CN105413656B - A kind of preparation method for water-oil separating super hydrophobic polyurethane sponge/ferric oxide composite material - Google Patents
A kind of preparation method for water-oil separating super hydrophobic polyurethane sponge/ferric oxide composite material Download PDFInfo
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- CN105413656B CN105413656B CN201510877184.4A CN201510877184A CN105413656B CN 105413656 B CN105413656 B CN 105413656B CN 201510877184 A CN201510877184 A CN 201510877184A CN 105413656 B CN105413656 B CN 105413656B
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 54
- 239000004814 polyurethane Substances 0.000 title claims abstract description 54
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 23
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 24
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 16
- 238000004140 cleaning Methods 0.000 claims abstract description 15
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 19
- 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 17
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 238000011010 flushing procedure Methods 0.000 claims description 11
- 238000007788 roughening Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical class [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
- 235000011091 sodium acetates Nutrition 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 21
- 238000000034 method Methods 0.000 abstract description 16
- 235000019198 oils Nutrition 0.000 abstract description 12
- 239000000126 substance Substances 0.000 abstract description 7
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 235000019476 oil-water mixture Nutrition 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 230000005389 magnetism Effects 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 38
- 239000003921 oil Substances 0.000 description 25
- 238000001179 sorption measurement Methods 0.000 description 8
- 239000011259 mixed solution Substances 0.000 description 5
- 238000007654 immersion Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000005213 imbibition Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000628997 Flos Species 0.000 description 1
- 229920001730 Moisture cure polyurethane Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 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
- 239000008235 industrial water Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 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
- 239000010865 sewage Substances 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- -1 trihydroxy methyl amino Chemical group 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 kind of preparation method for water-oil separating super hydrophobic polyurethane sponge/ferric oxide composite material, belong to field of compound material.Polyurethane sponge is cleaned by ultrasonic by the present invention with dichloromethane and deionized water respectively, prepare coarsening solution, polyurethane sponge after cleaning is roughened, again with materials such as ferric chloride (FeCl36H2O) and ethylene glycol, magnetic iron oxide particle is made by magnetism separate method, lauryl mercaptan will be added in magnetic iron oxide and adjust pH value and ultrasonic disperse, trishydroxymethylaminomethane is added in dispersion liquid, polyurethane sponge is added thereto after well mixed, it is stirred, cleaning, drying, the present invention constructs micro nano structure and introducing low-surface energy substance by preparing ferric oxide particles in sponge surface, prepare the composite with super-hydrophobic and super oil-wet behavior, make composite that there is high oil absorption ability, Selective Separation oil water mixture, the advantages of quick recovery of oil product and closed matereial cycle.
Description
Technical field
The invention discloses a kind of preparation side for water-oil separating super hydrophobic polyurethane sponge/ferric oxide composite material
Method, belong to field of compound material.
Background technology
In modern society, it is economical it is fast-developing produce largely by the industrial water resource of Organic Pollution, same oil
The marine pollution incidents such as oil leak easily occur in exploitation, transport and storing process.The water source of these oily pollutions is to ecology
Environment causes great destruction, how water-oil separating carried out to oily pollution water source caused national governments and public affairs rapidly and efficiently
Many extensive concerns.Carry out water-oil separating method mainly have 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 process environment and separated volume at that time, use suction
It is a kind of most simply and easily mode that attached method, which carries out water-oil separating,.But the interface imbibition characteristic of traditional water-oil separating material is failed to understand
Aobvious, oil absorption and water-resistance are weaker, and large quantity of moisture is also absorbed while oil suction, and separative efficiency is relatively low, and only 50% or so,
Influence the using effect of material.The new water-oil separating material for developing a kind of function admirable and environmental protection is needed in this case.
Polyurethane sponge also has abundant macroporous structure and good bullet in addition to price and the advantage being produced on a large scale
Property.Therefore, it is matrix to emerge in large numbers a collection of use polyurethane sponge, prepares the research of the water-oil separating material with superhydrophobic characteristic.
Nguyen of Taiwan National Tsing Hua University etc. and the Gao Jianping of University Of Tianjin etc. make the sponge table of commercialization using solution dipping method
The upper graphene sheet layer of face covering, make sponge material that there is super-hydrophobic-super oil-wet behavior, the absorbable about own wt of composite
40~165 times of organic solvent or oil product.Calcagnile of the Italian Institute of Technology etc. by Iron oxide magnetic nanoparticles with
PTFE powder mixing is wrapped in sponge surface and forms super-hydrophobic magnetic sponge material, is carried out using external magnetic field driving composite
Water-oil separating.Polyurethane sponge also is placed in into dipping in polyurethane prepolymer or nano-particles reinforcement solution to be formed with super thin
The sponge composite of water characteristic, or the super-hydrophobic sponge material by chemical vapor deposition polyaniline, and pass through chromic acid acid
Change and silicon fluoride soaks the super-hydrophobic sponge material to be formed.
The content of the invention
Present invention mainly solves technical problem：For the interface imbibition characteristic unobvious of current water-oil separating material, inhale
Oiliness and water-resistance are weaker, and large quantity of moisture is also absorbed while oil suction, and separative efficiency is relatively low, and material circulation performance is poor
The problem of, there is provided a kind of preparation method for water-oil separating super hydrophobic polyurethane sponge/ferric oxide composite material, the present invention
First polyurethane sponge is cleaned by ultrasonic with dichloromethane and deionized water respectively, coarsening solution is configured, by the poly- ammonia after cleaning
Ester sponge is roughened, then with materials such as ferric chloride (FeCl36H2O) and ethylene glycol, magnetic iron oxide is made by magnetism separate method
Grain, lauryl mercaptan will be added in magnetic iron oxide and adjust pH value and ultrasonic disperse, trihydroxy methyl amino is added in dispersion liquid
Methane, polyurethane sponge is added thereto after well mixed, is stirred, cleans, drying, the present invention is aoxidized by preparing
Iron particle constructs micro nano structure in sponge surface and introduces low-surface energy substance, prepares with super-hydrophobic and super oil-wet behavior
Composite, makes that composite has high oil absorption ability, Selective Separation oil water mixture, oil product fast reclaims and material circulation
The advantages of utilization.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
(1) polyurethane sponge of one piece of 10cm × 8cm × 2cm sizes is taken, first is put into dichloromethane solution by sponge
Row is cleaned by ultrasonic 1~2h, takes out to put again afterwards and carries out 50~60min of ultrasonic cleaning in deionized water, and cleaning is taken out after terminating,
40~50min is dried in 60~65 DEG C of baking oven, you can；
(2) chromium oxide that 40~50mL mass concentrations are 100g/L and the sulfuric acid that 20~30mL mass concentrations are 80g/L are taken
Solution is well mixed, and is configured to coarsening solution, above-mentioned dried polyurethane sponge is placed in coarsening solution carry out roughening 2~
3min, take out after roughening and be rinsed 3~5 times with distilled water immediately, remove the coarsening solution of residual, then by polyurethane sponge 50
30~40min is dried in~55 DEG C of baking oven, is left and taken standby；
(3) 5~7g ferric chloride (FeCl36H2O)s and 50~60mL ethylene glycol are separately added into 250mL three-necked flask, is stirred
Until solids is completely dissolved, backward bottle in add 6~8g sodium acetates, continue 25~35min of stirring, formed and uniformly mixed
Solution, three-necked flask is put into baking oven, 10~12h is placed at 150~180 DEG C, taken out be cooled to room temperature afterwards, stand 5
Magneto separate is carried out with magnet after~7min, isolate is washed 3~5 times with absolute ethyl alcohol, then with distilled water flushing 2~3 times, most
The isolate after cleaning is dried completely at 70~85 DEG C afterwards, obtains magnetic iron oxide particle；
(4) magnetic iron oxide particle of the above-mentioned preparations of 1~3g is taken, 15~20mL7~8mol/L lauryl mercaptan is added to, enters
Row is uniformly mixed, and it is 10~11 that the sodium hydroxide solution regulation pH value that mass fraction is 35% is added dropwise thereto, afterwards will
Mixed liquor carries out 25~30min of ultrasonic disperse with ultrasonic wave, then it is 10mmol/ to add 5~7mL concentration into the solution after disperseing
L trishydroxymethylaminomethanes, and be uniformly mixed；
(5) dried polyurethane sponge in step (2) is put into the mixed liquor obtained in step (4), stirred with magnetic force
Mix device and 2~3h is at the uniform velocity stirred under 400~500r/min rotating speed, by polyurethane sponge taking-up distilled water flushing 3 after stirring
~5 times, it is put into afterwards in 75~80 DEG C of baking oven and dries 2~3h, you can obtain super hydrophobic polyurethane sponge/iron oxide composite wood
Material.
The application process of the present invention：The present invention is prepared into super hydrophobic polyurethane sponge/ferric oxide composite material to apply
Water-oil separating is handled, and handles the industry water of Organic Pollution, in the organically-polluted water containing 6~8%, adds composite,
5~10min is soaked in sewage, takes out material after immersion, it is 0.2~0.3% to measure Organic substance in water content, and adsorption rate is
More than 96%, after reusing 10~12 times, adsorption rate still can reach 82~85%.
The beneficial effects of the invention are as follows：
(1) present invention constructs micro nano structure and introducing low-surface-energy thing by preparing ferric oxide particles in sponge surface
Matter, prepare the composite with super-hydrophobic and super oil-wet behavior；
(2) there is composite prepared by the present invention high oil absorption ability, Selective Separation oil water mixture, oil product fast to return
The advantages of receipts and closed matereial cycle.
Embodiment
The polyurethane sponge of one piece of 10cm × 8cm × 2cm sizes is taken first, first is put into dichloromethane solution by sponge
Row is cleaned by ultrasonic 1~2h, takes out to put again afterwards and carries out 50~60min of ultrasonic cleaning in deionized water, and cleaning is taken out after terminating,
40~50min is dried in 60~65 DEG C of baking oven, you can；Take 40~50mL mass concentrations be 100g/L chromium oxide and 20~
30mL mass concentrations are that 80g/L sulfuric acid solution is well mixed, and are configured to coarsening solution, by above-mentioned dried polyurethane sea
Silk floss, which is placed in coarsening solution, carries out 2~3min of roughening, takes out after roughening and is rinsed 3~5 times with distilled water immediately, removes residual
Coarsening solution, then polyurethane sponge is dried into 30~40min in 50~55 DEG C of baking oven, leave and take standby；In 250mL three mouthfuls of burnings
Be separately added into 5~7g ferric chloride (FeCl36H2O)s and 50~60mL ethylene glycol in bottle, stirring until solids is completely dissolved, backward bottle
Middle addition 6~8g sodium acetates, continue 25~35min of stirring, form uniform mixed solution, three-necked flask is put into baking oven,
10~12h is placed at 150~180 DEG C, takes out be cooled to room temperature afterwards, Magneto separate is carried out with magnet after 5~7min of standing, will
Isolate is washed 3~5 times with absolute ethyl alcohol, then with distilled water flushing 2~3 times, finally by the isolate after cleaning 70~85
Dried completely at DEG C, obtain magnetic iron oxide particle；Take 1~3g prepare magnetic iron oxide particle, be added to 15~20mL7~
8mol/L lauryl mercaptan, it is stirred the sodium hydroxide solution regulation well mixed, dropwise addition mass fraction is 35% thereto
PH value is 10~11, mixed liquor is carried out into 25~30min of ultrasonic disperse with ultrasonic wave afterwards, then add into the solution after disperseing
5~7mL concentration is 10mmol/L trishydroxymethylaminomethanes, and is uniformly mixed；Dried polyurethane sponge is put into
In mixed liquor, 2~3h is at the uniform velocity stirred under 400~500r/min rotating speed with magnetic stirring apparatus, by polyurethane sponge after stirring
Take out and use distilled water flushing 3~5 times, be put into afterwards in 75~80 DEG C of baking oven and dry 2~3h, you can obtain super hydrophobic polyurethane
Sponge/ferric oxide composite material.
Example 1
The polyurethane sponge of one piece of 10cm × 8cm × 2cm sizes is taken first, first is put into dichloromethane solution by sponge
Row is cleaned by ultrasonic 1h, takes out to put again afterwards and carries out ultrasonic cleaning 50min in deionized water, and cleaning is taken out after terminating, at 60 DEG C
Baking oven in dry 40min, you can；It is 80g/L's to take chromium oxide that 40mL mass concentrations are 100g/L and 20mL mass concentrations
Sulfuric acid solution is well mixed, and is configured to coarsening solution, and above-mentioned dried polyurethane sponge is placed in coarsening solution and carried out slightly
Change 2min, take out after roughening and be rinsed 3 times with distilled water immediately, remove the coarsening solution of residual, then by polyurethane sponge 50
DEG C baking oven in dry 30min, leave and take standby；5g ferric chloride (FeCl36H2O)s and 50mL are separately added into 250mL three-necked flask
Ethylene glycol, stirring until solids be completely dissolved, backward bottle in add 6g sodium acetates, continue stir 25min, formed uniformly
Mixed solution, three-necked flask is put into baking oven, 10h is placed at 150 DEG C, taken out be cooled to room temperature afterwards, after standing 5min
Magneto separate is carried out with magnet, isolate is washed 3 times with absolute ethyl alcohol, then with distilled water flushing 2 times, finally by point after cleaning
Dried completely at 70 DEG C from thing, obtain magnetic iron oxide particle；The magnetic iron oxide particle for taking 1g to prepare, is added to 15mL7mol/L
Lauryl mercaptan, be stirred it is well mixed, thereto be added dropwise mass fraction be 35% sodium hydroxide solution regulation pH value be
10, mixed liquor is subjected to ultrasonic disperse 25min with ultrasonic wave afterwards, then add 5mL concentration into the solution after disperseing and be
10mmol/L trishydroxymethylaminomethanes, and be uniformly mixed；Dried polyurethane sponge is put into mixed liquor, uses magnetic
Power agitator at the uniform velocity stirs 2h under 400r/min rotating speed, by polyurethane sponge taking-up distilled water flushing 3 times after stirring, it
It is put into afterwards in 75 DEG C of baking oven and dries 2h, you can obtains super hydrophobic polyurethane sponge/ferric oxide composite material.
The application process of the present invention：The present invention is prepared into super hydrophobic polyurethane sponge/ferric oxide composite material to apply
Water-oil separating is handled, and handles the industry water of Organic Pollution, in the organically-polluted water containing 6%, composite is added, in dirt
5min is soaked in water, takes out material after immersion, it is 0.2% to measure Organic substance in water content, and adsorption rate 96.7%, repetition makes
After 10 times, adsorption rate still can reach 85%.
Example 2
The polyurethane sponge of one piece of 10cm × 8cm × 2cm sizes is taken first, first is put into dichloromethane solution by sponge
Row is cleaned by ultrasonic 1.5h, takes out to put again afterwards and carries out ultrasonic cleaning 55min in deionized water, and cleaning is taken out after terminating, 63
DEG C baking oven in dry 45min, you can；It is 80g/L to take chromium oxide that 45mL mass concentrations are 100g/L and 25mL mass concentrations
Sulfuric acid solution be well mixed, be configured to coarsening solution, above-mentioned dried polyurethane sponge be placed in coarsening solution and carried out
It is roughened 2.5min, takes out after roughening and be rinsed 4 times with distilled water immediately, removes the coarsening solution of residual, then by polyurethane sponge
35min is dried in 53 DEG C of baking oven, is left and taken standby；Be separately added into 250mL three-necked flask 6g ferric chloride (FeCl36H2O)s and
55mL ethylene glycol, stirring until solids be completely dissolved, backward bottle in add 7g sodium acetates, continue stir 30min, formed
Even mixed solution, three-necked flask is put into baking oven, and 11h is placed at 170 DEG C, takes out be cooled to room temperature afterwards, stand
Magneto separate is carried out with magnet after 6min, isolate is washed 4 times with absolute ethyl alcohol, then with distilled water flushing 2 times, finally will cleaning
Isolate afterwards is dried completely at 76 DEG C, obtains magnetic iron oxide particle；The magnetic iron oxide particle for taking 2g to prepare, is added to
17mL7.5mol/L lauryl mercaptan, be stirred it is well mixed, thereto be added dropwise mass fraction be 35% sodium hydroxide it is molten
Liquid regulation pH value is 10.5, mixed liquor is carried out into ultrasonic disperse 27min with ultrasonic wave afterwards, then add into the solution after disperseing
6mL concentration is 10mmol/L trishydroxymethylaminomethanes, and is uniformly mixed；Dried polyurethane sponge is put into mixing
In liquid, 2.5h is at the uniform velocity stirred under 450r/min rotating speed with magnetic stirring apparatus, distills polyurethane sponge taking-up after stirring
Water rinses 4 times, is put into afterwards in 78 DEG C of baking oven and dries 2.5h, you can obtains super hydrophobic polyurethane sponge/iron oxide composite wood
Material.
The application process of the present invention：The present invention is prepared into super hydrophobic polyurethane sponge/ferric oxide composite material to apply
Water-oil separating is handled, and handles the industry water of Organic Pollution, in the organically-polluted water containing 7%, composite is added, in dirt
8min is soaked in water, takes out material after immersion, it is 0.5% to measure Organic substance in water content, and adsorption rate 96.4%, repetition makes
After 11 times, adsorption rate still can reach 83%.
Example 3
The polyurethane sponge of one piece of 10cm × 8cm × 2cm sizes is taken first, first is put into dichloromethane solution by sponge
Row is cleaned by ultrasonic 2h, takes out to put again afterwards and carries out ultrasonic cleaning 60min in deionized water, and cleaning is taken out after terminating, at 65 DEG C
Baking oven in dry 50min, you can；It is 80g/L's to take chromium oxide that 50mL mass concentrations are 100g/L and 30mL mass concentrations
Sulfuric acid solution is well mixed, and is configured to coarsening solution, and above-mentioned dried polyurethane sponge is placed in coarsening solution and carried out slightly
Change 3min, take out after roughening and be rinsed 5 times with distilled water immediately, remove the coarsening solution of residual, then by polyurethane sponge 55
DEG C baking oven in dry 40min, leave and take standby；7g ferric chloride (FeCl36H2O)s and 60mL are separately added into 250mL three-necked flask
Ethylene glycol, stirring until solids be completely dissolved, backward bottle in add 8g sodium acetates, continue stir 35min, formed uniformly
Mixed solution, three-necked flask is put into baking oven, 12h is placed at 180 DEG C, taken out be cooled to room temperature afterwards, after standing 7min
Magneto separate is carried out with magnet, isolate is washed 5 times with absolute ethyl alcohol, then with distilled water flushing 3 times, finally by point after cleaning
Dried completely at 85 DEG C from thing, obtain magnetic iron oxide particle；The magnetic iron oxide particle for taking 3g to prepare, is added to 20mL8mol/L
Lauryl mercaptan, be stirred it is well mixed, thereto be added dropwise mass fraction be 35% sodium hydroxide solution regulation pH value be
11, mixed liquor is subjected to ultrasonic disperse 30min with ultrasonic wave afterwards, then add 7mL concentration into the solution after disperseing and be
10mmol/L trishydroxymethylaminomethanes, and be uniformly mixed；Dried polyurethane sponge is put into mixed liquor, uses magnetic
Power agitator at the uniform velocity stirs 3h under 500r/min rotating speed, by polyurethane sponge taking-up distilled water flushing 5 times after stirring, it
It is put into afterwards in 80 DEG C of baking oven and dries 3h, you can obtains super hydrophobic polyurethane sponge/ferric oxide composite material.
The application process of the present invention：The present invention is prepared into super hydrophobic polyurethane sponge/ferric oxide composite material to apply
Water-oil separating is handled, and handles the industry water of Organic Pollution, in the organically-polluted water containing 8%, composite is added, in dirt
10min is soaked in water, takes out material after immersion, it is 0.3% to measure Organic substance in water content, adsorption rate 96.3%, is repeated
After 12 times, adsorption rate still can reach 85%.
Claims (1)
- A kind of 1. preparation method for water-oil separating super hydrophobic polyurethane sponge/ferric oxide composite material, it is characterised in that tool Preparation step is：(1) polyurethane sponge of one piece of 10cm × 8cm × 2cm sizes is taken, first sponge is put into dichloromethane solution and surpassed Sound cleans 1~2h, takes out to put again afterwards and carries out 50~60min of ultrasonic cleaning in deionized water, and cleaning is taken out after terminating, 60 40~50min is dried in~65 DEG C of baking oven, you can；(2) chromium oxide that 40~50mL mass concentrations are 100g/L and the sulfuric acid solution that 20~30mL mass concentrations are 80g/L are taken Be well mixed, be configured to coarsening solution, above-mentioned dried polyurethane sponge is placed in coarsening solution carry out roughening 2~ 3min, take out after roughening and be rinsed 3~5 times with distilled water immediately, remove the coarsening solution of residual, then by polyurethane sponge 50 30~40min is dried in~55 DEG C of baking oven, is left and taken standby；(3) be separately added into 5~7g ferric chloride (FeCl36H2O)s and 50~60mL ethylene glycol in 250mL three-necked flask, stirring until Solids is completely dissolved, backward bottle in add 6~8g sodium acetates, continue 25~35min of stirring, formation uniformly mixes molten Liquid, three-necked flask is put into baking oven, 10~12h is placed at 150~180 DEG C, taken out be cooled to room temperature afterwards, standing 5~ Magneto separate is carried out with magnet after 7min, isolate is washed 3~5 times with absolute ethyl alcohol, then with distilled water flushing 2~3 times, finally Isolate after cleaning is dried completely at 70~85 DEG C, obtains magnetic iron oxide particle；(4) magnetic iron oxide particle of the above-mentioned preparations of 1~3g is taken, 15~20mL7~8mol/L lauryl mercaptan is added to, is stirred Mix it is well mixed, thereto be added dropwise mass fraction be 35% sodium hydroxide solution regulation pH value be 10~11, afterwards will mixing Liquid carries out 25~30min of ultrasonic disperse with ultrasonic wave, then it is 10mmol/L tri- to add 5~7mL concentration into the solution after disperseing Hydroxymethyl aminomethane, and be uniformly mixed；(5) dried polyurethane sponge in step (2) is put into the mixed liquor obtained in step (4), uses magnetic stirring apparatus 2~3h is at the uniform velocity stirred under 400~500r/min rotating speed, by polyurethane sponge taking-up distilled water flushing 3~5 after stirring It is secondary, it is put into afterwards in 75~80 DEG C of baking oven and dries 2~3h, you can obtains super hydrophobic polyurethane sponge/ferric oxide composite material.
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| CN105778149B (en) * | 2016-03-30 | 2018-12-21 | 天津大学 | A kind of preparation method of super hydrophobic polyurethane sponge |
| CN106283161B (en) * | 2016-08-25 | 2018-08-03 | 山东清大银光金属海绵新材料有限责任公司 | The preparation method of sponge structure sections/SiC particulate base water-oil separating reinforcement material |
| CN106337283A (en) * | 2016-09-21 | 2017-01-18 | 江苏盖姆纳米材料科技有限公司 | Preparation method of hydrophilic mesh cloth or fabric applicable to oil-water separation |
| CN106622146B (en) * | 2016-10-17 | 2019-01-15 | 西安交通大学 | A kind of cuprous oxide/melamine sponge preparation method for oil spilling recycling |
| CN107970898B (en) * | 2017-11-24 | 2021-01-01 | 清华大学 | Method for preparing in-situ synthesis sponge iron oxide-loaded nanoparticle composite material |
| CN110339822B (en) * | 2018-04-02 | 2022-02-18 | 南京理工大学 | Preparation method of oleophylic and hydrophobic magnetic polystyrene-polyurethane composite sponge |
| CN109126743B (en) * | 2018-09-19 | 2021-12-24 | 鲁东大学 | Preparation method of polyurethane foam adsorption material |
| CN109232966B (en) * | 2018-10-11 | 2021-01-22 | 东莞市润富高分子材料有限公司 | High-elasticity melamine resin oil absorption sponge and preparation method thereof |
| CN109621923A (en) * | 2018-12-13 | 2019-04-16 | 沈阳建筑大学 | A kind of super-hydrophobic oleophylic sponge material and preparation method thereof and water-oil separating application |
| CN110628076B (en) * | 2019-10-09 | 2022-01-28 | 西南石油大学 | Simple method for modifying melamine sponge by super-hydrophobicity |
| CN111495314A (en) * | 2020-05-13 | 2020-08-07 | 兰州交通大学 | Magnetic oil-water separation material, preparation method thereof and oil-water separation sponge |
| CN111499920A (en) * | 2020-06-15 | 2020-08-07 | 中国石油大学(华东) | Super-hydrophobic oil absorption sponge with demulsification function and preparation method thereof |
| CN114732247B (en) * | 2022-04-01 | 2023-08-01 | 佛山市优迪家居制品有限公司 | High-resilience sponge cushion and preparation method thereof |
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| CN104725662B (en) * | 2013-12-18 | 2018-02-09 | 上海仪耐新材料科技有限公司 | A kind of lipophile polyurethane sponge and preparation method thereof |
| US20150197679A1 (en) * | 2014-01-10 | 2015-07-16 | Empire Technology Development Llc | Thermostatic packaging and methods for their preparation and use |
| CN104338519A (en) * | 2014-09-17 | 2015-02-11 | 上海大学 | Modified graphene-loaded polyurethane sponge and preparation method thereof |
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