CN111749017A - High-strength antibacterial melt-blown air filter material and preparation method thereof - Google Patents
High-strength antibacterial melt-blown air filter material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-strength antibacterial melt-blown air filter material and a preparation method thereof, wherein the preparation method comprises the following steps: s1, carrying out melt extrusion granulation on the coupling agent modified beta-cyclodextrin, the coupling agent modified nano titanium dioxide and polypropylene to obtain modified polypropylene master batches; s2, melting the modified polypropylene master batches and the polypropylene slices, spraying the melted polypropylene master batches and the polypropylene slices through a spinneret to form fibers, spraying beta-cyclodextrin on the surfaces of the formed fibers while spraying the fibers through the spinneret to obtain a melt-blown air filter material base material; s3, padding and drying the melt-blown air filter material base material in the antibacterial finishing liquid to obtain a modified melt-blown air filter material base material; and S4, performing electret treatment on the modified melt-blown air filter material substrate. The melt-blown air filter material disclosed by the invention is high in efficiency, low in resistance, good in antibacterial performance, high in mechanical strength and excellent in protective performance.
Description
Technical Field
The invention relates to the technical field of melt-blown filter materials, in particular to a high-strength antibacterial melt-blown air filter material and a preparation method thereof.
Background
Pollutants such as dust, bacteria and the like in the floating air have great influence on human health, and along with the gradual improvement of living standard, people also put forward higher requirements on air quality. The main raw materials of the melt-blown filter material comprise polypropylene, polyethylene, polylactic acid, PBT and the like, have the characteristics of low fiber fineness, more pores, large specific surface area and complex three-dimensional structure, have good filter performance, and are core materials in the fields of air filtration, protective masks and the like. The mechanical strength of the melt-blown filter material influences the use effect to a great extent, the melt-blown filter material with low strength is easy to tear, the durability is not good, bacteria easily enter from the tear, the filter efficiency is reduced, and the protection effect is seriously influenced; meanwhile, in order to better play a role in disease protection and cut off the disease transmission path, the melt-blown filter material is required to have good antibacterial activity. Therefore, in order to make the melt-blown filter material have a good protection effect, the filter efficiency is required to be high, and higher requirements on the strength and the bacteriostatic performance are provided.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a high-strength antibacterial melt-blown air filter material and a preparation method thereof.
The invention provides a preparation method of a high-strength antibacterial melt-blown air filter material, which comprises the following steps:
s1, uniformly mixing the coupling agent modified beta-cyclodextrin, the coupling agent modified nano titanium dioxide and polypropylene, and then carrying out melt extrusion granulation by a double-screw extruder to obtain modified polypropylene master batches;
s2, uniformly mixing the modified polypropylene master batches and polypropylene slices, adding the mixture into melt-blown equipment, spraying the mixture through a spinneret to form fibers after the mixture is melted, spraying beta-cyclodextrin on the surfaces of the formed fibers while spraying the fibers through the spinneret, and cooling, stretching and shaping the fibers to obtain a melt-blown air filter material base material;
s3, padding and drying the melt-blown air filter material base material in an antibacterial finishing liquid to obtain a modified melt-blown air filter material base material, wherein the antibacterial finishing liquid is prepared by mixing an acetic acid solution of chitosan and epichlorohydrin;
and S4, performing electret treatment on the modified melt-blown air filter material base material through a corona electret device.
Preferably, the coupling agent modified beta-cyclodextrin is prepared by modifying beta-cyclodextrin by using a coupling agent, wherein the weight ratio of the coupling agent to the beta-cyclodextrin is (0.05-0.15): 1.
preferably, the preparation method of the coupling agent modified beta-cyclodextrin comprises the following steps: adding beta-cyclodextrin and a coupling agent into a proper amount of toluene, uniformly dispersing, reacting for 6-12h at 70-90 ℃, centrifuging, washing and drying to obtain the beta-cyclodextrin beta.
Preferably, the coupling agent modified nano titanium dioxide is prepared by modifying nano titanium dioxide by using a coupling agent, wherein the weight ratio of the coupling agent to the nano titanium dioxide is (0.05-0.1): 1.
preferably, the preparation method of the coupling agent modified nano titanium dioxide comprises the following steps: adding nano titanium dioxide and a coupling agent into a proper amount of toluene, uniformly dispersing, reacting at 80-100 ℃ for 6-12h, centrifuging, washing and drying to obtain the nano titanium dioxide.
Preferably, the coupling agent is a silane coupling agent or a titanate coupling agent.
Preferably, the coupling agent modified beta-cyclodextrin accounts for 3-6% of the total weight of the modified polypropylene master batch, and the coupling agent modified nano titanium dioxide accounts for 1-2% of the total weight of the modified polypropylene master batch.
Preferably, the weight ratio of the modified polypropylene master batch to the polypropylene chip is 1: (5-8).
Preferably, in step S2, the weight ratio of the sum of the weights of the modified polypropylene masterbatch and the polypropylene chip to the β -cyclodextrin is 100: (0.3-0.8).
Preferably, the antibacterial finishing liquid is prepared by mixing 1-2% of chitosan acetic acid solution and epichlorohydrin in a volume ratio of (20-30): 1, mixing and preparing.
Preferably, the preparation method of the antibacterial finishing liquid comprises the following steps: adding epichlorohydrin into acetic acid solution of chitosan, and stirring at 60-80 deg.C for 0.5-2 hr.
Preferably, the preparation method of the acetic acid solution of chitosan comprises the following steps: adding chitosan into 0.5-1 wt% acetic acid solution, and stirring at 60-80 deg.C until completely dissolved.
Preferably, in step S3, the bath ratio of the padding process is 1: (40-80) and the rolling allowance is 80-100%.
Preferably, in the step S3, the padding temperature is 40 to 70 ℃, and the drying temperature is 60 to 90 ℃.
Preferably, in step S4, the electret voltage is 5-20kV, and the electret distance is 2.5-4 cm.
Preferably, in the step S1, the temperature for melt extrusion granulation by the twin-screw extruder is 260-280 ℃.
Preferably, in the step S2, the melting temperature in the melt-blowing equipment is 260-280 ℃, and the temperature of the spinneret is 230-250 ℃.
A high-strength antibacterial melt-blown air filter material is prepared by the preparation method.
The invention has the following beneficial effects:
according to the invention, nano titanium dioxide modified by a coupling agent and beta-cyclodextrin modified by the coupling agent are added into a melt-blown raw material of a melt-blown air filter material, and the beta-cyclodextrin is embedded into a fiber surface layer in a spraying manner during melt-blown fiber formation, so that a melt-blown air filter material substrate containing the nano titanium dioxide and the beta-cyclodextrin in the fiber and containing the beta-cyclodextrin on the fiber surface layer is obtained, then chitosan is loaded on the surface of the melt-blown air filter material substrate under the cross-linking action of epoxy chloropropane through the dipping of chitosan antibacterial liquid, and the melt-blown air filter material is finally obtained after electret treatment. The beta-cyclodextrin and the nano titanium dioxide are introduced into the fiber, and the beta-cyclodextrin and the nano titanium dioxide have certain nucleation effect, so that the crystallinity of the material is improved, and the filtering performance and the mechanical strength of the material are improved; the surface of beta-cyclodextrin loaded on the surface layer of the fiber has a large number of hydroxyl active groups, so that chitosan can be more stably fixed on the surface of the fiber under the crosslinking action of epoxy chloropropane, the synergistic effect of the chitosan and nano titanium dioxide can be better exerted, the antibacterial effect and the antibacterial stability of the material are improved, and the fixation of the chitosan on the surface of the material is also beneficial to improving the mechanical strength of the material; meanwhile, the chitosan is loaded on the surface of the material, so that the pores of the material can be reduced, the air resistance is increased, and the beta-cyclodextrin in the fiber and on the surface layer can also play a role in increasing the pores, so that the resistance is reduced on the premise of ensuring the antibacterial effect, and the material has good air permeability. Therefore, the melt-blown air filter material prepared by the invention has the advantages of high efficiency, low resistance, good antibacterial performance, high mechanical strength and excellent protective performance.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
Preparing a high-strength antibacterial melt-blown air filter material:
s1, uniformly mixing the coupling agent modified beta-cyclodextrin, the coupling agent modified nano titanium dioxide and polypropylene, and then performing melt extrusion granulation at the temperature of 260-280 ℃ by using a double-screw extruder to obtain modified polypropylene master batches, wherein the coupling agent modified beta-cyclodextrin accounts for 3% of the total weight of the modified polypropylene master batches, and the coupling agent modified nano titanium dioxide accounts for 2% of the total weight of the modified polypropylene master batches;
s2, mixing the modified polypropylene master batch and the polypropylene slices according to the weight ratio of 1: 5, uniformly mixing, adding the mixture into a melt-blowing device, melting the mixture at the temperature of 260-280 ℃, spraying the mixture through a spinneret at the temperature of 230 ℃ to form fibers, spraying beta-cyclodextrin on the surfaces of the formed fibers while spraying the mixture through the spinneret, cooling, stretching and shaping to obtain the base material of the melt-blown air filter material, wherein the weight ratio of the sum of the modified polypropylene master batches and the polypropylene slices to the beta-cyclodextrin is 100: 0.3;
s3, putting the melt-blown air filter material base material in an antibacterial finishing liquid, wherein the bath ratio is 1: and (40), padding at the temperature of 40 ℃ under the condition that the rolling residual rate is 80%, and drying at the temperature of 60 ℃ to obtain the modified melt-blown air filter material base material, wherein the antibacterial finishing liquid is prepared by mixing an acetic acid solution of chitosan with the mass fraction of 1% and epichlorohydrin according to the volume ratio of 20: 1, the preparation method comprises the following steps: adding chitosan into 0.5% acetic acid solution at 60 deg.C, stirring for dissolving completely to obtain acetic acid solution of chitosan, adding epichlorohydrin, and stirring at 60 deg.C for 0.5 hr to obtain the final product;
and S4, performing electret treatment on the modified melt-blown air filter material base material through a corona electret device, wherein the electret voltage is 5kV, and the electret distance is 2.5 cm.
The preparation method of the coupling agent modified beta-cyclodextrin comprises the following steps: adding 1g of beta-cyclodextrin and 0.05g of silane coupling agent KH-550 into 50mL of toluene for uniform dispersion, reacting at 70 ℃ for 6h, centrifuging, washing and drying to obtain the beta-cyclodextrin modified silane coupling agent; the preparation method of the coupling agent modified nano titanium dioxide comprises the following steps: adding 1g of nano titanium dioxide and 0.05g of silane coupling agent KH-550 into 40mL of toluene, uniformly dispersing, reacting at 80 ℃ for 6h, centrifuging, washing and drying to obtain the nano titanium dioxide/silane coupling agent.
Example 2
Preparing a high-strength antibacterial melt-blown air filter material:
s1, uniformly mixing the coupling agent modified beta-cyclodextrin, the coupling agent modified nano titanium dioxide and polypropylene, and then performing melt extrusion granulation at the temperature of 260-280 ℃ by using a double-screw extruder to obtain modified polypropylene master batches, wherein the coupling agent modified beta-cyclodextrin accounts for 6% of the total weight of the modified polypropylene master batches, and the coupling agent modified nano titanium dioxide accounts for 1% of the total weight of the modified polypropylene master batches;
s2, mixing the modified polypropylene master batch and the polypropylene slices according to the weight ratio of 1: 5, uniformly mixing, adding the mixture into a melt-blowing device, melting the mixture at the temperature of 260-280 ℃, spraying the mixture through a spinneret at the temperature of 250 ℃ to form fibers, spraying beta-cyclodextrin on the surfaces of the formed fibers while spraying the mixture through the spinneret, cooling, stretching and shaping to obtain the base material of the melt-blown air filter material, wherein the weight ratio of the sum of the modified polypropylene master batches and the polypropylene slices to the beta-cyclodextrin is 100: 0.8;
s3, putting the melt-blown air filter material base material in an antibacterial finishing liquid, wherein the bath ratio is 1: and (5) carrying out padding treatment at the temperature of 70 ℃ and the rolling residual rate of 100%, and drying at the temperature of 90 ℃ to obtain the modified melt-blown air filter material base material, wherein the antibacterial finishing liquid is prepared by mixing 2% by mass of acetic acid solution of chitosan and epichlorohydrin in a volume ratio of 30: 1, the preparation method comprises the following steps: adding chitosan into an acetic acid solution with the mass fraction of 1% and stirring at 80 ℃ until the chitosan is completely dissolved to obtain an acetic acid solution of chitosan, adding epichlorohydrin, and stirring at 80 ℃ for 2 hours to obtain the chitosan-containing aqueous solution;
and S4, performing electret treatment on the modified melt-blown air filter material base material through a corona electret device, wherein the electret voltage is 20kV, and the electret distance is 4 cm.
The preparation method of the coupling agent modified beta-cyclodextrin comprises the following steps: adding 1g of beta-cyclodextrin and 0.15g of silane coupling agent KH-550 into 50mL of toluene for uniform dispersion, reacting at 90 ℃ for 12h, centrifuging, washing and drying to obtain the beta-cyclodextrin modified silane coupling agent; the preparation method of the coupling agent modified nano titanium dioxide comprises the following steps: adding 1g of nano titanium dioxide and 0.1g of silane coupling agent KH-550 into 40mL of toluene, uniformly dispersing, reacting at 100 ℃ for 12h, centrifuging, washing and drying to obtain the nano titanium dioxide/silane coupling agent.
Example 3
Preparing a high-strength antibacterial melt-blown air filter material:
s1, uniformly mixing the coupling agent modified beta-cyclodextrin, the coupling agent modified nano titanium dioxide and polypropylene, and then performing melt extrusion granulation at the temperature of 260-280 ℃ by using a double-screw extruder to obtain modified polypropylene master batches, wherein the coupling agent modified beta-cyclodextrin accounts for 4.5% of the total weight of the modified polypropylene master batches, and the coupling agent modified nano titanium dioxide accounts for 1.5% of the total weight of the modified polypropylene master batches;
s2, mixing the modified polypropylene master batch and the polypropylene slices according to the weight ratio of 1: 7, uniformly mixing, adding the mixture into a melt-blowing device, melting the mixture at the temperature of 260-280 ℃, spraying the mixture through a spinneret at the temperature of 245 ℃ to form fibers, spraying beta-cyclodextrin on the surfaces of the formed fibers while spraying the mixture through the spinneret, cooling, stretching and shaping to obtain the base material of the melt-blown air filter material, wherein the weight ratio of the sum of the modified polypropylene master batches and the polypropylene slices to the beta-cyclodextrin is 100: 0.5;
s3, putting the melt-blown air filter material base material in an antibacterial finishing liquid, wherein the bath ratio is 1: padding at the temperature of 60 ℃ and the rolling residual rate of 85%, and drying at the temperature of 80 ℃ to obtain the modified melt-blown air filter material base material, wherein the antibacterial finishing liquid is prepared by mixing 1.5% by mass of chitosan acetic acid solution and epichlorohydrin in a volume ratio of 25: 1, the preparation method comprises the following steps: adding chitosan into 0.5-1% acetic acid solution by mass percent, stirring at 60-80 ℃ until completely dissolving to obtain acetic acid solution of chitosan, adding epichlorohydrin, and stirring at 75 ℃ for 1h to obtain the chitosan acetate solution;
and S4, performing electret treatment on the modified melt-blown air filter material base material through a corona electret device, wherein the electret voltage is 10kV, and the electret distance is 3 cm.
The preparation method of the coupling agent modified beta-cyclodextrin comprises the following steps: adding 1g of beta-cyclodextrin and 0.1g of silane coupling agent KH-550 into 50mL of toluene for uniform dispersion, reacting at 80 ℃ for 10h, centrifuging, washing and drying to obtain the beta-cyclodextrin modified silane coupling agent; the preparation method of the coupling agent modified nano titanium dioxide comprises the following steps: adding 1g of nano titanium dioxide and 0.08g of silane coupling agent KH-550 into 40mL of toluene, uniformly dispersing, reacting at 90 ℃ for 10h, centrifuging, washing and drying to obtain the nano titanium dioxide/silane coupling agent KH-550.
Comparative example 1
Preparing a melt-blown air filter material:
s1, uniformly mixing the coupling agent modified nano titanium dioxide and polypropylene, and then performing melt extrusion granulation at the temperature of 260-280 ℃ through a double-screw extruder to obtain modified polypropylene master batches, wherein the coupling agent modified nano titanium dioxide accounts for 1.5% of the total weight of the modified polypropylene master batches;
s2, mixing the modified polypropylene master batch and the polypropylene slices according to the weight ratio of 1: 7, uniformly mixing, adding the mixture into melt-blowing equipment, melting the mixture at the temperature of 260-280 ℃, spraying the mixture through a spinneret at the temperature of 245 ℃ to form fibers, and cooling, stretching and shaping the fibers to obtain a melt-blown air filter material base material;
s3, putting the melt-blown air filter material base material in an antibacterial finishing liquid, wherein the bath ratio is 1: padding at the temperature of 60 ℃ and the rolling residual rate of 85%, and drying at the temperature of 80 ℃ to obtain the modified melt-blown air filter material base material, wherein the antibacterial finishing liquid is prepared by mixing 1.5% by mass of chitosan acetic acid solution and epichlorohydrin in a volume ratio of 25: 1, the preparation method comprises the following steps: adding chitosan into 0.5-1% acetic acid solution by mass percent, stirring at 60-80 ℃ until completely dissolving to obtain acetic acid solution of chitosan, adding epichlorohydrin, and stirring at 75 ℃ for 1h to obtain the chitosan acetate solution;
and S4, performing electret treatment on the modified melt-blown air filter material base material through a corona electret device, wherein the electret voltage is 10kV, and the electret distance is 3 cm.
The preparation method of the coupling agent modified nano titanium dioxide comprises the following steps: adding 1g of nano titanium dioxide and 0.08g of silane coupling agent KH-550 into 40mL of toluene, uniformly dispersing, reacting at 90 ℃ for 10h, centrifuging, washing and drying to obtain the nano titanium dioxide/silane coupling agent KH-550.
Comparative example 2
Preparing a high-strength antibacterial melt-blown air filter material:
s1, uniformly mixing the coupling agent modified beta-cyclodextrin, the coupling agent modified nano titanium dioxide and polypropylene, and then performing melt extrusion granulation at the temperature of 260-280 ℃ by using a double-screw extruder to obtain modified polypropylene master batches, wherein the coupling agent modified beta-cyclodextrin accounts for 4.5% of the total weight of the modified polypropylene master batches, and the coupling agent modified nano titanium dioxide accounts for 1.5% of the total weight of the modified polypropylene master batches;
s2, mixing the modified polypropylene master batch and the polypropylene slices according to the weight ratio of 1: 7, uniformly mixing, adding the mixture into melt-blowing equipment, melting the mixture at the temperature of 260-280 ℃, spraying the mixture through a spinneret at the temperature of 245 ℃ to form fibers, and cooling, stretching and shaping the fibers to obtain a melt-blown air filter material base material;
s3, putting the melt-blown air filter material base material in an antibacterial finishing liquid, wherein the bath ratio is 1: padding at the temperature of 60 ℃ and the rolling residual rate of 85%, and drying at the temperature of 80 ℃ to obtain the modified melt-blown air filter material base material, wherein the antibacterial finishing liquid is prepared by mixing 1.5% by mass of chitosan acetic acid solution and epichlorohydrin in a volume ratio of 25: 1, the preparation method comprises the following steps: adding chitosan into 0.5-1% acetic acid solution by mass percent, stirring at 60-80 ℃ until completely dissolving to obtain acetic acid solution of chitosan, adding epichlorohydrin, and stirring at 75 ℃ for 1h to obtain the chitosan acetate solution;
and S4, performing electret treatment on the modified melt-blown air filter material base material through a corona electret device, wherein the electret voltage is 10kV, and the electret distance is 3 cm.
The preparation method of the coupling agent modified beta-cyclodextrin comprises the following steps: adding 1g of beta-cyclodextrin and 0.1g of silane coupling agent KH-550 into 50mL of toluene for uniform dispersion, reacting at 80 ℃ for 10h, centrifuging, washing and drying to obtain the beta-cyclodextrin modified silane coupling agent; the preparation method of the coupling agent modified nano titanium dioxide comprises the following steps: adding 1g of nano titanium dioxide and 0.08g of silane coupling agent KH-550 into 40mL of toluene, uniformly dispersing, reacting at 90 ℃ for 10h, centrifuging, washing and drying to obtain the nano titanium dioxide/silane coupling agent KH-550.
The melt-blown air filter materials prepared in the embodiment 3 and the comparative examples 1-2 are tested for mechanical property and filter performance, wherein the filter efficiency and the resistance are tested according to the method of GB2626-2006, and the test flow is 32L/min; the results are shown in table 1:
TABLE 1 mechanical Properties of melt blown air filtration materials and Filter Performance test results
Test items | Example 3 | Comparative example 1 | Comparative example 2 |
0.3 μm filtration efficiency (%) | 97.1 | 95.2 | 94.8 |
Resistance (Pa) | 2.2 | 5.7 | 3.4 |
Elongation at Break in longitudinal direction (%) | 27.5 | 21.4 | 23.0 |
Transverse elongation at Break (%) | 40.2 | 29.6 | 32.8 |
The antibacterial performance test of the melt-blown air filter materials prepared in example 3 and comparative examples 1-2 is carried out according to GB/T20944-:
TABLE 2 antibacterial Performance test results for melt blown air filter materials
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A preparation method of a high-strength antibacterial melt-blown air filter material is characterized by comprising the following steps:
s1, uniformly mixing the coupling agent modified beta-cyclodextrin, the coupling agent modified nano titanium dioxide and polypropylene, and then carrying out melt extrusion granulation by a double-screw extruder to obtain modified polypropylene master batches;
s2, uniformly mixing the modified polypropylene master batches and polypropylene slices, adding the mixture into melt-blown equipment, spraying the mixture through a spinneret to form fibers after the mixture is melted, spraying beta-cyclodextrin on the surfaces of the formed fibers while spraying the fibers through the spinneret, and cooling, stretching and shaping the fibers to obtain a melt-blown air filter material base material;
s3, padding and drying the melt-blown air filter material base material in an antibacterial finishing liquid to obtain a modified melt-blown air filter material base material, wherein the antibacterial finishing liquid is prepared by mixing an acetic acid solution of chitosan and epichlorohydrin;
and S4, performing electret treatment on the modified melt-blown air filter material base material through a corona electret device.
2. The preparation method of the high-strength antibacterial melt-blown air filter material as claimed in claim 1, wherein the coupling agent modified beta-cyclodextrin is prepared by modifying beta-cyclodextrin with a coupling agent, and the coupling agent modified nano titanium dioxide is prepared by modifying nano titanium dioxide with a coupling agent; the coupling agent is a silane coupling agent or a titanate coupling agent.
3. The preparation method of the high-strength antibacterial melt-blown air filter material according to claim 1 or 2, wherein the coupling agent modified beta-cyclodextrin accounts for 3-6% of the total weight of the modified polypropylene master batch, and the coupling agent modified nano titanium dioxide accounts for 1-2% of the total weight of the modified polypropylene master batch.
4. The preparation method of the high-strength antibacterial melt-blown air filter material as claimed in any one of claims 1 to 3, wherein the weight ratio of the modified polypropylene master batch to the polypropylene chips is 1: (5-8).
5. The preparation method of the high-strength antibacterial melt-blown air filter material according to any one of claims 1 to 4, wherein in the step S2, the weight ratio of the sum of the weight of the modified polypropylene master batch and the weight of the polypropylene slices to the weight of the beta-cyclodextrin is 100: (0.3-0.8).
6. The preparation method of the high-strength bacteriostatic melt-blown air filter material according to any one of claims 1 to 5, wherein the antibacterial finishing liquid is prepared by mixing 1 to 2 mass percent of acetic acid solution of chitosan and epichlorohydrin according to a volume ratio of (20 to 30): 1, mixing and preparing.
7. The method for preparing a high-strength antibacterial melt-blown air filter material according to any one of claims 1 to 6, wherein in the step S3, the bath ratio of the padding treatment is 1: (40-80) and the rolling allowance is 80-100%.
8. A high-strength bacteriostatic melt-blown air filter material, which is prepared by the preparation method of any one of claims 1 to 7.
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