling point organic compound below 260 DEG C under normal pressure at normal temperatures.This kind of material has that kind is many, the feature of complicated component, long-term low dose release, it is that a class has carcinogenic, the chemical substance of teratogenesis, mutagenicity to human body, participate in photochemical reaction, be also the major prerequisites material of Atmospheric particulates formation simultaneously, huge to atmospheric environment and human injury.In May, 2010; the General Office of the State Council does departments such as forwarded Environmental Protection Department " improving the notice of the instruction of region air quality about propelling atmospheric pollution groupcontrol work " (Office of the State Council sends out [2010] No. 33), proposes to carry out the prevention and cure of pollution work of VOCs first from the level of country.JIUYUE in 2013 General Office of the State Council on the 12nd has issued " prevention and control of air pollution action plan ", it is indicated that strengthen comprehensive control dynamics, reduces multi-pollutant discharge, advances volatile organic matter pollution control.The work the most how administering VOCs has become as one of Contemporary Environmental Problems significant problem urgently to be resolved hurrily.
For at present, the improvement control method of VOCs can be divided mainly into two categories below: absorption method and decomposition method.A kind of be absorption method be exactly by the gas containing VOCs by condensation method, the VOCs of gaseous state is transformed into liquid, the method being then collected re-using is the most only higher at exhaust gas concentration, the price of volatile material costly, just can be selected in the case of having recovery value；Two kinds be decomposition method be by directly burning, heat-accumulation combustion and the means of catalysis burning, VOCs is decomposed into H2O and CO2Method.Either use absorption method or decomposition method, all there is bigger problem: a wherein seldom part can only be carried out condensation recovery by absorption method, and efficiency is the lowest；Decomposition method makes the most concentration of tail gas of industrial discharge relatively low, and compare both approaches, and the third Production by Catalytic Combustion Process is low due to its initiation temperature, and energy consumption is relatively low, to advantages such as the requirement of equipment are low, is a kind of combustion system the most economic.But combustion method requires the biggest due to tolerance, therefore it is required that the air quantity that combustor can process is sufficiently high, either equipment takes up an area or operation energy consumption is the highest.Molecular sieve concentration runner system then can solve this problem.The operation principle of molecular sieve concentration runner system is: concentration runner is using molecular sieve as adsorbing material, when the gas containing low concentration VOCs passes through, molecular sieve can be by wherein Adsorption of Organic above, inorganic molecules composition directly passes through, with the hot blast of little air quantity, the Organic substance on molecular sieve is desorbed the most again, obtain the VOCs gas of high concentration, then carry out next step process further according to actual situation.Either absorption method or decomposition method, this system is all suitable for.The critical component of molecular sieve concentration runner system is sorption wheel (runner), runner is as adsorbing material by molecular sieve, it is coated on honeycomb ceramic carrier and is made, swivel bearing is installed in the middle part of it, equipped with gas seal corrosion-resistant, resistant to elevated temperatures on runner, runner is isolated into 3 regions: adsorption treatment district, desorption and regeneration district and cooling zone.A complete set of equipment is mainly made up of waste gas filter, molecular sieve concentration runner, air exhauster and heat-exchange system.Patent CN102389773A proposes and a kind of uses traditional copy paper method to the method preparing molecular sieve concentration runner adsorption stuffing, but the equipment required for the method is more, and plant area is bigger, and molding difficulty is relatively big, complex technical process, is difficult to realize.
Summary of the invention
For the problem prepared by traditional copy paper method in above-mentioned prior art existing for the method for molecular sieve concentration runner adsorption stuffing, the present invention proposes a kind of coating molecular sieve on ceramic honeycomb carrier, then hydrophobically modified is carried out, obtain the preparation method of hydrophobic molecular sieve concentration runner adsorption stuffing, preparation method technique of the present invention is simple, equipment and Factory Building are required relatively low, it is easy to accomplish industrialization.
The technical scheme that the technical problem to be solved in the present invention is taken is: the preparation method of described process VOCs molecular sieve concentration runner adsorption stuffing, and it comprises the following steps:
A, the preparation of ceramic honeycomb carrier, aggregate 60-90wt % and the raw material 10-40wt% being made by cordierite chemistry that ceramic honeycomb carrier is processed by cordierite are mixed to form basic material, add the basic binding agent expecting 2-5wt%, the pore creating material of 5-10wt%, after the lubricant batch mixing pugging of 0.1-3wt%, extrusion molding, follow-up process is dried, sintering obtains honeycomb ceramic carrier, it is covered with hole on described honeycomb ceramic carrier hole wall, hole aperture is between 2-12 μm, and described honeycomb ceramic carrier apparent porosity is at 30-65%；Described raw material are by 30-50tw% raw Pulvis Talci, 15-30tw%Al203Powder and 30-50tw% Kaolin composition.
B, the process of molecular sieve, make compound by different types of molecular sieve proportionally ball milling, then by compound: abrading-ball: the weight ratio of water is 1:(3 ~ 6): (3 ~ 10) carry out ball milling and obtain the molecular sieve base material that particle diameter is 0.5-4 μm；
C, preparation molecular sieve slurry, molecular sieve base material, Ludox, Alumina gel and four kinds of raw materials of water are pressed following weight ratio is (15～20): (10～15): (5～10): after the stirring of (60～65) mixing machinery, obtain molecular sieve slurry；
D, the preparation of adsorption stuffing, immerse among molecular sieve slurry by honeycomb ceramic carrier, takes out after a period of time, blows away additional size, is dried, and insulation is fired and obtained molecular sieve concentration runner adsorption stuffing；
E, the hydrophobically modified of molecular sieve concentration runner adsorption stuffing, by the molecular sieve concentration runner adsorption stuffing obtained by step d, immerse containing in organic silicon surfactant or the solution containing fluorocarbon surfactant, wherein the mass fraction of organic silicon surfactant and fluorocarbon surfactant is respectively 0.1%-2% and 0.01%-2%, after a period of time, take out, blow away unnecessary serosity, follow-up 60 DEG C ~ 200 DEG C drying, obtain the hydrophobic molecular sieve concentration runner adsorption stuffing of modification.
Described Ludox, Alumina gel content are 1% ~ 40%, and water is RO water or distilled water, and the solution containing organic silicon surfactant and fluoro-carbon surface active is alcoholic solution (such as methanol, ethanol, propanol, ethanol exist) or the mixed solution based on alcohol.
Molecular sieve concentration runner adsorption stuffing of the present invention is the key core parts processing VOCs gas molecular sieve concentration runner system.
The present invention also adds flat silica flour more than 10% or the vitreous silica of raw material weight in raw material.
The molecular sieve preparing molecular sieve slurry of the present invention can be type ZSM 5 molecular sieve, 4A type molecular sieve, 5A type molecular sieve, 13X type molecular sieve or other model hydrophobic molecules sieve.
The preferred hydroxypropyl methyl cellulose of bonding agent of the present invention (HPMC), it is possible to be organic adhesive (such as epoxy resin etc.) as other；The preferred polymethyl methacrylate of described pore creating material (PMMA) or ethylmethylcellulose, it is possible to be other similar pore creating material；The preferred poly alpha olefin of described lubricant, it is possible to be other similar lubricant (such as silicone oil, fatty acid amide etc.).
The section holes of honeycomb ceramic carrier of the present invention can be delthyrium, four square holes, hexagon ring or ripple hole, and hole mesh number is between 50-400 mesh, and thickness of honeycomb wall is between 0.25-0.70mm.
The preparation method of molecular sieve concentration runner adsorption stuffing of the present invention is compared with prior art: the innovation of its technical scheme is:
One is to use ceramic honey comb as the carrier of molecular sieve, on the one hand the problem existing for carrier manufacture in traditional method it is that of avoiding, two aspects can be made into again surface and have the hole of net distribution, are greatly improved the porosity of molecular sieve and the molecular sieve carrier of adsorption surface area
Two is the molecular sieve slurry made of compound and Ludox, Alumina gel and the water using different molecular sieve series the to become adsorption layer as molecular sieve surface, making molecular sieve surface layer have the features such as intensity is high, corrosion-resistant, biofilm is good, described raw material use raw Pulvis Talci, Al203Powder, Kaolin and silica flour preparation of raw material and mean diameter are 2 μm-40 μm, dispersion or span ＜ 3.0.
Three is, with silicone active agent or fluorocarbon surfactant, molecular sieve has been carried out modification, makes molecular sieve surface activity be greatly improved, and evenly, absorption strengthens activity distribution with regeneration capacity.
Summary, the present invention is compared with prior art: not only preparation method technique is simple, equipment and Factory Building are required relatively low, it is easy to accomplish industrialization, and the molecular sieve concentration runner adsorption stuffing intensity for preparing high, corrosion-resistant good, biofilm is good, high adsorption capacity.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1: described method step is:
1. the preparation of honeycomb ceramic carrier, the aggregate 70% processed with cordierite, it is mixed to form basic material by the raw material 30% of cordierite chemical analysis preparation, then adds basic hydroxypropyl methyl cellulose (HPMC) binding agent expecting weight 5%, polymethyl methacrylate (PMMA) pore creating material of 10%, the poly alpha olefin lubricant of 1%, after batch mixing pugging, extrusion molding, follow-up through being dried, sintering, obtains honeycomb ceramic carrier.Being covered with hole on this carrier hole wall, aperture requires between 4-12 μm, and D50 is about 8 μm, and dispersion≤1.4, apparent porosity is at 30%-65%；Described raw material are by 40tw% raw Pulvis Talci, 20tw%Al203Powder and 40tw% Kaolin composition.
2. ball milling molecular sieve, in mass ratio 6:2:2 weigh ZSM-5 molecular sieve, 4A molecular sieve, and compound made by 13X molecular sieve, then by compound: abrading-ball: the part by weight of water is 1:4:9, then carry out high speed ball milling, the particle diameter to molecular sieve is about 2 μm；
3. preparation molecular sieve slurry, according to molecular sieve: Ludox: Alumina gel: the ratio of water=15:14:6:65 weighs raw material, after mechanical agitation 30min, obtains molecular sieve slurry；
4. the load of molecular sieve, immerses in molecular sieve slurry by cellular structure ceramic carrier, after carrier is fully wet out, is taken out by ceramic honey comb, blows away the unnecessary serosity in duct, after drying, puts into 500 DEG C of insulation 2h in electric furnace, obtain molecular sieve concentration runner adsorption stuffing；
5. the hydrophobically modified of filler, preparation mass fraction is the solution of the fluorocarbon surfactant of 0.05%, and filler step 4 obtained impregnates in this solution, after 10min, take out, blow away surplus liquid, 250 DEG C are dried, obtain the molecular sieve concentration runner adsorption stuffing of hydrophobically modified.
Embodiment 2: described method step is:
1. the aggregate 80% processed with cordierite, it is mixed to form basic material by the raw material 20% of cordierite chemical composition preparation, add basic hydroxypropyl methyl cellulose (HPMC) binding agent expecting weight 3% again, polymethyl methacrylate (PMMA) pore creating material of 8%, the poly alpha olefin lubricant of 2%, after batch mixing pugging, extrusion molding, follow-up through being dried, sintering, obtain honeycomb ceramic carrier, being covered with pothole on this carrier hole wall, aperture requires between 4-12 μm, and D50 is about 8 μm, dispersion≤1.4, apparent porosity is at 30%-65%；Described raw material are by 35tw% raw Pulvis Talci, 30tw%Al203Powder and 35tw% Kaolin composition.
2. ball milling molecular sieve, in mass ratio 5:3:2 weigh ZSM-5 molecular sieve, 5A molecular sieve, and 13X molecular sieve is made compound, then pressed compound: abrading-ball: the part by weight 1:5:7 of water, then carry out high speed ball milling, and the particle diameter to molecular sieve is about 1 μm；
3. preparation molecular sieve slurry, according to molecular sieve: Ludox: Alumina gel: the ratio of water=20:14:6:60 weighs raw material, after mechanical agitation 30min, obtains molecular sieve slurry；
4. the load of molecular sieve, immerses in molecular sieve slurry by cellular structure ceramic carrier, after carrier is fully wet out, is taken out by ceramic honey comb, blows away the unnecessary serosity in hole wall, after drying, puts into 500 DEG C of insulation 2h in electric furnace, obtain molecular sieve concentration runner adsorption stuffing；
5. the hydrophobically modified of filler, preparation mass fraction is the solution of the fluorocarbon surfactant of 0.1%, in this solution of filler step 4 obtained, after 10min, takes out, blows away surplus liquid, and 250 DEG C are dried, obtain the molecular sieve concentration runner adsorption stuffing of hydrophobically modified.
Embodiment 3: described method step is:
1. the preparation of honeycomb ceramic carrier, the aggregate (powder) 85% processed with cordierite, it is mixed to form basic material by the raw material (powder) 15% of cordierite chemical composition preparation, then adds the basic epoxy adhesive expecting weight 2%, the ethylmethylcellulose pore creating material of 6%, the organic silicone oil lubricant of 0.5%, after batch mixing pugging, extrusion molding, follow-up through being dried, sintering, obtains honeycomb ceramic carrier.Being covered with hole on this carrier hole wall, aperture requires between 4-12 μm, and D50 is about 8 μm, and dispersion≤1.4, apparent porosity is at 30%-65%；Described raw material are by 45tw% raw Pulvis Talci, 25tw%Al203Powder and 30tw% Kaolin and account for the silica flour composition of above-mentioned three kinds of raw material weights 6%.
2. ball milling molecular sieve, in mass ratio 7:3 weigh ZSM-5 molecular sieve, and compound made by 13X molecular sieve, then by compound: abrading-ball: the weight of water is 1:6:4, then carry out high speed ball milling, the particle diameter to molecular sieve is about 0.5 μm；
3. preparation molecular sieve slurry, according to molecular sieve: Ludox: Alumina gel: the ratio of water=18:12:8:63 weighs raw material, after mechanical agitation 30min, obtains molecular sieve slurry；
4. the load of molecular sieve, immerses in molecular sieve slurry by cellular structure ceramic carrier, after carrier is fully wet out, is taken out by ceramic honey comb, blows away the unnecessary serosity in duct, after drying, puts into 500 DEG C of insulation 2h in electric furnace, obtain molecular sieve concentration runner adsorption stuffing；
5. the hydrophobically modified of filler, preparation mass fraction is the solution of the organic silicon surfactant of 0.5%, and filler step 4 obtained impregnates in this solution, after 10min, take out, blow away surplus liquid, 250 DEG C are dried, obtain the molecular sieve concentration runner adsorption stuffing of hydrophobically modified.
Last it is noted that above example only in order to the present invention is described and and unrestricted technical scheme described in the invention；Therefore, although this specification with reference to each above-mentioned embodiment to present invention has been detailed description, but, it will be understood by those within the art that, still the present invention can be modified or equivalent；And all are without departing from the technical scheme of spirit and scope of invention and improvement thereof, it all should be contained in the middle of scope of the presently claimed invention.
Claims (4)
1. the preparation method processing VOCs molecular sieve concentration runner adsorption stuffing, it is characterised in that: it comprises the following steps:
Aggregate 60-90wt % and the raw material 10-40wt% prepared by cordierite chemical analysis that a, ceramic honeycomb carrier are processed by cordierite are mixed to form basic material, after adding the lubricant batch mixing pugging of the basic material binding agent of 2-5wt%, the pore creating material of 5-10wt%, 0.1-3wt%, extrusion molding, follow-up process is dried, sintering obtains honeycomb ceramic carrier, it is covered with hole on described honeycomb ceramic carrier hole wall, described hole aperture is between 2-12 μm, and described honeycomb ceramic carrier apparent porosity is at 30-65%；Described raw material are by 30-50tw% raw Pulvis Talci, 15-30tw%Al203Powder and 30-50tw% Kaolin composition；
B, the process of molecular sieve, make compound by different types of molecular sieve proportionally ball milling, then by compound: abrading-ball: the weight ratio of water is 1:(3 ~ 6): (3 ~ 10) carry out ball milling and obtain the molecular sieve base material that particle diameter is 0.5-4 μm；
C, preparation molecular sieve slurry, molecular sieve base material, Ludox, Alumina gel and four kinds of raw materials of water are pressed following weight ratio is (15～20): (10～15): (5～10): after the stirring of (60～65) mixing machinery, obtain molecular sieve slurry；
D, the preparation of adsorption stuffing, immerse among molecular sieve slurry by honeycomb ceramic carrier, takes out after a period of time, blows away additional size, is dried, and insulation is fired and obtained molecular sieve concentration runner adsorption stuffing；
E, the hydrophobically modified of molecular sieve concentration runner adsorption stuffing, by the molecular sieve concentration runner adsorption stuffing obtained by step d, immerse containing in organic silicon surfactant or the solution containing fluorocarbon surfactant, wherein the mass fraction of organic silicon surfactant and fluorocarbon surfactant is respectively 0.1%-2% and 0.01%-2.0%, after a period of time, take out, blow away unnecessary serosity, follow-up 60 DEG C ~ 200 DEG C drying, obtain the hydrophobic molecular sieve concentration runner adsorption stuffing of modification.
A kind of preparation method processing VOCs molecular sieve concentration runner adsorption stuffing the most according to claim 1, is characterized in that: add the silica flour less than raw material weight 10% in described raw material.
A kind of preparation method processing VOCs molecular sieve concentration runner adsorption stuffing the most according to claim 1 and 2, is characterized in that: described bonding agent is hydroxypropyl methyl cellulose or ethylmethylcellulose；Described pore creating material is polymethyl methacrylate；Described lubricant is poly alpha olefin.
A kind of preparation method processing VOCs molecular sieve concentration runner adsorption stuffing the most according to claim 1 and 2, it is characterized in that: the section holes of described honeycomb ceramic carrier can be delthyrium, four square holes, hexagon ring or ripple hole, hole mesh number is between 50-400 mesh, and thickness of honeycomb wall is between 0.25-0.70mm.
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