CN105214630A - A kind of preparation method of super-hydrophobic magnetic polyurethane/ferriferrous oxide composite material - Google Patents
A kind of preparation method of super-hydrophobic magnetic polyurethane/ferriferrous oxide composite material Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of super-hydrophobic magnetic polyurethane/ferriferrous oxide composite material, belong to material modified field.The present invention is directed to bionical interface water-oil separating materials adsorption ability poor, large-area water-oil separating recovery cannot be realized and sorbing material cannot reusable drawback, be matrix by polyurethane sponge, dopamine fixes the method for ferriferrous oxide particles and lauryl mercaptan, construct micro nano structure at sponge surface and introduce low-surface energy substance, preparation has the sponge composite of super-hydrophobic and super oil-wet behavior.Make that composite has high oil absorption, Selective Separation oil water mixture, oil product fast reclaim and the performance of closed matereial cycle.
Description
Technical field
The present invention relates to a kind of preparation method of super-hydrophobic magnetic polyurethane/ferriferrous oxide composite material, belong to material modified field.
Background technology
In modern society, economic fast development produces in a large number by the industry water resource of Organic Pollution, all easily the marine pollution incidents such as oil leak occurs in the exploitation of same oil, transport and storing process.The water source of these oil pollutions causes great destruction to ecological environment, how rapidly and efficiently the extensive concern that water-oil separating has caused national governments and the public is carried out to oil pollution water source.The method of carrying out water-oil separating mainly contains centrifugal process, gravitational method, absorption method, floatation, biological oxidation process and chemical method etc.Select also to need to consider during oil-water separation method the factors such as water treatment environment at that time and separated volume, using absorption method to carry out water-oil separating is one mode the most simply and easily.But the interface imbibition characteristic of traditional water-oil separating material is not obvious, and oil absorption and water-resistance are all more weak, also absorb large quantity of moisture while oil suction, and separative efficiency is lower, only have about 50%, affects the result of use of material.Need in this case to develop a kind of function admirable and the novel water-oil separating material of environmental protection.
The bionical interface water-oil separating material prepared so far is mainly divided into super-hydrophobic, super oleophylic water-oil separating material, super hydrophilic super oleophobic water-oil separating material and intelligent water-oil separating material three major types.Oil product mainly absorbs in material by super-hydrophobic super-oleophylic water-oil separating material, and water is excluded from outside material, and the bionical interface of this material is easily polluted by the oil, and the interfacial characteristics after water-oil separating also needs further research.Then develop super hydrophilic super oleophobic water-oil separating material, this material absorbs water in material, oil product is ostracised outside material, decrease the possibility that biomimetic material interface is polluted by the oil, but filter again after oil water mixture need being collected when using this material, inconvenience is caused to the oil water mixture being separated large volume.Intelligent water-oil separating material is then changed by external condition, and the special wetting property of material is changed, and can realize the material that oil absorbs or water absorbs at different conditions.In these three kinds bionical interface water-oil separating materials, owing to being more suitable for the oil water mixture of separating large, most study remain the water-oil separating material with super-hydrophobic super-oleophylic characteristic.But existing this material still shows many drawbacks in application process, as not recyclable in lower adsorption capacity, oil product or material circulation serviceability is poor, and these defects limit the practical application of super-hydrophobic water-oil separating material.
Summary of the invention
The technical problem that the present invention mainly solves: poor for bionical interface water-oil separating materials adsorption ability, large-area water-oil separating recovery cannot be realized and sorbing material cannot reusable drawback, providing a kind of is matrix by polyurethane sponge, dopamine fixes the method for ferriferrous oxide particles and lauryl mercaptan, construct micro nano structure at sponge surface and introduce low-surface energy substance, preparation has the sponge composite of super-hydrophobic and super oil-wet behavior.Make that composite has high oil absorption, Selective Separation oil water mixture, oil product fast reclaim and the performance of closed matereial cycle.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention:
(1) in mass ratio 2:1 by FeCl
3
6H
2
o and FeCl
2
4H
2
o is uniformly mixed, and be dissolved in distilled water, subsequently nitrogen is passed into distilled water, stir 10 ~ 15min at 600 ~ 800r/min lower magnetic force and be prepared into iron chloride and frerrous chloride mixed solution, subsequently mixed solution is transferred in there-necked flask, and continue to pass into nitrogen to it, after being warming up to 60 ~ 65 DEG C, under 600 ~ 800r/min magnetic agitation, dripping mass fraction with 3mL/min speed is the hydrochloric acid solution of 50%, regulate pH to be 3 ~ 4, be placed on the supersonic oscillations process 50 ~ 60min of 70 ~ 80KHz subsequently;
(2) tri-iron tetroxide predecessor is prepared into, subsequently obtained tri-iron tetroxide predecessor is proceeded in teflon-lined autoclave, 5 ~ 6h is reacted at intensification is heated to 160 ~ 170 DEG C, after question response completes, by product distilled water washing 2 ~ 3 times, and centrifugation under being placed in 1000 ~ 1200r/min, collecting lower sediment and spending deionized water to pH is 7.0 ~ 7.2, dry 6 ~ 7h at 60 ~ 65 DEG C, can be prepared into magnetic ferroferric oxide for subsequent use subsequently;
(3) take polyurethane sponge as matrix, subsequently blank sponge is placed in the CrO of 100mg/L
3
the sulfuric acid solution of solution and 100mg/L, the coarsening solution that 1:1 is mixed with by volume carries out alligatoring 10 ~ 15min, again it is placed in respectively acetone and deionized water for ultrasonic cleaning 2 ~ 3h subsequently, and dry 6 ~ 8h at being placed in 50 ~ 60 DEG C, be prepared into alligatoring polyurethane sponge for subsequent use;
(4) magnetic ferroferric oxide step (3) prepared in mass ratio 1:125 is scattered in absolute ethyl alcohol, under 600 ~ 800r/min, after mix and blend 10 ~ 15min, by the ethanol solution containing ferriferrous oxide particles and the lauryl alcohol of 2.1mmol/L and the Dopamine hydrochloride 1:2:3 by volume of 10.4mmol/L, through 200 ~ 300W ultrasonic disperse, 15 ~ 20min, be prepared into reaction dispersion liquid;
(5) alligatoring polyurethane sponge for subsequent use is placed in above-mentioned reaction dispersion liquid, mechanical agitator is used to stir 10 ~ 12h with 1200 ~ 1500r/min speed, subsequently sponge taken out and spend deionized water 2 ~ 3 times, and dry 4 ~ 5h at being placed in 80 ~ 85 DEG C, a kind of super-hydrophobic magnetic polyurethane/ferriferrous oxide composite material can be prepared into.
application of the present invention: when after generation oil spill events, super-hydrophobic magnetic polyurethane/ferriferrous oxide composite material the present invention prepared is prepared into the sponge of 1 ~ 2cm, is covered in oil spilling top layer, adsorbs it, after 5 ~ 6h upon adsorption, namely reusable after the oil pressurization after absorption is extruded.
The invention has the beneficial effects as follows:
(1) super-hydrophobic magnetic polyurethane/ferriferrous oxide composite material water-oil separating rate that the present invention obtains reaches 95 ~ 98%;
(2), after having adsorbed, pressurization is extruded namely reusable.
Detailed description of the invention
First in mass ratio 2:1 is by FeCl
36H
2o and FeCl
24H
2o is uniformly mixed, and be dissolved in distilled water, subsequently nitrogen is passed into distilled water, stir 10 ~ 15min at 600 ~ 800r/min lower magnetic force and be prepared into iron chloride and frerrous chloride mixed solution, subsequently mixed solution is transferred in there-necked flask, and continue to pass into nitrogen to it, after being warming up to 60 ~ 65 DEG C, under 600 ~ 800r/min magnetic agitation, dripping mass fraction with 3mL/min speed is the hydrochloric acid solution of 50%, regulate pH to be 3 ~ 4, be placed on the supersonic oscillations process 50 ~ 60min of 70 ~ 80KHz subsequently; Be prepared into tri-iron tetroxide predecessor, subsequently obtained tri-iron tetroxide predecessor is proceeded in teflon-lined autoclave, 5 ~ 6h is reacted at intensification is heated to 160 ~ 170 DEG C, after question response completes, by product distilled water washing 2 ~ 3 times, and centrifugation under being placed in 1000 ~ 1200r/min, collecting lower sediment and spending deionized water to pH is 7.0 ~ 7.2, dry 6 ~ 7h at 60 ~ 65 DEG C, can be prepared into magnetic ferroferric oxide for subsequent use subsequently; Take polyurethane sponge as matrix, subsequently blank sponge is placed in the CrO of 100mg/L
3the sulfuric acid solution of solution and 100mg/L, the coarsening solution that 1:1 is mixed with by volume carries out alligatoring 10 ~ 15min, again it is placed in respectively acetone and deionized water for ultrasonic cleaning 2 ~ 3h subsequently, and dry 6 ~ 8h at being placed in 50 ~ 60 DEG C, be prepared into alligatoring polyurethane sponge for subsequent use; By the magnetic ferroferric oxide of preparation in mass ratio 1:125 be scattered in absolute ethyl alcohol, under 600 ~ 800r/min, after mix and blend 10 ~ 15min, by the ethanol solution containing ferriferrous oxide particles and the lauryl alcohol of 2.1mmol/L and the Dopamine hydrochloride 1:2:3 by volume of 10.4mmol/L, through 200 ~ 300W ultrasonic disperse, 15 ~ 20min, be prepared into reaction dispersion liquid; Alligatoring polyurethane sponge for subsequent use is placed in above-mentioned reaction dispersion liquid, mechanical agitator is used to stir 10 ~ 12h with 1200 ~ 1500r/min speed, subsequently sponge taken out and spend deionized water 2 ~ 3 times, and dry 4 ~ 5h at being placed in 80 ~ 85 DEG C, a kind of super-hydrophobic magnetic polyurethane/ferriferrous oxide composite material can be prepared into.
Example 1
First in mass ratio 2:1 is by FeCl
36H
2o and FeCl
24H
2o is uniformly mixed, and be dissolved in distilled water, subsequently nitrogen is passed into distilled water, stir 10min at 600r/min lower magnetic force and be prepared into iron chloride and frerrous chloride mixed solution, subsequently mixed solution is transferred in there-necked flask, and continue to pass into nitrogen to it, after being warming up to 60 DEG C, under 600r/min magnetic agitation, dripping mass fraction with 3mL/min speed is the hydrochloric acid solution of 50%, regulate pH to be 3, be placed on the supersonic oscillations process 50min of 70KHz subsequently; Be prepared into tri-iron tetroxide predecessor, subsequently obtained tri-iron tetroxide predecessor is proceeded in teflon-lined autoclave, intensification reacts 5h at being heated to 160 DEG C, after question response completes, product distilled water is washed 2 times, and centrifugation under being placed in 1000r/min, collecting lower sediment and spending deionized water to pH is 7.0, dry 6h at 60 DEG C, can be prepared into magnetic ferroferric oxide for subsequent use subsequently; Take polyurethane sponge as matrix, subsequently blank sponge is placed in the CrO of 100mg/L
3the sulfuric acid solution of solution and 100mg/L, the coarsening solution that 1:1 is mixed with by volume carries out alligatoring 10min, it is placed in respectively acetone and deionized water for ultrasonic cleaning 2h subsequently again, and dry 6h at being placed in 50 DEG C, be prepared into alligatoring polyurethane sponge for subsequent use; By the magnetic ferroferric oxide of preparation in mass ratio 1:125 be scattered in absolute ethyl alcohol, under 600 ~ 800r/min, after mix and blend 10min, by the ethanol solution containing ferriferrous oxide particles and the lauryl alcohol of 2.1mmol/L and the Dopamine hydrochloride 1:2:3 by volume of 10.4mmol/L, through 200W ultrasonic disperse 15min, be prepared into reaction dispersion liquid; Alligatoring polyurethane sponge for subsequent use is placed in above-mentioned reaction dispersion liquid, mechanical agitator is used to stir 10h with 1200r/min speed, subsequently sponge taken out and spend deionized water 2 times, and dry 4h at being placed in 80 DEG C, a kind of super-hydrophobic magnetic polyurethane/ferriferrous oxide composite material can be prepared into.
example 2
First in mass ratio 2:1 is by FeCl
36H
2o and FeCl
24H
2o is uniformly mixed, and be dissolved in distilled water, subsequently nitrogen is passed into distilled water, stir 12min at 700r/min lower magnetic force and be prepared into iron chloride and frerrous chloride mixed solution, subsequently mixed solution is transferred in there-necked flask, and continue to pass into nitrogen to it, after being warming up to 62 DEG C, under 700r/min magnetic agitation, dripping mass fraction with 3mL/min speed is the hydrochloric acid solution of 50%, regulate pH to be 3, be placed on the supersonic oscillations process 55min of 75KHz subsequently; Be prepared into tri-iron tetroxide predecessor, subsequently obtained tri-iron tetroxide predecessor is proceeded in teflon-lined autoclave, intensification reacts 5h at being heated to 165 DEG C, after question response completes, product distilled water is washed 2 times, and centrifugation under being placed in 1100r/min, collecting lower sediment and spending deionized water to pH is 7.1, dry 6h at 62 DEG C, can be prepared into magnetic ferroferric oxide for subsequent use subsequently; Take polyurethane sponge as matrix, subsequently blank sponge is placed in the CrO of 100mg/L
3the sulfuric acid solution of solution and 100mg/L, the coarsening solution that 1:1 is mixed with by volume carries out alligatoring 12min, it is placed in respectively acetone and deionized water for ultrasonic cleaning 2h subsequently again, and dry 7h at being placed in 55 DEG C, be prepared into alligatoring polyurethane sponge for subsequent use; By the magnetic ferroferric oxide of preparation in mass ratio 1:125 be scattered in absolute ethyl alcohol, under 700r/min, after mix and blend 12min, by the ethanol solution containing ferriferrous oxide particles and the lauryl alcohol of 2.1mmol/L and the Dopamine hydrochloride 1:2:3 by volume of 10.4mmol/L, through 250W ultrasonic disperse 17min, be prepared into reaction dispersion liquid; Alligatoring polyurethane sponge for subsequent use is placed in above-mentioned reaction dispersion liquid, mechanical agitator is used to stir 11h with 1350r/min speed, subsequently sponge taken out and spend deionized water 2 times, and dry 4h at being placed in 82 DEG C, a kind of super-hydrophobic magnetic polyurethane/ferriferrous oxide composite material can be prepared into.
Example 3
First in mass ratio 2:1 is by FeCl
36H
2o and FeCl
24H
2o is uniformly mixed, and be dissolved in distilled water, subsequently nitrogen is passed into distilled water, stir 15min at 800r/min lower magnetic force and be prepared into iron chloride and frerrous chloride mixed solution, subsequently mixed solution is transferred in there-necked flask, and continue to pass into nitrogen to it, after being warming up to 65 DEG C, under 800r/min magnetic agitation, dripping mass fraction with 3mL/min speed is the hydrochloric acid solution of 50%, regulate pH to be 4, be placed on the supersonic oscillations process 60min of 80KHz subsequently; Be prepared into tri-iron tetroxide predecessor, subsequently obtained tri-iron tetroxide predecessor is proceeded in teflon-lined autoclave, intensification reacts 6h at being heated to 170 DEG C, after question response completes, product distilled water is washed 3 times, and centrifugation under being placed in 1200r/min, collecting lower sediment and spending deionized water to pH is 7.2, dry 7h at 65 DEG C, can be prepared into magnetic ferroferric oxide for subsequent use subsequently; Take polyurethane sponge as matrix, subsequently blank sponge is placed in the CrO of 100mg/L
3the sulfuric acid solution of solution and 100mg/L, the coarsening solution that 1:1 is mixed with by volume carries out alligatoring 15min, it is placed in respectively acetone and deionized water for ultrasonic cleaning 3h subsequently again, and dry 8h at being placed in 60 DEG C, be prepared into alligatoring polyurethane sponge for subsequent use; By the magnetic ferroferric oxide of preparation in mass ratio 1:125 be scattered in absolute ethyl alcohol, under 800r/min, after mix and blend 15min, by the ethanol solution containing ferriferrous oxide particles and the lauryl alcohol of 2.1mmol/L and the Dopamine hydrochloride 1:2:3 by volume of 10.4mmol/L, through 300W ultrasonic disperse 20min, be prepared into reaction dispersion liquid; Alligatoring polyurethane sponge for subsequent use is placed in above-mentioned reaction dispersion liquid, mechanical agitator is used to stir 12h with 1500r/min speed, subsequently sponge taken out and spend deionized water 3 times, and dry 5h at being placed in 85 DEG C, a kind of super-hydrophobic magnetic polyurethane/ferriferrous oxide composite material can be prepared into.
Claims (1)
1. a preparation method for super-hydrophobic magnetic polyurethane/ferriferrous oxide composite material, is characterized in that concrete preparation process is:
(1) in mass ratio 2:1 by FeCl
36H
2o and FeCl
24H
2o is uniformly mixed, and be dissolved in distilled water, subsequently nitrogen is passed into distilled water, stir 10 ~ 15min at 600 ~ 800r/min lower magnetic force and be prepared into iron chloride and frerrous chloride mixed solution, subsequently mixed solution is transferred in there-necked flask, and continue to pass into nitrogen to it, after being warming up to 60 ~ 65 DEG C, under 600 ~ 800r/min magnetic agitation, dripping mass fraction with 3mL/min speed is the hydrochloric acid solution of 50%, regulate pH to be 3 ~ 4, be placed on the supersonic oscillations process 50 ~ 60min of 70 ~ 80KHz subsequently;
(2) tri-iron tetroxide predecessor is prepared into, subsequently obtained tri-iron tetroxide predecessor is proceeded in teflon-lined autoclave, 5 ~ 6h is reacted at intensification is heated to 160 ~ 170 DEG C, after question response completes, by product distilled water washing 2 ~ 3 times, and centrifugation under being placed in 1000 ~ 1200r/min, collecting lower sediment and spending deionized water to pH is 7.0 ~ 7.2, dry 6 ~ 7h at 60 ~ 65 DEG C, can be prepared into magnetic ferroferric oxide for subsequent use subsequently;
(3) take polyurethane sponge as matrix, subsequently blank sponge is placed in the CrO of 100mg/L
3the sulfuric acid solution of solution and 100mg/L, the coarsening solution that 1:1 is mixed with by volume carries out alligatoring 10 ~ 15min, again it is placed in respectively acetone and deionized water for ultrasonic cleaning 2 ~ 3h subsequently, and dry 6 ~ 8h at being placed in 50 ~ 60 DEG C, be prepared into alligatoring polyurethane sponge for subsequent use;
(4) magnetic ferroferric oxide step (3) prepared in mass ratio 1:125 is scattered in absolute ethyl alcohol, under 600 ~ 800r/min, after mix and blend 10 ~ 15min, by the ethanol solution containing ferriferrous oxide particles and the lauryl alcohol of 2.1mmol/L and the Dopamine hydrochloride 1:2:3 by volume of 10.4mmol/L, through 200 ~ 300W ultrasonic disperse, 15 ~ 20min, be prepared into reaction dispersion liquid;
(5) alligatoring polyurethane sponge for subsequent use is placed in above-mentioned reaction dispersion liquid, mechanical agitator is used to stir 10 ~ 12h with 1200 ~ 1500r/min speed, subsequently sponge taken out and spend deionized water 2 ~ 3 times, and dry 4 ~ 5h at being placed in 80 ~ 85 DEG C, a kind of super-hydrophobic magnetic polyurethane/ferriferrous oxide composite material can be prepared into.
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