CN105148875A - Preparing method of easy-to-recover and recyclable polyaniline loading polyurethane sponge adsorption material - Google Patents
Preparing method of easy-to-recover and recyclable polyaniline loading polyurethane sponge adsorption material Download PDFInfo
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- CN105148875A CN105148875A CN201510551055.6A CN201510551055A CN105148875A CN 105148875 A CN105148875 A CN 105148875A CN 201510551055 A CN201510551055 A CN 201510551055A CN 105148875 A CN105148875 A CN 105148875A
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Abstract
The invention discloses a preparing method of an easy-to-recover and recyclable polyaniline loading polyurethane sponge adsorption material. The method comprises the steps of taking commercial polyurethane sponge as a carrier, firstly immersing the carrier in a mixed solution of carbon nanotubes and water for ultrasonic treatment to obtain the carbon nanotube-modified polyurethane sponge, and then performing in situ polymerization on a polyurethane sponge skeleton by aniline monomers to obtain the polyaniline loading polyurethane sponge adsorption material. The polyurethane sponge is taken as the carrier, the polyaniline loading polyurethane sponge is obtained in one step by the in situ polymerization on the carbon nanotube-modified polyurethane sponge skeleton, the preparing method is simple and convenient, and low in cost, the polyaniline loading polyurethane sponge has a three dimensional porous structure, is large in specific area, had characteristics of elasticity of the carrier, light weight and easiness in separation, has a well adsorption effect for organic dye, and realizes full separation of an adsorbate and the adsorbent, and recycle of materials by a manner of extruding the materials by external force.
Description
Technical field
The present invention relates to a kind of preparation method of Polyaniline-Supported polyurethane sponge sorbing material.
Background technology
In recent years, absorption method, as a kind of physico-chemical process of simple to operate, easy to use, wide accommodation, obtains investigation and application widely in field of waste water treatment.Traditional industrial high-efficient adsorbent also exists that price is high, the not easily problem such as recovery, limits its extensive use.Polyurethane sponge has three-dimensional cavernous structure, and the carrier as sorbing material effectively can improve the specific area of material, and lightening material density has played important effect in sorbing material field.
Summary of the invention
In order to solve the problem that existing sorbing material not easily reclaims, cost is high, the invention provides the preparation method of the Polyaniline-Supported polyurethane sponge sorbing material that a kind of easy recovery can be recycled, adopt eco-friendly synthesis mode, without the need to the severe corrosive such as chromium trioxide, concentrated sulfuric acid reagent pretreatment sponge, reaction condition is gentle, method is easy, can be used for organic dyestuff process field.
The object of the invention is to be achieved through the following technical solutions:
The preparation method of the Polyaniline-Supported polyurethane sponge sorbing material that a kind of easy recovery can be recycled, with commercial polyurethane sponge for carrier, first carrier is dipped in ultrasonic process in the mixed solution of CNT and water, obtain the polyurethane sponge of carbon nano-tube modification, again by the in-situ polymerization of aniline monomer on polyurethane sponge skeleton, obtain Polyaniline-Supported polyurethane sponge composite.Concrete steps are as follows:
One, polyurethane sponge is cut into fritter, is positioned over ultrasonic process 1 ~ 2h in distilled water and alcohol solvent respectively, then dries under 40 ~ 60 DEG C of conditions and is cut into the regular cuboid that quality is 0.1 ~ 0.2g; Wherein, ultrasonic power is 180W.
Two, CNT 0.2 ~ 0.4g is scattered in the distilled water of 1000mL, disperses 3 ~ 5h under ultrasound condition, obtain the mixture of carbon nanotube dispersed in water; Wherein, CNT is functionalized multi-wall carbonnanotubes, and diameter is 10-20nm.
Three, the polyurethane sponge that step one obtains is immersed in the CNT of step 2 and the mixture of water, by the mode of extruding, the mixture of CNT and water is drawn in sponge, more ultrasonic process 1.5 ~ 3h; Then the polyurethane sponge tweezers having adsorbed CNT are taken out, be placed in the dry 8 ~ 16h of 60 ~ 80 DEG C of baking ovens, obtain the polyurethane sponge of carbon nano-tube modification; Wherein, the volume of the mixture of CNT and water is 500mL.
Four, prepare the aqueous solution of aniline by the amount ratio of aniline and water 0.9 ~ 6mL:328.5mL, the pH value regulating solution is 1 ~ 3; Prepare ammonium persulfate aqueous solution by the amount ratio of ammonium persulfate and water 2.1 ~ 14g:300mL, the pH value regulating solution is 1 ~ 3; Wherein, for regulating the solution of pH to be hydrochloric acid or sulfuric acid.
Five, the aniline-water solution that step 4 obtains is placed in there-necked flask, under the condition of ice bath of 0 ~ 10 DEG C, mechanical agitation is even, dropwise adds the ammonium persulfate aqueous solution described in step 4, dropwises rear Keep agitation 1 ~ 15min; Wherein, the volume of aniline-water solution is 36 ~ 65mL, and the volume of ammonium persulfate aqueous solution is 36 ~ 65mL, and aniline monomer is 1:0.8 ~ 1.5 with the amount of substance ratio of ammonium persulfate.
The polyurethane sponge composite of the carbon nano-tube modification six, step 3 obtained is immersed in the mixed solution that step 5 obtains, and makes sponge absorb mixed solution, then mixture is stirred 3 ~ 8h under the condition of 0 ~ 10 DEG C by extruding; Wherein, the polyurethane sponge of carbon nano-tube modification and the mass ratio of aniline monomer are 1 ~ 24:1.
Seven, take out the solid formation in step 6, squeeze out unnecessary liquid and clarify to filtrate with distilled water and the washing of ethanol alternate immersion, forced air drying 8 ~ 20h under 40 ~ 60 DEG C of conditions, obtains Polyaniline-Supported polyurethane sponge sorbing material.
Tool of the present invention has the following advantages:
1, the present invention adopts polyurethane sponge to be carrier, and by the in-situ polymerization of aniline monomer on the polyurethane sponge skeleton of carbon nano-tube modification, single step reaction obtains Polyaniline-Supported polyurethane sponge, and preparation method is easy, and cost is low.
2, the Polyaniline-Supported polyurethane sponge that prepared by the present invention has three-dimensional cavernous structure, and specific area is large, has good adsorption effect to organic dyestuff.
3, the Polyaniline-Supported polyurethane sponge that prepared by the present invention has the absorption property of polyaniline to organic dyestuff, have the elasticity of carrier, the segregative characteristic of lightweight simultaneously concurrently, adsorbate can be realized by the mode of external force extrded material and be separated fully with adsorbent and the recycling of material.
Accompanying drawing explanation
Fig. 1 is the photo in kind of the Polyaniline-Supported polyurethane sponge sorbing material that in detailed description of the invention one, step 7 obtains;
Fig. 2 is the photo in kind of the Polyaniline-Supported polyurethane sponge sorbing material that in detailed description of the invention two, step 7 obtains.
Detailed description of the invention
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described; but be not limited thereto; everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Detailed description of the invention one: the preparation method of the Polyaniline-Supported polyurethane sponge sorbing material that present embodiment provides carries out according to the following steps:
One, polyurethane sponge is cut into fritter, is positioned over ultrasonic process 1h in distilled water and alcohol solvent respectively, then dries under 60 DEG C of conditions and is cut into the regular cuboid that quality is 0.1g.
Two, be that the functionalized multi-wall carbonnanotubes 0.25g of 10 ~ 20nm is scattered in the distilled water of 1000mL by diameter, disperse 3h under ultrasound condition, obtain the mixture of carbon nanotube dispersed in water.
Three, the polyurethane sponge that step one obtains is immersed in the mixture of CNT water of step 2, by the mode of extruding, the mixture of CNT and water is drawn in sponge, more ultrasonic process 2h.Then the polyurethane sponge tweezers having adsorbed CNT are taken out, be placed in 60 DEG C of dry 8h of baking oven, obtain the polyurethane sponge of carbon nano-tube modification.Wherein, CNT aqueous mixtures volume is 500mL.
Four, prepare the aqueous solution of aniline by the amount ratio of aniline and water 6mL:328.5mL, the pH value regulating solution is 1.5.Prepare ammonium persulfate aqueous solution by the amount ratio of ammonium persulfate and water 14g:300mL, the pH value regulating solution is 1.5.Wherein, for regulating the solution of pH to be hydrochloric acid.
Five, the aniline-water solution that step 4 obtains is placed in there-necked flask, under the condition of ice bath of 4 ~ 6 DEG C, mechanical agitation is even, dropwise adds the ammonium persulfate aqueous solution described in step 4, dropwises rear Keep agitation 1min; Wherein, the volume of aniline-water solution is 65mL, and the volume of ammonium persulfate aqueous solution is 65mL.
The polyurethane sponge composite of the carbon nano-tube modification six, step 3 obtained is immersed in the mixed solution that step 5 obtains, and makes sponge absorb mixed solution, then mixture is stirred 6h under the condition of 4 ~ 6 DEG C by extruding; Wherein, the polyurethane sponge of carbon nano-tube modification and the mass ratio of aniline monomer are 24:1.
Seven, take out the solid formation in step 6, squeeze out unnecessary liquid and clarify to filtrate with distilled water and the washing of ethanol alternate immersion, forced air drying 15h under 60 DEG C of conditions, obtains Polyaniline-Supported polyurethane sponge sorbing material (Fig. 1).
The preparation method of the Polyaniline-Supported polyurethane sponge sorbing material of present embodiment, with commercial polyurethane sponge for carrier, by the in-situ polymerization of aniline monomer on the polyurethane sponge skeleton of carbon nano-tube modification, obtain Polyaniline-Supported polyurethane sponge sorbing material.The Polyaniline-Supported polyurethane sponge of present embodiment adopts eco-friendly synthesis mode, and without the need to the pretreatment of the severe corrosive such as chromium trioxide, concentrated sulfuric acid reagent, reaction condition is gentle, and single step reaction can obtain Polyaniline-Supported polyurethane sponge sorbing material.The Polyaniline-Supported polyurethane sponge of present embodiment has high-specific surface area, elasticity, lightweight, easily reclaims the characteristic be separated.
Get Polyaniline-Supported polyurethane sponge sorbing material prepared by present embodiment for adsorption test, adsorbent is Polyaniline-Supported polyurethane sponge sorbing material, the methyl blue solution of adsorbate to be concentration be 10mg/L.30mL adsorbent solution is divided and adsorbs for three times, in each adsorption process, the amount ratio of adsorbate and adsorbent is 10mg:10mL, concussion absorption 1h under the condition of 25 DEG C, solution in Polyaniline-Supported polyurethane sponge sorbing material is discharged by the mode extruded by external force after having adsorbed, and carries out absorption next time.Test result shows, under this adsorption conditions, Polyaniline-Supported polyurethane sponge adsorption effect prepared by present embodiment is obvious, and adsorption rate can reach 80%.
Detailed description of the invention two: the preparation method of the Polyaniline-Supported polyurethane sponge sorbing material that present embodiment provides carries out according to the following steps:
One, polyurethane sponge is cut into fritter, is positioned over ultrasonic process 1h in distilled water and alcohol solvent respectively, then dries under 40 DEG C of conditions and be cut into the cuboid that quality is 0.1g; Wherein, ultrasonic power is 180W.
Two, be that the functionalized multi-wall carbonnanotubes 0.25g of 10 ~ 20nm is scattered in the distilled water of 1000mL by diameter, disperse 3h under ultrasound condition, obtain the mixture of carbon nanotube dispersed in water.
Three, the polyurethane sponge that step one obtains is immersed in the mixture of CNT water of step 2.By the mode of extruding, the mixture of CNT and water is drawn in sponge, more ultrasonic process 2h.Then the polyurethane sponge tweezers having adsorbed CNT are taken out, be placed in 80 DEG C of dry 10h of baking oven, obtain the polyurethane sponge of carbon nano-tube modification.Wherein, CNT aqueous mixtures volume is 500mL.
Four, prepare the aqueous solution of aniline by the amount ratio of aniline and water 0.9mL:328.5mL, the pH value regulating solution is 1.5.Prepare ammonium persulfate aqueous solution by the amount ratio of ammonium persulfate and water 2.1g:300mL, the pH value regulating solution is 1.5.Wherein, for regulating the solution of pH to be hydrochloric acid;
Five, the aniline-water solution that step 4 obtains is placed in there-necked flask, under the condition of ice bath of 2 ~ 8 DEG C, mechanical agitation is even, dropwise adds the ammonium persulfate aqueous solution described in step 4, dropwises rear Keep agitation 15min; Wherein, the volume of aniline-water solution is 36mL, and the volume of ammonium persulfate aqueous solution is 36mL.
The polyurethane sponge composite of the carbon nano-tube modification six, step 3 obtained is immersed in the mixed solution that step 5 obtains, and makes sponge absorb mixed solution, then mixture is stirred 6h under the condition of 2 ~ 8 DEG C by extruding; Wherein, the polyurethane sponge of carbon nano-tube modification and the mass ratio of aniline monomer are 1:1.
Seven, take out the solid formation in step 6, squeeze out unnecessary liquid and clarify to filtrate with distilled water and the washing of ethanol alternate immersion, forced air drying 20h under 40 DEG C of conditions, obtains Polyaniline-Supported polyurethane sponge sorbing material (Fig. 2).
Claims (8)
1. easily reclaim a preparation method for the Polyaniline-Supported polyurethane sponge sorbing material that can be recycled, it is characterized in that described preparation method is as follows:
One, polyurethane sponge is cut into fritter, is positioned over ultrasonic process 1 ~ 2h in distilled water and alcohol solvent respectively, then dries under 40 ~ 60 DEG C of conditions and is cut into the regular cuboid that quality is 0.1 ~ 0.2g;
Two, CNT 0.2 ~ 0.4g is scattered in the distilled water of 1000mL, disperses 3 ~ 5h under ultrasound condition, obtain the mixture of carbon nanotube dispersed in water;
Three, the polyurethane sponge that step one obtains is immersed in the CNT of step 2 and the mixture of water, by the mode of extruding, the mixture of CNT and water is drawn in sponge, more ultrasonic process 1.5 ~ 3h; Then the polyurethane sponge tweezers having adsorbed CNT are taken out, be placed in the dry 8 ~ 16h of 60 ~ 80 DEG C of baking ovens, obtain the polyurethane sponge of carbon nano-tube modification;
Four, prepare the aqueous solution of aniline by the amount ratio of aniline and water 0.9 ~ 6mL:328.5mL, the pH value regulating solution is 1 ~ 3; Prepare ammonium persulfate aqueous solution by the amount ratio of ammonium persulfate and water 2.1 ~ 14g:300mL, the pH value regulating solution is 1 ~ 3;
Five, the aniline-water solution that step 4 obtains is placed in there-necked flask, under the condition of ice bath of 0 ~ 10 DEG C, mechanical agitation is even, dropwise adds the ammonium persulfate aqueous solution described in step 4, dropwises rear Keep agitation 1 ~ 15min;
The polyurethane sponge composite of the carbon nano-tube modification six, step 3 obtained is immersed in the mixed solution that step 5 obtains, and makes sponge absorb mixed solution, then mixture is stirred 3 ~ 8h under the condition of 0 ~ 10 DEG C by extruding;
Seven, take out the solid formation in step 6, squeeze out unnecessary liquid and clarify to filtrate with distilled water and the washing of ethanol alternate immersion, forced air drying 8 ~ 20h under 40 ~ 60 DEG C of conditions, obtains Polyaniline-Supported polyurethane sponge sorbing material.
2. the preparation method of Polyaniline-Supported polyurethane sponge sorbing material that can be recycled of easy recovery according to claim 1, it is characterized in that in described step one, ultrasonic power is 180W.
3. the preparation method of Polyaniline-Supported polyurethane sponge sorbing material that can be recycled of easy recovery according to claim 1, it is characterized in that in described step 2, CNT is functionalized multi-wall carbonnanotubes.
4. the preparation method of the Polyaniline-Supported polyurethane sponge sorbing material that the easy recovery according to claim 1 or 3 can be recycled, is characterized in that the diameter of described CNT is 10-20nm.
5. the preparation method of Polyaniline-Supported polyurethane sponge sorbing material that can be recycled of easy recovery according to claim 1, it is characterized in that in described step 3, the volume of the mixture of CNT and water is 500mL.
6. the preparation method of Polyaniline-Supported polyurethane sponge sorbing material that can be recycled of easy recovery according to claim 1, it is characterized in that in described step 4, is hydrochloric acid or sulfuric acid for regulating the solution of pH.
7. the preparation method of Polyaniline-Supported polyurethane sponge sorbing material that can be recycled of easy recovery according to claim 1, is characterized in that in described step 5, and the amount of substance of aniline monomer and ammonium persulfate is than being 1:0.8 ~ 1.5.
8. the preparation method of Polyaniline-Supported polyurethane sponge sorbing material that can be recycled of easy recovery according to claim 1, it is characterized in that in described step 6, the polyurethane sponge of carbon nano-tube modification and the mass ratio of aniline monomer are 1 ~ 24:1.
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| CN111569843A (en) * | 2020-04-22 | 2020-08-25 | 湖南大学 | Material for treating diclofenac wastewater and preparation method and application thereof |
| CN114984903A (en) * | 2022-05-23 | 2022-09-02 | 中南大学 | Calcium-magnesium-aluminum ternary fluoride loaded polyurethane sponge and preparation method and application thereof |
| CN115304121A (en) * | 2022-06-27 | 2022-11-08 | 河海大学 | Preparation method and application of polyaniline-wood double-layer evaporation material |
| CN115554999A (en) * | 2022-09-27 | 2023-01-03 | 南京大学 | Synthetic method and application of aminated polyurethane sponge adsorbent |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108899498A (en) * | 2018-06-26 | 2018-11-27 | 宁波革创新材料科技有限公司 | The preparation method of environmental protection flexible lithium ion cell positive framework material |
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| CN115554999A (en) * | 2022-09-27 | 2023-01-03 | 南京大学 | Synthetic method and application of aminated polyurethane sponge adsorbent |
| CN115554999B (en) * | 2022-09-27 | 2024-03-19 | 南京大学 | Synthesis method and application of aminated polyurethane sponge adsorbent |
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