CN105413656A - Preparation method of super-hydrophobic polyurethane sponge/iron oxide composite material used for oil-water separation - Google Patents
Preparation method of super-hydrophobic polyurethane sponge/iron oxide composite material used for oil-water separation Download PDFInfo
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000004814 polyurethane Substances 0.000 title claims abstract description 56
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000000926 separation method Methods 0.000 title abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 23
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 8
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 46
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000012153 distilled water Substances 0.000 claims description 18
- 238000011010 flushing procedure Methods 0.000 claims description 18
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 14
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 7
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 6
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 6
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000001632 sodium acetate Substances 0.000 claims description 6
- 235000017281 sodium acetate Nutrition 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 abstract description 22
- 239000000463 material Substances 0.000 abstract description 17
- 235000019198 oils Nutrition 0.000 abstract description 15
- 239000000126 substance Substances 0.000 abstract description 9
- 238000010521 absorption reaction Methods 0.000 abstract description 7
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 235000019476 oil-water mixture Nutrition 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract 1
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 abstract 1
- 238000007885 magnetic separation Methods 0.000 abstract 1
- FYFFGSSZFBZTAH-UHFFFAOYSA-N methylaminomethanetriol Chemical compound CNC(O)(O)O FYFFGSSZFBZTAH-UHFFFAOYSA-N 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 1
- 241000243142 Porifera Species 0.000 description 56
- 239000003921 oil Substances 0.000 description 28
- 238000001179 sorption measurement Methods 0.000 description 8
- 238000007654 immersion Methods 0.000 description 4
- 239000010865 sewage Substances 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005213 imbibition Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920001730 Moisture cure polyurethane Polymers 0.000 description 1
- 241001346815 Spongia officinalis Species 0.000 description 1
- -1 after mixing Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention discloses a preparation method of a super-hydrophobic polyurethane sponge/iron oxide composite material used for oil-water separation and belongs to the field of composite materials. The preparation method comprises the following steps: carrying out ultrasonic washing on polyurethane sponge by dichloromethane and de-ionized water respectively to prepare a coarsening solution; coarsening the washed polyurethane sponge; preparing magnetic iron oxide particles from substances including ferric trichloride hexahydrate, glycol and the like through a magnetic separation method; adding 1-dodecanethiol into the magnetic iron oxide, adjusting the pH value and carrying out ultrasonic dispersion; adding tri-hydroxymethyl aminomethane into the dispersion solution, uniformly mixing and adding the polyurethane sponge; and stirring, washing and drying to obtain the super-hydrophobic polyurethane sponge/iron oxide composite material. According to the prepared iron oxide particles, a micro-nano structure is constructed on the surface of the sponge and low-surface-energy substances are introduced to prepare the composite material with super-hydrophobic and super-oleophylic properties, so that the composite material has the advantages of high oil absorption capability, selective separation of oil-water mixtures, rapid recycling of oil products and cyclic utilization of the material.
Description
Technical field
The invention discloses a kind of preparation method for water-oil separating super hydrophobic polyurethane sponge/ferric oxide composite material, belong to field of compound material.
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.
Polyurethane sponge, except having price with except the advantage be produced on a large scale, also has abundant macroporous structure and good elasticity.Therefore, emerging in large numbers a collection of use polyurethane sponge is matrix, and preparation has the research of the water-oil separating material of superhydrophobic characteristic.The Nguyen of Taiwan National Tsing Hua University etc. and the Gao Jianping etc. of University Of Tianjin all adopt solution dipping method to make commercial sponge surface cover upper graphene sheet layer, sponge material is had super-hydrophobic-super oil-wet behavior, composite Absorbable rod is about organic solvent or the oil product of own wt 40 ~ 165 times.Iron oxide magnetic nanoparticles mixes with PTFE powder and is wrapped in sponge surface and forms super-hydrophobic magnetic sponge material by the Calcagnile etc. of the Institute of Technology of Italy, utilizes external magnetic field driving composite to carry out water-oil separating.Also have and polyurethane sponge is placed in polyurethane prepolymer or nano-particles reinforcement solution dipping forms the sponge composite with superhydrophobic characteristic, or pass through the super-hydrophobic sponge material of chemical vapour deposition (CVD) polyaniline, and soak by chromic acid acidifying and silicon fluoride the super-hydrophobic sponge material formed.
Summary of the invention
The technical problem that the present invention mainly solves: the interface imbibition characteristic for current water-oil separating material is not obvious, oil absorption and water-resistance are all more weak, also large quantity of moisture is absorbed while oil suction, separative efficiency is lower, the problem of material circulation serviceability difference, provide a kind of preparation method for water-oil separating super hydrophobic polyurethane sponge/ferric oxide composite material, polyurethane sponge is first carried out ultrasonic cleaning by carrene and deionized water by the present invention respectively, configuration coarsening solution, polyurethane sponge after cleaning is carried out alligatoring, use the material such as ferric chloride (FeCl36H2O) and ethylene glycol again, magnetic iron oxide particle is obtained by magnetism separate method, lauryl mercaptan will be added and adjust ph and ultrasonic disperse in magnetic oxide, trishydroxymethylaminomethane is added in dispersion liquid, after mixing, polyurethane sponge is added wherein, stir, cleaning, dry, the present invention constructs micro nano structure and introducing low-surface energy substance by preparing ferric oxide particles at sponge surface, preparation has the composite of super-hydrophobic and super oil-wet behavior, composite is made to have high oil absorption, Selective Separation oil water mixture, oil product fast reclaims the advantage with closed matereial cycle.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) polyurethane sponge of one piece of 10cm × 8cm × 2cm size is got, first sponge is put into dichloromethane solution and carry out ultrasonic cleaning 1 ~ 2h, take out afterwards to put again and carry out ultrasonic cleaning 50 ~ 60min in deionized water, cleaning terminates rear taking-up, dry 40 ~ 50min in the baking oven of 60 ~ 65 DEG C;
(2) getting chromium oxide that 40 ~ 50mL mass concentration is 100g/L and 20 ~ 30mL mass concentration is that the sulfuric acid solution of 80g/L mixes, be configured to coarsening solution, above-mentioned dried polyurethane sponge is placed in coarsening solution and carries out alligatoring 2 ~ 3min, take out after alligatoring and carry out flushing 3 ~ 5 times with distilled water immediately, the coarsening solution that removing is residual, again by polyurethane sponge dry 30 ~ 40min in the baking oven of 50 ~ 55 DEG C, leave and take for subsequent use;
(3) in the there-necked flask of 250mL, 5 ~ 7g ferric chloride (FeCl36H2O) and 50 ~ 60mL ethylene glycol is added respectively, stir until solids dissolves completely, backward bottle in add 6 ~ 8g sodium acetate, continue stirring 25 ~ 35min, form uniform mixed solution, there-necked flask is put into baking oven, 10 ~ 12h is placed at 150 ~ 180 DEG C, take out afterwards and be cooled to room temperature, Magneto separate is carried out with magnet after leaving standstill 5 ~ 7min, by separator absolute ethanol washing 3 ~ 5 times, use distilled water flushing again 2 ~ 3 times, finally that the separator after cleaning is completely dry at 70 ~ 85 DEG C, obtain magnetic iron oxide particle,
(4) magnetic iron oxide particle of the above-mentioned preparation of 1 ~ 3g is got, be added to the lauryl mercaptan of 15 ~ 20mL7 ~ 8mol/L, be uniformly mixed, dropping mass fraction is the sodium hydroxide solution adjust ph of 35% is wherein 10 ~ 11, afterwards mixed liquor ultrasonic wave is carried out ultrasonic disperse 25 ~ 30min, in the solution after dispersion, adding 5 ~ 7mL concentration is again 10mmol/L trishydroxymethylaminomethane, and is uniformly mixed;
(5) dried polyurethane sponge in step (2) is put into above-mentioned mixed liquor, under the rotating speed of 400 ~ 500r/min, at the uniform velocity 2 ~ 3h is stirred with magnetic stirring apparatus, by polyurethane sponge taking-up distilled water flushing 3 ~ 5 times after stirring, put into the dry 2 ~ 3h of baking oven of 75 ~ 80 DEG C afterwards, super hydrophobic polyurethane sponge/ferric oxide composite material can be obtained.
Application process of the present invention: the present invention is prepared super hydrophobic polyurethane sponge/ferric oxide composite material and be applied in water-oil separating process, the industry water of process Organic Pollution, containing in the organically-polluted water of 6 ~ 8%, add composite, in sewage, soak 5 ~ 10min, after immersion, material is taken out, recording Organic substance in water content is 0.2 ~ 0.3%, adsorption rate is more than 96%, and after reusing 10 ~ 12 times, adsorption rate still can reach 82 ~ 85%.
The invention has the beneficial effects as follows:
(1) the present invention constructs micro nano structure and introducing low-surface energy substance by preparing ferric oxide particles at sponge surface, and preparation has the composite of super-hydrophobic and super oil-wet behavior;
(2) composite that prepared by the present invention has high oil absorption, Selective Separation oil water mixture, oil product fast reclaim and the advantage of closed matereial cycle.
Detailed description of the invention
First the polyurethane sponge of one piece of 10cm × 8cm × 2cm size is got, first sponge is put into dichloromethane solution and carry out ultrasonic cleaning 1 ~ 2h, take out afterwards to put again and carry out ultrasonic cleaning 50 ~ 60min in deionized water, cleaning terminates rear taking-up, dry 40 ~ 50min in the baking oven of 60 ~ 65 DEG C, getting chromium oxide that 40 ~ 50mL mass concentration is 100g/L and 20 ~ 30mL mass concentration is that the sulfuric acid solution of 80g/L mixes, be configured to coarsening solution, above-mentioned dried polyurethane sponge is placed in coarsening solution and carries out alligatoring 2 ~ 3min, take out after alligatoring and carry out flushing 3 ~ 5 times with distilled water immediately, the coarsening solution that removing is residual, again by polyurethane sponge dry 30 ~ 40min in the baking oven of 50 ~ 55 DEG C, leave and take for subsequent use, 5 ~ 7g ferric chloride (FeCl36H2O) and 50 ~ 60mL ethylene glycol is added respectively in the there-necked flask of 250mL, stir until solids dissolves completely, backward bottle in add 6 ~ 8g sodium acetate, continue stirring 25 ~ 35min, form uniform mixed solution, there-necked flask is put into baking oven, 10 ~ 12h is placed at 150 ~ 180 DEG C, take out afterwards and be cooled to room temperature, Magneto separate is carried out with magnet after leaving standstill 5 ~ 7min, by separator absolute ethanol washing 3 ~ 5 times, use distilled water flushing again 2 ~ 3 times, finally that the separator after cleaning is completely dry at 70 ~ 85 DEG C, obtain magnetic iron oxide particle, get magnetic iron oxide particle prepared by 1 ~ 3g, be added to the lauryl mercaptan of 15 ~ 20mL7 ~ 8mol/L, be uniformly mixed, dropping mass fraction is the sodium hydroxide solution adjust ph of 35% is wherein 10 ~ 11, afterwards mixed liquor ultrasonic wave is carried out ultrasonic disperse 25 ~ 30min, in the solution after dispersion, adding 5 ~ 7mL concentration is again 10mmol/L trishydroxymethylaminomethane, and is uniformly mixed, dried polyurethane sponge is put into mixed liquor, under the rotating speed of 400 ~ 500r/min, at the uniform velocity 2 ~ 3h is stirred with magnetic stirring apparatus, by polyurethane sponge taking-up distilled water flushing 3 ~ 5 times after stirring, put into the dry 2 ~ 3h of baking oven of 75 ~ 80 DEG C afterwards, super hydrophobic polyurethane sponge/ferric oxide composite material can be obtained.
Example 1
First the polyurethane sponge of one piece of 10cm × 8cm × 2cm size is got, first sponge is put into dichloromethane solution and carry out ultrasonic cleaning 1h, take out afterwards to put again and carry out ultrasonic cleaning 50min in deionized water, cleaning terminates rear taking-up, dry 40min in the baking oven of 60 DEG C; Getting chromium oxide that 40mL mass concentration is 100g/L and 20mL mass concentration is that the sulfuric acid solution of 80g/L mixes, be configured to coarsening solution, above-mentioned dried polyurethane sponge is placed in coarsening solution and carries out alligatoring 2min, take out after alligatoring and carry out flushing 3 times with distilled water immediately, the coarsening solution that removing is residual, again by polyurethane sponge dry 30min in the baking oven of 50 DEG C, leave and take for subsequent use; 5g ferric chloride (FeCl36H2O) and 50mL ethylene glycol is added respectively in the there-necked flask of 250mL, stir until solids dissolves completely, backward bottle in add 6g sodium acetate, continue to stir 25min, form uniform mixed solution, there-necked flask is put into baking oven, 10h is placed at 150 DEG C, take out afterwards and be cooled to room temperature, leave standstill after 5min and carry out Magneto separate with magnet, by separator absolute ethanol washing 3 times, then use distilled water flushing 2 times, finally that the separator after cleaning is completely dry at 70 DEG C, obtain magnetic iron oxide particle; Get magnetic iron oxide particle prepared by 1g, be added to the lauryl mercaptan of 15mL7mol/L, be uniformly mixed, dropping mass fraction is the sodium hydroxide solution adjust ph of 35% is wherein 10, afterwards mixed liquor ultrasonic wave is carried out ultrasonic disperse 25min, in the solution after dispersion, adding 5mL concentration is again 10mmol/L trishydroxymethylaminomethane, and is uniformly mixed; Dried polyurethane sponge is put into mixed liquor, under the rotating speed of 400r/min, at the uniform velocity 2h is stirred with magnetic stirring apparatus, by polyurethane sponge taking-up distilled water flushing 3 times after stirring, put into the dry 2h of baking oven of 75 DEG C afterwards, super hydrophobic polyurethane sponge/ferric oxide composite material can be obtained.
Application process of the present invention: the present invention is prepared super hydrophobic polyurethane sponge/ferric oxide composite material and be applied in water-oil separating process, the industry water of process Organic Pollution, containing in the organically-polluted water of 6%, add composite, in sewage, soak 5min, after immersion, material is taken out, recording Organic substance in water content is 0.2%, adsorption rate is 96.7%, and after reusing 10 times, adsorption rate still can reach 85%.
Example 2
First the polyurethane sponge of one piece of 10cm × 8cm × 2cm size is got, first sponge is put into dichloromethane solution and carry out ultrasonic cleaning 1.5h, take out afterwards to put again and carry out ultrasonic cleaning 55min in deionized water, cleaning terminates rear taking-up, dry 45min in the baking oven of 63 DEG C; Getting chromium oxide that 45mL mass concentration is 100g/L and 25mL mass concentration is that the sulfuric acid solution of 80g/L mixes, be configured to coarsening solution, above-mentioned dried polyurethane sponge is placed in coarsening solution and carries out alligatoring 2.5min, take out after alligatoring and carry out flushing 4 times with distilled water immediately, the coarsening solution that removing is residual, again by polyurethane sponge dry 35min in the baking oven of 53 DEG C, leave and take for subsequent use; 6g ferric chloride (FeCl36H2O) and 55mL ethylene glycol is added respectively in the there-necked flask of 250mL, stir until solids dissolves completely, backward bottle in add 7g sodium acetate, continue to stir 30min, form uniform mixed solution, there-necked flask is put into baking oven, 11h is placed at 170 DEG C, take out afterwards and be cooled to room temperature, leave standstill after 6min and carry out Magneto separate with magnet, by separator absolute ethanol washing 4 times, then use distilled water flushing 2 times, finally that the separator after cleaning is completely dry at 76 DEG C, obtain magnetic iron oxide particle; Get magnetic iron oxide particle prepared by 2g, be added to the lauryl mercaptan of 17mL7.5mol/L, be uniformly mixed, dropping mass fraction is the sodium hydroxide solution adjust ph of 35% is wherein 10.5, afterwards mixed liquor ultrasonic wave is carried out ultrasonic disperse 27min, in the solution after dispersion, adding 6mL concentration is again 10mmol/L trishydroxymethylaminomethane, and is uniformly mixed; Dried polyurethane sponge is put into mixed liquor, under the rotating speed of 450r/min, at the uniform velocity 2.5h is stirred with magnetic stirring apparatus, by polyurethane sponge taking-up distilled water flushing 4 times after stirring, put into the dry 2.5h of baking oven of 78 DEG C afterwards, super hydrophobic polyurethane sponge/ferric oxide composite material can be obtained.
Application process of the present invention: the present invention is prepared super hydrophobic polyurethane sponge/ferric oxide composite material and be applied in water-oil separating process, the industry water of process Organic Pollution, containing in the organically-polluted water of 7%, add composite, in sewage, soak 8min, after immersion, material is taken out, recording Organic substance in water content is 0.5%, adsorption rate is 96.4%, and after reusing 11 times, adsorption rate still can reach 83%.
Example 3
First the polyurethane sponge of one piece of 10cm × 8cm × 2cm size is got, first sponge is put into dichloromethane solution and carry out ultrasonic cleaning 2h, take out afterwards to put again and carry out ultrasonic cleaning 60min in deionized water, cleaning terminates rear taking-up, dry 50min in the baking oven of 65 DEG C; Getting chromium oxide that 50mL mass concentration is 100g/L and 30mL mass concentration is that the sulfuric acid solution of 80g/L mixes, be configured to coarsening solution, above-mentioned dried polyurethane sponge is placed in coarsening solution and carries out alligatoring 3min, take out after alligatoring and carry out flushing 5 times with distilled water immediately, the coarsening solution that removing is residual, again by polyurethane sponge dry 40min in the baking oven of 55 DEG C, leave and take for subsequent use; 7g ferric chloride (FeCl36H2O) and 60mL ethylene glycol is added respectively in the there-necked flask of 250mL, stir until solids dissolves completely, backward bottle in add 8g sodium acetate, continue to stir 35min, form uniform mixed solution, there-necked flask is put into baking oven, 12h is placed at 180 DEG C, take out afterwards and be cooled to room temperature, leave standstill after 7min and carry out Magneto separate with magnet, by separator absolute ethanol washing 5 times, then use distilled water flushing 3 times, finally that the separator after cleaning is completely dry at 85 DEG C, obtain magnetic iron oxide particle; Get magnetic iron oxide particle prepared by 3g, be added to the lauryl mercaptan of 20mL8mol/L, be uniformly mixed, dropping mass fraction is the sodium hydroxide solution adjust ph of 35% is wherein 11, afterwards mixed liquor ultrasonic wave is carried out ultrasonic disperse 30min, in the solution after dispersion, adding 7mL concentration is again 10mmol/L trishydroxymethylaminomethane, and is uniformly mixed; Dried polyurethane sponge is put into mixed liquor, under the rotating speed of 500r/min, at the uniform velocity 3h is stirred with magnetic stirring apparatus, by polyurethane sponge taking-up distilled water flushing 5 times after stirring, put into the dry 3h of baking oven of 80 DEG C afterwards, super hydrophobic polyurethane sponge/ferric oxide composite material can be obtained.
Application process of the present invention: the present invention is prepared super hydrophobic polyurethane sponge/ferric oxide composite material and be applied in water-oil separating process, the industry water of process Organic Pollution, containing in the organically-polluted water of 8%, add composite, in sewage, soak 10min, after immersion, material is taken out, recording Organic substance in water content is 0.3%, adsorption rate is 96.3%, and after reusing 12 times, adsorption rate still can reach 85%.
Claims (1)
1., for a preparation method for water-oil separating super hydrophobic polyurethane sponge/ferric oxide composite material, it is characterized in that concrete preparation process is:
(1) polyurethane sponge of one piece of 10cm × 8cm × 2cm size is got, first sponge is put into dichloromethane solution and carry out ultrasonic cleaning 1 ~ 2h, take out afterwards to put again and carry out ultrasonic cleaning 50 ~ 60min in deionized water, cleaning terminates rear taking-up, dry 40 ~ 50min in the baking oven of 60 ~ 65 DEG C;
(2) getting chromium oxide that 40 ~ 50mL mass concentration is 100g/L and 20 ~ 30mL mass concentration is that the sulfuric acid solution of 80g/L mixes, be configured to coarsening solution, above-mentioned dried polyurethane sponge is placed in coarsening solution and carries out alligatoring 2 ~ 3min, take out after alligatoring and carry out flushing 3 ~ 5 times with distilled water immediately, the coarsening solution that removing is residual, again by polyurethane sponge dry 30 ~ 40min in the baking oven of 50 ~ 55 DEG C, leave and take for subsequent use;
(3) in the there-necked flask of 250mL, 5 ~ 7g ferric chloride (FeCl36H2O) and 50 ~ 60mL ethylene glycol is added respectively, stir until solids dissolves completely, backward bottle in add 6 ~ 8g sodium acetate, continue stirring 25 ~ 35min, form uniform mixed solution, there-necked flask is put into baking oven, 10 ~ 12h is placed at 150 ~ 180 DEG C, take out afterwards and be cooled to room temperature, Magneto separate is carried out with magnet after leaving standstill 5 ~ 7min, by separator absolute ethanol washing 3 ~ 5 times, use distilled water flushing again 2 ~ 3 times, finally that the separator after cleaning is completely dry at 70 ~ 85 DEG C, obtain magnetic iron oxide particle,
(4) magnetic iron oxide particle of the above-mentioned preparation of 1 ~ 3g is got, be added to the lauryl mercaptan of 15 ~ 20mL7 ~ 8mol/L, be uniformly mixed, dropping mass fraction is the sodium hydroxide solution adjust ph of 35% is wherein 10 ~ 11, afterwards mixed liquor ultrasonic wave is carried out ultrasonic disperse 25 ~ 30min, in the solution after dispersion, adding 5 ~ 7mL concentration is again 10mmol/L trishydroxymethylaminomethane, and is uniformly mixed;
(5) dried polyurethane sponge in step (2) is put into above-mentioned mixed liquor, under the rotating speed of 400 ~ 500r/min, at the uniform velocity 2 ~ 3h is stirred with magnetic stirring apparatus, by polyurethane sponge taking-up distilled water flushing 3 ~ 5 times after stirring, put into the dry 2 ~ 3h of baking oven of 75 ~ 80 DEG C afterwards, super hydrophobic polyurethane sponge/ferric oxide composite material can be obtained.
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