CN113797650A - Preparation method of PTFE (polytetrafluoroethylene) filtering material with high catalyst loading rate - Google Patents
Preparation method of PTFE (polytetrafluoroethylene) filtering material with high catalyst loading rate Download PDFInfo
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Abstract
The invention discloses a preparation method of a PTFE (polytetrafluoroethylene) filtering material with high catalyst loading rate, which relates to the technical field of PTFE filtering materials and comprises the following steps: (1) preparing a PTFE porous fiber material; (2) loading of a catalyst; (3) the PTFE filter material is obtained by opening, mixing, fine opening, carding, lapping, adding base cloth and needling to prepare a needled felt, and then sequentially burning, pressing, polishing and heat setting. The invention has the beneficial effects that: the invention mixes the two-component substances, and the matrix material is thermally decomposed or volatilized under the high-temperature condition, so as to prepare the porous material, and the prepared porous material fiber is used for the high-efficiency loading of the catalyst and the dedusting and denitration filter material, thereby realizing the application in the field of industrial flue gas cooperative treatment. The PTFE porous short fiber can effectively load more catalysts, can effectively avoid the production side effect caused by hardening of the filter material in the post-treatment, and avoids the falling of the catalysts in the use process.
Description
Technical Field
The invention relates to the technical field of PTFE (polytetrafluoroethylene) filter materials, in particular to a preparation method of a PTFE filter material with high catalyst loading rate.
Background
At present, industrial flue gas nitrogen oxides are mostly removed by a Selective Catalytic Reduction (SCR) technology, and particulate pollutants are mostly removed by a dust removal filter bag. Two kinds of pollutants are equallyd divide at present and do not carry out the desorption alone through special device, and the construction, operation and the maintenance cost etc. of its device are all higher, and need occupy great place and space. With the development of the industrial flue gas treatment technology, the cooperative treatment of various pollutants becomes the development trend of the industrial tail gas treatment technology, mainly reflects the cooperation between the dust removal technology and the technologies of denitration, desulfurization, dioxin removal and the like, and achieves the cooperative treatment of multiple pollutants by realizing the combination of multiple functions on the same product.
Patent publication No. CN104998467A discloses a filter material with denitration and dioxin-removing effects and a preparation method thereof. The problems with this technique are as follows: the filtering material is prepared by PTFE fibers containing a catalyst, a PTFE microporous membrane containing the catalyst and PTFE base cloth into a PTFE felt layer, and then the PTFE felt layer is subjected to integral impregnation with an emulsion containing an active metal catalyst and subsequent high-temperature sintering, so that the whole preparation process of the catalytic filtering material is long and complicated, and the effective catalyst component loaded by the filtering material is insufficient.
The porous material has a higher loading rate compared to the non-porous material and U.S. patent publication No. US4482516A increases the density of the dry extrudate to greater than about 2.0gm/cc through a calendering densification step, the porous polytetrafluoroethylene material fibers having a certain porosity compared to conventional materials of the same matrix tensile strength, but the manufacturing process is more complex.
Disclosure of Invention
The invention aims to solve the technical problems that the PTFE filter material in the prior art has low catalyst loading rate and the preparation method of the porous polytetrafluoroethylene fiber is complex, and provides the preparation method of the PTFE filter material with high catalyst loading rate.
The invention solves the technical problems through the following technical means:
a preparation method of a PTFE filter material with high catalyst loading rate comprises the following steps:
(1) PTFE porous fibrous material: mixing and stirring PEFE dispersion resin, a silane coupling agent and a base material, wherein the total addition amount of the silane coupling agent and the base material is 3-7% of the mass of the PTFE dispersion resin, the mass ratio of the silane coupling agent to the base material is 1:3, drying, adding aviation kerosene for mixing, placing the mixed powder in a drying room at 50-60 ℃ for curing for 48-72h, pressing a rod by a rod pressing machine, extruding wires by a wire extruding machine, soaking in a water tank at 70 ℃, rolling the powder into a film by a rolling machine, sintering at 350-450 ℃ for 4-6h, and carding and curling by needling to obtain a PTFE porous fiber material; the base material comprises petroleum-based polymer, bio-based polymer or fluorocarbon resin;
(2) mixing a manganese nitrate solution: cerium nitrate crystal: coupling agent: mixing deionized water according to a mass ratio of 80:60 (2-6) to (15-40), stirring to form a denitration catalyst precursor solution, dipping the PTFE porous fiber material obtained in the step (1) into the denitration catalyst precursor solution, drying, rolling and cutting into PTFE porous short fibers;
(3) and (3) opening, mixing, finely opening, carding, lapping, adding base cloth and needling the PTFE short fibers prepared in the step (2) to prepare a needled felt, and then sequentially performing burning, pressing and molding and heat setting to obtain the PTFE filter material.
Has the advantages that: the invention mixes the two-component substances, and the matrix material is thermally decomposed or volatilized under the high-temperature condition, so as to prepare the porous material, and the prepared porous material fiber is used for the high-efficiency loading of the catalyst and the dedusting and denitration filter material, thereby realizing the application in the field of industrial flue gas cooperative treatment.
The PTFE porous short fiber can effectively load more catalysts, can effectively avoid the production side effect caused by hardening of the filter material in the post-treatment, and avoids the falling of the catalysts in the use process.
The petroleum-based polymer does not melt or has a softening point lower than the temperature range in which most fluoroolefin polymers melt and the polymers decompose into carbonaceous substances, the bio-based polymer has a low thermal decomposition temperature, and the temperature range in which fluorocarbon resin thermally decomposes into carbonaceous substances or thermally volatilizes is smaller than that of PTFE resin.
The PTFE resin and the denitration catalyst precursor solution or the catalyst powder are not directly mixed, and the precursor solution is in a micro-nano particle state, so that fibers are easy to break when being in a fiber state, and the production efficiency is hindered.
Preferably, the petroleum-based polymer comprises PA6, PA11, PVA, or PET.
Preferably, the petroleum-based polymer is PVA.
Preferably, the bio-based polymer comprises methylcellulose, hydroxyethylcellulose, methylhydroxypropylcellulose, hydroxypropylmethylcellulose, hydroxypropylcellulose, ethylcellulose or carboxymethylcellulose.
Preferably, the bio-based polymer is carboxymethyl cellulose.
Preferably, the fluorocarbon resin is FEP resin.
Preferably, the silane coupling agent is a silane coupling agent hk 560.
Preferably, the PEFE dispersion resin, the silane coupling agent and the matrix material are mixed and stirred for 0.5-1.5h, and the drying temperature is 150-180 ℃.
Preferably, the pressure of the rod pressing machine during rod pressing is 4-5 MPa.
Preferably, the gram weight of the needled felt is 800-850g/m2。
The invention has the advantages that: the invention mixes the two-component substances, and the matrix material is thermally decomposed or volatilized under the high-temperature condition, so as to prepare the porous material, and the prepared porous material fiber is used for the high-efficiency loading of the catalyst and the dedusting and denitration filter material, thereby realizing the application in the field of industrial flue gas cooperative treatment.
The PTFE porous short fiber can effectively load more catalysts, can effectively avoid the production side effect caused by hardening of the filter material in the post-treatment, and effectively reduce the falling of the catalysts in the use process.
The PTFE resin and the denitration catalyst precursor solution or the catalyst powder are not directly mixed, and the precursor solution is in a micro-nano particle state, so that fibers are easy to break when being in a fiber state, and the production efficiency is hindered.
Drawings
Fig. 1 is a denitration efficiency testing system in an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
TABLE 1 decomposition temperatures of the base materials
Example 1
The preparation method of the PTFE filter material with high catalyst loading rate specifically comprises the following steps:
(1) preparation of PTFE porous fiber material:
pretreatment: mixing and stirring PEFE dispersed resin, an isocyanate silane coupling agent hk560 and PVA for 1.5h, wherein the mass ratio of the isocyanate silane coupling agent hk560 to the PVA is 1:3, the total addition amount of the isocyanate silane coupling agent hk560 and the PVA is 3 percent of the mass of the PTFE dispersed resin, then placing the mixture in a drying oven at 180 ℃ for drying, uniformly spraying the weighed aviation kerosene which is equivalent to 40 percent of the mass of the PTFE dispersed resin into powder by using an oil spray rod, sealing the powder in a rotating machine at 20 ℃, and carrying out forward rotation for 30min and reverse rotation for 30 min. Finally, the mixed powder is placed in a drying room at 60 ℃ for curing for 72 hours. Pressing the bar with a bar press under 5MPa, extruding with a filament extruder, and soaking in 70 deg.C water tank for 25 min. And then calendering by a calender to form a film, and obtaining the PTFE filament by sintering, degreasing, drafting, needling, carding and curling. Wherein, the sintering process is controlled differently, and the performance of the sintered product is greatly different. The heating temperature for sintering and removing oil is 450 ℃, and simultaneously, the matrix material is thermally decomposed to form the porous PTFE fiber material.
(2) Preparation of catalyst-loaded PTFE porous staple fiber:
manganese nitrate solution: cerium nitrate crystal: coupling agent: mixing deionized water according to the mass ratio of 80:60:5:25, stirring the mixture in a stirring device for 90min to form a uniform denitration catalyst precursor solution, soaking the PTFE filaments prepared in the step (1), drying, rolling and cutting into PTFE porous short fibers.
(3) Preparing the dust removal and denitration integrated needled felt:
opening, mixing, fine opening, carding, lapping, adding base cloth and needling the PTFE short fibers manufactured in the step (2) to manufacture a needled felt; the gram weight is controlled to be 850g/m2. Wherein, opening, mixing, fine opening, carding, lapping, adding base cloth and needling are all the prior art.
(4) Post-treatment process
And (4) sequentially carrying out burning, pressing and heat setting on the needled felt woven in the step (3) to prepare the flue gas filtering material with high dust removal and denitration efficiency and stability. Wherein, firing, pressing and heat setting are both the prior art.
Example 2
The preparation method of the PTFE filter material with high catalyst loading rate specifically comprises the following steps:
(1) preparation of PTFE porous fiber material:
pretreatment: mixing and stirring PEFE dispersion resin, an isocyanate silane coupling agent hk560 and carboxymethyl cellulose for 1.5h, wherein the mass ratio of the isocyanate silane coupling agent hk560 to the carboxymethyl cellulose is 1:3, the total addition amount of the isocyanate silane coupling agent hk560 and the carboxymethyl cellulose is 5 percent of the mass of the PTFE dispersion resin, then placing the mixture in a 180 ℃ oven for drying, uniformly spraying extrusion aid aviation kerosene with the weighed mass of 40 percent of the PTFE dispersion resin in powder by using an oil spray rod, sealing the powder in a rotating machine at the temperature of 20 ℃, and carrying out forward rotation for 30min and reverse rotation for 30 min. Finally, the mixed powder is placed in a drying room at 60 ℃ for curing for 72 hours. Pressing the bar with a bar press under 5MPa, extruding with a filament extruder, and soaking in 70 deg.C water tank for 25 min. And then calendering by a calender to form a film, and obtaining the PTFE filament by sintering, degreasing, drafting, needling, carding and curling. Wherein, the sintering process is controlled differently, and the performance of the sintered product is greatly different. The heating temperature for sintering and removing oil is 450 ℃, and simultaneously, the base material is fully thermally decomposed to form the porous PTFE fiber material.
(2) Preparation of catalyst-loaded PTFE porous staple fiber:
manganese nitrate solution: cerium nitrate crystal: coupling agent: mixing deionized water according to the mass ratio of 80:60:5:25, stirring the mixture in a stirring device for 90min to form a uniform denitration catalyst precursor solution, soaking the PTFE filaments prepared in the step (1), drying, rolling and cutting into PTFE porous short fibers.
(3) Preparing the dust removal and denitration integrated needled felt:
opening, mixing, fine opening, carding, lapping, adding base cloth and needling the PTFE short fibers manufactured in the step (2) to manufacture a needled felt; the gram weight is controlled to be 850g/m2. Wherein, opening, mixing, fine opening, carding, lapping, adding base cloth and needling are all the prior art.
(4) Post-treatment process
And (4) sequentially carrying out burning, pressing and heat setting on the needled felt woven in the step (3) to prepare the flue gas filtering material with high dust removal and denitration efficiency and stability. Wherein, firing, pressing and heat setting are both the prior art.
Example 3
The preparation method of the PTFE filter material with high catalyst loading rate specifically comprises the following steps:
(1) preparation of PTFE porous fiber material:
pretreatment: mixing and stirring PEFE dispersed resin, isocyanate silane coupling agent hk560 and FEP resin for 1.5h, wherein the mass ratio of the isocyanate silane coupling agent hk560 to the FEP resin is 1:3, the total addition amount of the isocyanate silane coupling agent hk560 and the FEP resin is 7% of the mass of the PTFE dispersed resin, then placing the mixture in a drying oven at 180 ℃ for drying, uniformly spraying extrusion aid aviation kerosene with the weighed mass of 40% of the mass of the PTFE dispersed resin into powder by using an oil spray rod, sealing the powder in a rotating machine at 20 ℃, and carrying out forward rotation for 30min and backward rotation for 30 min. Finally, the mixed powder is placed in a drying room at 60 ℃ for curing for 72 hours. Pressing the bar with a bar press under 5MPa, extruding with a filament extruder, and soaking in 70 deg.C water tank for 25 min. And then calendering by a calender to form a film, and obtaining the PTFE filament by sintering, degreasing, drafting, needling, carding and curling. Wherein, the sintering process is controlled differently, and the performance of the sintered product is greatly different. The heating temperature for sintering and removing oil is 450 ℃, and simultaneously, the base material is fully thermally decomposed to form the porous PTFE fiber material.
(2) Preparation of catalyst-loaded PTFE porous staple fiber:
manganese nitrate solution: cerium nitrate crystal: coupling agent: mixing deionized water according to the mass ratio of 80:60:5:25, stirring the mixture in a stirring device for 90min to form a uniform denitration catalyst precursor solution, soaking the PTFE filaments prepared in the step (1), drying, rolling and cutting into PTFE porous short fibers.
(3) Preparing the dust removal and denitration integrated needled felt:
opening, mixing, fine opening, carding, lapping, adding base cloth and needling the PTFE short fibers manufactured in the step (2) to manufacture a needled felt; the gram weight is controlled to be 850g/m2. Wherein the opening, mixing, fine opening, carding, lapping, base cloth adding and needling are all the prior artAnd (4) performing the operation.
(4) Post-treatment process
And (4) sequentially carrying out burning, pressing and heat setting on the needled felt woven in the step (3) to prepare the flue gas filtering material with high dust removal and denitration efficiency and stability. Wherein, firing, pressing and heat setting are both the prior art.
Comparative example 1
Preparation of PTFE fiber:
a pretreatment part: placing PTFE dispersion resin (Dongye 240 brand) in an oven at 180 deg.C for drying; then, an extrusion aid aviation kerosene (tin-free new mechanical chemical product company, Ltd.) in an amount of 40% by mass of the weighed PTFE dispersion resin was uniformly sprayed into the powder by using an oil spray rod, and the powder was sealed in a rotary machine at 20 ℃ to rotate forward for 30min and reverse for 30 min. Finally, the mixed powder is placed in a drying room at 60 ℃ for curing for 72 hours. Pressing the bar with a bar press under 5MPa, extruding with a filament extruder, and soaking in 70 deg.C water tank for 25 min. And then calendering by a calender to form a film, sintering to remove oil, drafting, needling and carding, curling to obtain PTFE filaments, rolling and cutting into PTFE short fibers.
(2) Manufacturing a dedusting and denitration integrated needled felt;
opening, mixing, fine opening, carding, lapping, adding base cloth and needling the PTFE short fibers manufactured in the step (1) to manufacture a needled felt; the gram weight is controlled to be 850g/m2。
(3) Post-treatment process
Sequentially carrying out burning, pressing and heat setting on the needled felt woven in the step (2), wherein the impregnation liquid used in the heat setting impregnation link is as follows: manganese nitrate solution: cerium nitrate crystal: coupling agent: deionized water is mixed and prepared according to the mass ratio of 80:60:5:25, and the mixture is placed into a stirring device to be stirred for 90min to form a uniform denitration catalyst precursor solution.
Experimental data and analysis:
the weight gain and denitration efficiency of the filter materials in examples 1 to 3 and comparative example 1 were measured, and the measurement results are shown in tables 2 and 3.
And (3) weight gain test: and measuring the mass change of the fiber with a certain length before and after impregnation, and repeating the test for multiple times (n is more than or equal to 5).
The weight gain rate is (m2-m1)/m1 is 100%
Wherein:
m 1: mass before treatment of fiber with certain length, unit: gram (g)
M2: mass after treatment of fiber with certain length, unit: gram (g)
TABLE 2 porous Filter Material fiber weight gain
| Serial number | Base material | Average weight gain (%) |
| Example 1 | Petroleum based polymers | 17±2 |
| Example 2 | Bio-based polymers | 20±5 |
| Example 3 | Fluorocarbon resin | 15±3 |
| Comparative example 1 | Polytetrafluoroethylene | 1±2 |
The denitration efficiency was evaluated as NOx or NO conversion, see the following formula. The denitration efficiency test is carried out on a fixed reaction bed, and the test gas simulates the actual kiln flue gas (NO or NOx, O2), reducing gas (NH3) and balance gas (Ar or N2), as shown in FIG. 1, and the test system in FIG. 1 is the prior art.
In the formula:
eta-denitration efficiency;
|MO|in-reaction tube inlet NO concentration;
|NO|out-reaction tube outlet NO concentration.
As can be seen from table 2, the fibers in the examples of the present invention can increase the loading of the catalyst.
TABLE 3 test results of dust removal and denitration efficiency
The air pressure in the using process of the filter material is normally 3 kilograms, in order to verify the non-shedding performance of the catalyst load, 5 kilograms of air is adopted to blow and blow the finished product filter material, wherein the filter material is 100cm2The front of the large and small dough sheet is sprayed for 60s, and the mass change before and after the filter material is sprayed is recorded.
Mass change rate (m2-m1)/m 1%
Wherein:
m 1: mass before filter material blowing, unit: gram (g)
m 2: mass after filter material blowing, unit: gram (g)
TABLE 4 Filter Material Mass Change
| Serial number | Base material | Mass change rate (%) |
| Example 1 | Petroleum based polymers | 3.0±0.2 |
| Example 2 | Bio-based polymers | 2.6±0.3 |
| Example 3 | Fluorocarbon resin | 2.8±0.4 |
| Comparative example 1 | Polytetrafluoroethylene | 6.4±0.1 |
As can be seen from table 4, the modified porous PTFE needled felt supported catalyst did not readily shed compared to the PTFE needled felt.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of a PTFE filter material with high catalyst loading rate is characterized by comprising the following steps: the method comprises the following steps:
(1) PTFE porous fibrous material: mixing and stirring PEFE dispersion resin, a silane coupling agent and a base material, wherein the total addition amount of the silane coupling agent and the base material is 3-7% of the mass of the PTFE dispersion resin, the mass ratio of the silane coupling agent to the base material is 1:3, drying, adding aviation kerosene for mixing, placing the mixed powder in a drying room at 50-60 ℃ for curing for 48-72h, pressing a rod by a rod pressing machine, extruding wires by a wire extruding machine, soaking in a water tank at 70 ℃, rolling the powder into a film by a rolling machine, sintering at 350-450 ℃ for 4-6h, and carding and curling by needling to obtain a PTFE porous fiber material; the base material comprises petroleum-based polymer, bio-based polymer or fluorocarbon resin;
(2) mixing a manganese nitrate solution: cerium nitrate crystal: coupling agent: mixing deionized water according to a mass ratio of 80:60 (2-6) to (15-40), stirring to form a denitration catalyst precursor solution, dipping the PTFE porous fiber material obtained in the step (1) into the denitration catalyst precursor solution, drying, rolling and slitting to form PTFE porous short fibers;
(3) and (3) opening, mixing, finely opening, carding, lapping, adding base cloth and needling the PTFE short fibers prepared in the step (2) to prepare a needled felt, and then sequentially performing burning, pressing and molding and heat setting to obtain the PTFE filter material.
2. The method for preparing a high catalyst loading rate PTFE filter material of claim 1, wherein: the petroleum-based polymer includes PA6, PA11, PVA, or PET.
3. The method for preparing a high catalyst loading rate PTFE filter material according to claim 2, wherein: the petroleum-based polymer is PVA.
4. The method for preparing a high catalyst loading rate PTFE filter material of claim 1, wherein: the bio-based polymer comprises methylcellulose, hydroxyethylcellulose, methylhydroxypropylcellulose, hydroxypropylmethylcellulose, hydroxypropylcellulose, ethylcellulose or carboxymethylcellulose.
5. The method for preparing a high catalyst loading rate PTFE filter material according to claim 4, wherein: the bio-based polymer is carboxymethyl cellulose.
6. The method for preparing a high catalyst loading rate PTFE filter material of claim 1, wherein: the fluorocarbon resin is FEP resin.
7. The method for preparing a high catalyst loading rate PTFE filter material of claim 1, wherein: the silane coupling agent is a silane coupling agent hk 560.
8. The method for preparing a high catalyst loading rate PTFE filter material of claim 1, wherein: the PEFE dispersion resin, the silane coupling agent and the matrix material are mixed and stirred for 0.5-1.5h, and the drying temperature is 150-180 ℃.
9. The method for preparing a high catalyst loading rate PTFE filter material of claim 1, wherein: the pressure of the bar pressing machine during bar pressing is 4-5 MPa.
10. The method for preparing a high catalyst loading rate PTFE filter material of claim 1, wherein: the gram weight of the needled felt is 800-850g/m2。
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| WO2023150340A1 (en) * | 2022-02-04 | 2023-08-10 | Cormetech, Inc. | Catalytic fibers and applications thereof |
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