CN104086710A - Preparation method for modified nano cotton oil-absorption material - Google Patents
Preparation method for modified nano cotton oil-absorption material Download PDFInfo
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- CN104086710A CN104086710A CN201410331109.3A CN201410331109A CN104086710A CN 104086710 A CN104086710 A CN 104086710A CN 201410331109 A CN201410331109 A CN 201410331109A CN 104086710 A CN104086710 A CN 104086710A
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Abstract
The invention relates to a preparation method for a modified nano cotton oil-absorption material capable of continuously and selectively absorbing oil. The preparation method comprises the following steps of (1), adding water and polyvinyl alcohol in a reaction container, heating and stirring, so that the polyvinyl alcohol is completely dissolved, and adding block-shaped nano cotton; (2), heating in water bath, adding monomer butyl acrylate, benzoyl peroxide and N, N- methylene bisacrylamide after temperature is stabilized, and stirring and reacting; and (3), after the reaction is ended, taking out modified nano cotton, washing by water, drying in vacuum until weight is constant. The preparation method disclosed by the invention has the advantages that (1), nano cotton with high internal porosity is selected as a reaction base body, so that the modified oil absorption material has good oil retaining ability; (2), the modifying method is simple to operate, and reaction conditions are gentle; (3), the oil absorption selectivity of the modified nano cotton is obviously improved, and the oil can be continuously adsorbed after the modified nano cotton is connected with a vacuum device.
Description
Technical field
The invention belongs to oil absorption material and environmental protection technical field, relate to a kind of preparation method of the cotton oil absorption material of modified Nano that can continue selectivity oil suction.
Background technology
In recent years, the pollution that the crude oil leakage of ocean causes has been considered to a large environmental problem in worldwide.Disadvantageous effect for fear of crude oil leakage to the ecosystem and the long-term hazards of greasy dirt, be necessary to develop the material that can effectively clear up greasy dirt.Traditional synthetic oil absorption material is mainly polyacrylate(s) high oil absorbing resin, and this class oil-absorbing resin oil absorbency is high, but has the saturated problem of oil suction, can not recycle continue oil suction.
In the last few years, the research that increasing investigators have invested oil suction foam sight comes up, but mostly concentrate in polyurethane foam, such as Wang Chi peak etc. utilizes carbon nanotube and polydimethylsiloxane to adopt dip coating to carry out modification to polyurethane foam, obviously improve the oil suction selectivity of polyurethane foam, simultaneously, in polyurethane foam, connect oil contaminants (the Wang C F that vacuum extractor can the continuous absorption water surface, Lin S J.Robust superhydrophobic/superoleophilic sponge for effective continuous absorption and expulsion of oil pollutants from water.ACS Applied materials and interfaces, 2013, 5:8861-8864), Zhou little Yan etc. utilize pyrroles's vapor deposition polymerization method, make pyrroles at polyurethane foam surface aggregate, thereby improve oil absorptiveness (the Zhou X Y of polyurethane foam, Zhang Z Z, et al.Facile Fabrication of superhydrophobic sponge with selective absorption and collection of oil from water.Industrial and engineering chemistry research.2013,52:9411-9416), the people such as Liu Lifen are using polyurethane foam as reactive matrix, there is the polyreaction of acrylate, thus in the oil absorptiveness that has improved polyurethane foam, make polyurethane foam oil suction repeatedly (Liu Lifen. a kind of preparation method of modified polyurethane foam oil absorption material. Chinese invention patent .201110415527.7.2013-6-5).The work report of preparing oil absorption material as matrix about nanometer cotton (trimeric cyanamide sponge) is less.
Summary of the invention
The object of the present invention is to provide the preparation method of the cotton oil absorption material of a kind of modified Nano, in order to promote its oil suction selectivity.
Of the present invention to solve the problems of the technologies described above adopted technical scheme as follows: the preparation method of the cotton oil absorption material of a kind of modified Nano, includes following steps:
1) in reaction vessel, add water and polyvinyl alcohol, heat up and stir, polyvinyl alcohol is dissolved completely, add lumpy nanometer cotton;
2) warming-in-water adds monomer butyl acrylate, benzoyl peroxide, N,N methylene bis acrylamide, stirring reaction after temperature-stable;
3) after reaction finishes, take out modified Nano cotton, wash with water, vacuum-drying is to constant weight.
Press such scheme, step 2) described warming-in-water is 80～90 DEG C, churning time is 4～10h.
Press such scheme, the volume of described monomer butyl acrylate is volume of water used 10%～50%.
Press such scheme, described polyvinyl alcohol consumption is 1%～15% of monomer butyl acrylate quality.
Press such scheme, described benzoyl peroxide consumption is 1%～5% of monomer butyl acrylate quality.
Press such scheme, described N,N methylene bis acrylamide consumption is 1%～5% of monomer butyl acrylate quality.
Press such scheme, the consumption of described nanometer cotton is 1%～10% of monomer butyl acrylate quality.
Reaction mechanism of the present invention: the present invention is taking nanometer cotton as matrix, by butyl acrylate and be crosslinking in nanometer cotton, makes this material possess super oil absorbency and good oil suction selectivity by suspension polymerization, can preferential adsorbed oil and non-planar water at water-oil interface; Utilize the loose and porous structure of nanometer cotton simultaneously, can realize the lasting oil suction on water-oil interface by connecting vacuum absorption device.
The present invention has following advantage:
1) select nanometer cotton that wood interior porosity is high as reactive matrix, make the oil absorption material after modification there is good oil-retaining;
2) method of modifying is simple to operate, reaction conditions gentleness;
3) the oil suction selectivity of the nanometer cotton after modification is obviously promoted, and modified Nano cotton can continue oil suction after connection vacuum unit.
Brief description of the drawings
Fig. 1 is the optical microscope image of unmodified nanometer cotton and embodiment 1 modified Nano cotton;
Fig. 2 is the surface wettability experimental image of unmodified nanometer cotton and embodiment 1 modified Nano cotton;
Fig. 3 is taking cyclohexane give as representing the selection oil absorbency experimentation of solvent embodiment 1 modified Nano cotton;
Fig. 4 is taking cyclohexane give as representing the cotton lasting oil suction experimentation connecting after vacuum pump of solvent embodiment 1 modified Nano.
Embodiment
Below by embodiment, the present invention will be further described in detail, and material used in the present invention, reagent etc. if no special instructions, obtain in all can be from commercial channels.
Embodiment 1
In reaction vessel, add 50mL water and 0.675g polyvinyl alcohol, temperature is risen to approximately 60 DEG C of stirrings, polyvinyl alcohol is dissolved completely.Add the cotton also stirring of 0.45g lumpy nanometer.Temperature is risen to 80 DEG C, add 5mL (4.5g) butyl acrylate, 0.225g benzoyl peroxide, 0.2g N,N methylene bis acrylamide after temperature-stable, stirring reaction 6h stops.Take out product and wash with water for several times, vacuum-drying is to constant weight.
As shown in Figure 1, left figure is the optical microscope image of blank nanometer cotton, and nanometer cotton is the reticulated structure of porous.Right figure is the optical microscope image of modified Nano cotton, can see in reticulated structure and have some polyacrylic ester oil-absorbing resin particles, makes retaining cotton porous its oil absorptiveness and the oil suction selectivity of simultaneously having improved of nanometer; As shown in Figure 2, two cubic blocks in figure, the left side is unmodified nanometer cotton, the right is modified Nano cotton.Drip water on the cotton surface of nanometer, the globule on unmodified nanometer cotton rapidly disappears because being inhaled in nanometer cotton, and can keep spherical at the cotton surface water drops of modified Nano, and 10min also changes little later.Nanometer cotton after modification is compared to unmodified nanometer cotton, and its hydrophobicity is significantly improved; As shown in Figure 3, in beaker, add the hexanaphthene (upper strata of certain water gaging and Sudan red III mark, aobvious red), immerse in this mixed system cotton modified Nano, can observe gradually hexanaphthene layer height reduces until disappear, and water layer height does not change substantially, nanometer cotton all reddens.Modified Nano cotton is in the first oil suction of oil mixing with water interfacial energy selectivity as can be seen here; As shown in Figure 4, the present invention taking nanometer cotton the nanometer cotton after matrix modification in oil-water mixing system, can preferentially select oil suction, and nanometer cotton has certain compressibility, modified Nano cotton is connected to vacuum absorption device by Glass tubing, and nanometer cotton is placed on the hexanaphthene interface that water and Sudan red III mark cross, after vacuum pump is opened, can be observed hexanaphthene and preferentially absorbed and be pumped in Glass tubing by nanometer cotton.This illustrates this material except having certain oil storage capacity, also has the ability of lasting oil suction.
Embodiment 2
In reactor, add 50mL water and 1g polyvinyl alcohol, temperature is risen to approximately 60 DEG C of stirrings, polyvinyl alcohol is dissolved completely.Add the cotton also stirring of 0.55g lumpy nanometer.Temperature is risen to 85 DEG C, add 10mL (9g) butyl acrylate, 0.18g benzoyl peroxide, 0.45g N,N methylene bis acrylamide after temperature-stable, stirring reaction 4h stops.Take out product and wash with water for several times, vacuum-drying is to constant weight.
Embodiment 3
In reactor, add 50mL water and 1g polyvinyl alcohol, temperature is risen to approximately 60 DEG C of stirrings, polyvinyl alcohol is dissolved completely.Add the cotton also stirring of 0.3g lumpy nanometer.Temperature is risen to 90 DEG C, add 15mL (13.5g) butyl acrylate, 0.27g benzoyl peroxide, 0.135g N,N methylene bis acrylamide after temperature-stable, stirring reaction 8h stops.Take out product and wash with water for several times, vacuum-drying is to constant weight.
Embodiment 4
In reactor, add 50mL water and 0.3g polyvinyl alcohol, temperature is risen to approximately 60 DEG C of stirrings, polyvinyl alcohol is dissolved completely.Add the cotton also stirring of 0.45g lumpy nanometer.Temperature is risen to 85 DEG C, add 20mL (18g) butyl acrylate, 0.18g benzoyl peroxide, 0.45g N,N methylene bis acrylamide after temperature-stable, stirring reaction 10h stops.Take out product and wash with water for several times, vacuum-drying is to constant weight.
Embodiment 5
In reactor, add 50mL water and 0.225g polyvinyl alcohol, temperature is risen to approximately 60 DEG C of stirrings, polyvinyl alcohol is dissolved completely.Add the cotton also stirring of 0.225g lumpy nanometer.Temperature is risen to 80 DEG C, add 25mL (22.5g) butyl acrylate, 0.3g benzoyl peroxide, 0.3g N,N methylene bis acrylamide after temperature-stable, stirring reaction 6h stops.Take out product and wash with water for several times, vacuum-drying is to constant weight.
Above embodiment passes through the microstructure change after the cotton modification of observation by light microscope nanometer; Meanwhile, selection oil absorbency and the lasting oil absorbency of modified Nano cotton have been measured taking cyclohexane give as representing solvent.
Claims (7)
1. a preparation method for the cotton oil absorption material of modified Nano, includes following steps:
1) in reaction vessel, add water and polyvinyl alcohol, heat up and stir, polyvinyl alcohol is dissolved completely, add lumpy nanometer cotton;
2) warming-in-water adds monomer butyl acrylate, benzoyl peroxide, N,N methylene bis acrylamide, stirring reaction after temperature-stable;
3) after reaction finishes, take out modified Nano cotton, wash with water, vacuum-drying is to constant weight.
2. the cotton oil absorption material preparation method of modified Nano according to claim 1, is characterized in that step 2) described warming-in-water is 80～90 DEG C, churning time is 4～10h.
3. the cotton oil absorption material preparation method of modified Nano according to claim 1 and 2, is characterized in that, the volume of described monomer butyl acrylate is volume of water used 10%～50%.
4. the cotton oil absorption material preparation method of modified Nano according to claim 1 and 2, is characterized in that, described polyvinyl alcohol consumption is 1%～15% of monomer butyl acrylate quality.
5. the cotton oil absorption material preparation method of modified Nano according to claim 1 and 2, is characterized in that, described benzoyl peroxide consumption is 1%～5% of monomer butyl acrylate quality.
6. the cotton oil absorption material preparation method of modified Nano according to claim 1 and 2, is characterized in that, described N,N methylene bis acrylamide consumption is 1%～5% of monomer butyl acrylate quality.
7. the cotton oil absorption material preparation method of modified Nano according to claim 1 and 2, is characterized in that, the consumption of described nanometer cotton is 1%～10% of monomer butyl acrylate quality.
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| CN104526095A (en) * | 2014-12-25 | 2015-04-22 | 佛山市大铁数控机械有限公司 | Wire cutting machine working solution activated-carbon nanometer multi-layer filtering water tank |
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| CN102874792A (en) * | 2012-10-23 | 2013-01-16 | 江西师范大学 | Preparation method of novel carbon sponge |
| CN103276707B (en) * | 2013-05-14 | 2015-03-25 | 中国科学技术大学 | Floating oil collecting device, manufacturing method thereof and applications thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104526095A (en) * | 2014-12-25 | 2015-04-22 | 佛山市大铁数控机械有限公司 | Wire cutting machine working solution activated-carbon nanometer multi-layer filtering water tank |
| CN104526095B (en) * | 2014-12-25 | 2017-08-08 | 广东大铁数控机械有限公司 | A kind of activated carbon of working liquid for wire-cutting machine, nano multilayer water tank with strainer |
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