CN102702563B - Oil-absorption material and preparation method thereof - Google Patents
Oil-absorption material and preparation method thereof Download PDFInfo
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- 238000010521 absorption reaction Methods 0.000 title claims abstract description 64
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- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 239000003921 oil Substances 0.000 claims description 110
- -1 poly(lactic acid) Polymers 0.000 claims description 54
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 19
- 238000000926 separation method Methods 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 5
- 235000013311 vegetables Nutrition 0.000 claims description 5
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- BQFCCCIRTOLPEF-UHFFFAOYSA-N chembl1976978 Chemical compound CC1=CC=CC=C1N=NC1=C(O)C=CC2=CC=CC=C12 BQFCCCIRTOLPEF-UHFFFAOYSA-N 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000007790 solid phase Substances 0.000 claims description 4
- 239000002283 diesel fuel Substances 0.000 claims description 3
- 239000003502 gasoline Substances 0.000 claims description 3
- 239000003350 kerosene Substances 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 2
- 239000010775 animal oil Substances 0.000 claims description 2
- 229960001701 chloroform Drugs 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 6
- 238000002474 experimental method Methods 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 4
- 239000000654 additive Substances 0.000 abstract 1
- 238000005191 phase separation Methods 0.000 abstract 1
- 239000010865 sewage Substances 0.000 abstract 1
- 229920002994 synthetic fiber Polymers 0.000 abstract 1
- 239000002250 absorbent Substances 0.000 description 13
- 230000002745 absorbent Effects 0.000 description 13
- 239000002699 waste material Substances 0.000 description 8
- 238000005259 measurement Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- 229920000520 poly(3-hydroxybutyrate-co-3-hydroxyvalerate) Polymers 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- JHUUPUMBZGWODW-UHFFFAOYSA-N 3,6-dihydro-1,2-dioxine Chemical compound C1OOCC=C1 JHUUPUMBZGWODW-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229920001432 poly(L-lactide) Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
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- 230000003075 superhydrophobic effect Effects 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
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Abstract
The invention discloses an oil-absorption material and a preparation method thereof. The preparation method of the oil-absorption material includes the following steps: 1) dissolving polyactic acid into organic solvent capable of dissolving the polyactic acid so as to obtain polyactic acid solution; and 2) performing phase separation on the polyactic acid to obtain the oil-absorption material. According to experiments, the preparation method of the oil-absorption material is easy and requires no other chemical additives, synthetic materials are wide in source, the prepared oil-absorption material has good oil-absorption effect, and the materials are biodegradable, so that the problems of secondary pollution caused by treatment of burning, burying and the like are well solved. The oil-absorption material can be used for treating sewage containing oil, cleaning floating oil on water surface, purifying water bodies and the like, and is nontoxic and harmless and strong in applicability.
Description
Technical field
The present invention relates to chemical, technical field of function materials, particularly a kind of oil absorption material and preparation method thereof.
Background technology
In recent years, the frequent generation of marine oil leakage accident and a large amount of discharges of industrial oily(waste)water, made oily water separation problem again become the focus that people pay close attention to.Oily(waste)water source is wider, industries as a lot of in Oil spills, land recover petroleum ore, food, weaving, mechanical workout etc. are all discharged a large amount of oily(waste)waters in environment, the any discharge that is industrial oily(waste)water or life oily(waste)water all causes very large pollution to productive life environment, and the environmental problem causing thus can not be ignored.The processing of oily(waste)water has many methods, and the method for conventional process oily water separation has Gravity separate, centrifugal separation, fractionation by adsorption, electricity separation etc., but these traditional methods all exist drawback, not can solve greasy dirt problem in water pollution and water.For addressing this problem, new materials and methods is is constantly researched and developed out, and nowadays, the application of oil absorption material becomes gradually cleaning oil slick, realizes the main method of oily water separation.
In recent decades, research and the application development of oil absorption material are rapid, and purposes is also very extensive.Traditional oil absorption material, as the porous masses such as sponge, clay are widely used, although these materials have good oil suction effect, but because the textural property of material itself makes traditional oil absorption material have the shortcoming that oil number is little, profit selectivity is not high, usually also absorb water when oil suction, and work-ing life is short.The high molecular polymer of synthetic of usining is just widely used as new oil absorption material, as urethane, polyethylene, polypropylene etc., it is large that this family macromolecule oil absorption material has oil number, the advantage that oil suction is effective, yet this class material is poisonous and hazardous petrochemical complex material mostly, after oil suction, be difficult for degraded, the comprehensive cost of processing waste is higher, reusability is poor, brings the problems such as secondary environmental pollution.Therefore, the R and D of environmentally friendly type oil absorption material become particularly important.
For overcoming the above problems, researched and developed the oil absorption material of reusable edible at present, as introduced respectively two kinds of oil absorption materials in CN1978511A, CN1884322A, all can repeatedly use, improved the utility value of material.Except strengthening recycling, developing biodegradable oil absorption material is also a highly effective approach.Utilize the oil suction character of Biodegradable material itself, the research that is prepared into oil absorption material has been reported, in CN1313348A, research and develop and take PHBV (PHBV) and prepare biodegradable oil absorption material as main raw material, and there is good oil suction effect.But this material has mainly utilized the lipophilic-hydrophobic property of PHBV intrinsic, do not have to improve the selectivity to profit, in the wetting property of material, do not improve.
Summary of the invention
An object of the present invention is to provide a kind of method of preparing oil absorption material.
Method provided by the invention, comprises the steps:
1) poly(lactic acid) is dissolved in the organic solvent of poly(lactic acid) described in solubilized, obtains poly(lactic acid) solution;
2) described poly(lactic acid) solution is separated, obtains oil absorption material.
In aforesaid method, in step 1), the organic solvent of poly(lactic acid) is at least one in Isosorbide-5-Nitrae-dioxane, methylene dichloride, trichloromethane, tetracol phenixin and toluene described in described solubilized;
The molecular weight of described poly(lactic acid) is 50000-100000; The molecular weight of described poly(lactic acid) is specially 69000;
Step 2) in, described in be separated as described poly(lactic acid) solution is mixed with the solvent orange 2 A that does not dissolve described poly(lactic acid), collect solid phase and be described oil absorption material, described solvent orange 2 A is specially dehydrated alcohol.
In aforesaid method, in step 1), the final concentration of described poly(lactic acid) in described poly(lactic acid) solution is 0.02-0.2g/mL;
Step 2) in, the time of described mixing is 10-60min, and the time of described mixing is specially 30min.
In aforesaid method, described oil absorption material has following 1)-4) in a kind of, two kinds, three kinds or four kinds of features:
1) described oil absorption material has micron and nano combined vesicular structure;
2) at oil absorption material described in air, the contact angle of water is greater than to 150 °;
3) at oil absorption material described in air, to oily contact angle, it is 0 °;
4) described oil absorption material is shaped as spherical, bulk or sheet.
In aforesaid method, the size in described hole is 50nm-7um;
At oil absorption material described in air, to the contact angle of water, it is 150 °-160 °.
The oil absorption material being prepared by above-mentioned method is also the scope of protection of the invention.
Above-mentioned oil absorption material has following 1)-4) in a kind of, two kinds, three kinds or four kinds of features:
1) described oil absorption material has micron and nano combined vesicular structure;
2) at oil absorption material described in air, the contact angle of water is greater than to 150 °;
3) at oil absorption material described in air, to oily contact angle, it is 0 °;
4) described oil absorption material is shaped as spherical, bulk or sheet.
In above-mentioned oil absorption material, the size in described hole is 50nm-7um;
At oil absorption material described in air, to the contact angle of water, it is 150 °-160 °.
The application in oil suction is processed of above-mentioned oil absorption material or described poly(lactic acid) is also the scope of protection of the invention; Described oil is specially normal hexane, sherwood oil, animal oil, vegetables oil, diesel oil, gasoline or kerosene.
Above-mentioned oil absorption material or described poly(lactic acid) are also the scope of protection of the invention in processing or the application in water body purification of oily water separation, oily water.
Of the present inventionly experiment showed, that oil absorption material of the present invention has that preparation method is simple, raw material is easy to get, separation efficiency advantages of higher, be applicable to the aspects such as processing, water body purification of oily(waste)water, can prepare on a large scale; Normal hexane, sherwood oil, vegetable and animals oils, diesel oil, gasoline, kerosene etc. are all had to good oil suction effect simultaneously; This oil absorption material good biocompatibility, nontoxic, and can be decomposed completely by microorganism, can not produce environmental pollution, environmental protection, can reuse good stability.
Accompanying drawing explanation
Fig. 1 is the surface topography stereoscan photograph of oil suction ball
Fig. 2 is the photo of oil suction ball to the absorption of water surface greasy dirt
Fig. 3 for measuring water droplet (2 microlitre) at the shape picture on the oil suction ball surface of preparation in air
Fig. 4 for measuring oil droplet (2 microlitre) at the shape picture on the oil suction ball surface of preparation in air
Fig. 5 is the surface topography stereoscan photograph of oil absorbent piece
Fig. 6 for measuring water droplet (2 microlitre) at the shape picture on the oil absorbent piece surface of preparation in air
Fig. 7 for measuring oil droplet (2 microlitre) at the shape picture on the oil absorbent piece surface of preparation in air
Embodiment
The experimental technique using in following embodiment if no special instructions, is ordinary method.
In following embodiment, material used, reagent etc., if no special instructions, all can obtain from commercial channels.
In following embodiment, when contact angle is greater than 65 °, just representative has hydrophobicity, when being greater than 150 °, represents to have super-hydrophobicity; Contact angle is less than 45 degree, represents wetting ability, when being less than 5 °, just represents super hydrophilic.Super-hydrophobic and super hydrophilic be all special infiltrating a kind of.
The preparation of embodiment 1, oil suction ball and Function Identification thereof
1, the preparation of oil suction ball
By PLA(poly(lactic acid), Shenzhen brilliance great achievement Industrial Co., Ltd., molecular weight=69000, Poly-L-lactic acid) be dissolved in 1, in 4-dioxane solvent, being mixed with concentration is the PLA solution of 0.1g/mL, PLA solution casting is entered in corresponding spherical mould, and immerse the 30min that is separated in dehydrated alcohol, removed 1,4-dioxane solvent and simultaneously PLA separate out into solid, collect solid phase and are oil absorption material, more simply process (being dried) and obtain oil suction ball.
2, the Function Identification of oil absorption material
By the above-mentioned 1 oil suction ball electron-microscope scanning obtaining, to amplify 410 times and observe surface topographies, result as shown in Figure 1, can find out, and this oil suction ball has micron and nanometer composite structure, and aperture is 50nm-7um; The aperture in maximum hole can reach 7um, and minimum aperture is only 50nm.
The above-mentioned 1 oil suction ball obtaining is thrown in and contained the absorption of carrying out greasy dirt on the water surface of vegetables oil (dying for redness), and result as shown in Figure 2, can see that this oil suction ball can absorb the oil slick of water surface (dying for redness) completely, has good assimilation effect.
In air, 2 microlitre water droplets are dropped in to the above-mentioned 1 oil suction ball obtaining, utilize contact angle measurement to detect, result as shown in Figure 3, can be found out, in air, to the contact angle of water, is 151.4 °.
In air, 2 microlitre normal hexanes are dropped in to the above-mentioned 1 oil suction ball obtaining, utilize contact angle measurement to detect, result as shown in Figure 4, can be found out, in air, to oily contact angle, is 0 °.
The preparation of embodiment 2, oil absorbent piece and Function Identification thereof
1, the preparation of oil absorbent piece
The PLA(poly(lactic acid) that is 69000 by molecular weight, Shenzhen brilliance great achievement Industrial Co., Ltd., Poly-L-lactic acid) be dissolved in 1, in 4-dioxane solvent, being mixed with concentration is the PLA solution of 0.1g/mL, by PLA solution uniform spreading in substrate of glass, 30min is separated in immersion dehydrated alcohol, removed Isosorbide-5-Nitrae-dioxane solvent and simultaneously PLA separate out into solid, collect solid phase and be oil absorption material, be shaped as sheet, again sheet oil absorption material is put into 40 ℃, baking oven inner drying, obtains oil absorbent piece.
2, the Function Identification of oil absorbent piece
By the above-mentioned 1 oil absorbent piece electron-microscope scanning obtaining, to be amplified 14000 times and observed surface topography, result is as shown in Figure 5, can find out to have the compound vesicular structure of micro-nano, size distribution is that aperture is 50nm-7um, the aperture in maximum hole can reach 7um, and minimum aperture is only 50nm.
In air, 2 microlitre water droplets are dropped in to above-mentioned 1 oil absorbent piece obtaining, utilize contact angle measurement to detect, result as shown in Figure 6, can be found out, in air, to the contact angle of water, is 151.6 °.
In air, 2 microlitre normal hexanes are dropped in to above-mentioned 1 oil absorbent piece obtaining, utilize contact angle measurement to detect, result as shown in Figure 7, can be found out, in air, to oily contact angle, is 0 °.
Above-mentioned 1 oil absorbent piece obtaining is placed on to the absorption of carrying out greasy dirt on the water surface that contains vegetables oil, and result can see that oil absorbent piece oil slick to water surface the same as oil suction ball has good oil suction effect.
Therefore, the oil suction ball of above-mentioned preparation and the special wetting property that oil absorbent piece has super-hydrophobic super oleophylic are described.
Claims (9)
1. a method of preparing oil absorption material, comprises the steps:
1) poly(lactic acid) is dissolved in the organic solvent of poly(lactic acid) described in solubilized, obtains poly(lactic acid) solution;
2) described poly(lactic acid) solution is separated, obtains oil absorption material;
In step 1), the molecular weight of described poly(lactic acid) is 50000-100000;
Step 2) in, described in be separated as described poly(lactic acid) solution is mixed with the solvent orange 2 A that does not dissolve described poly(lactic acid), collect solid phase and be described oil absorption material, the time of described mixing is 10-60min.
2. method according to claim 1, is characterized in that:
In step 1), the organic solvent of poly(lactic acid) is at least one in Isosorbide-5-Nitrae-dioxane, methylene dichloride, trichloromethane, tetracol phenixin and toluene described in described solubilized; The molecular weight of described poly(lactic acid) is 69000;
Described solvent orange 2 A is dehydrated alcohol.
3. method according to claim 1 and 2, is characterized in that:
In step 1), the final concentration of described poly(lactic acid) in described poly(lactic acid) solution is 0.02-0.2g/mL;
The time of described mixing is 30min.
4. the oil absorption material that arbitrary described method prepares in claim 1-3.
5. oil absorption material according to claim 4, is characterized in that:
Described oil absorption material has following 1)-4) in a kind of, two kinds, three kinds or four kinds of features:
1) described oil absorption material has micron and nano combined vesicular structure;
2) at oil absorption material described in air, the contact angle of water is greater than to 150 °;
3) at oil absorption material described in air, to oily contact angle, it is 0 °;
4) described oil absorption material is shaped as spherical, bulk or sheet.
6. oil absorption material according to claim 5, is characterized in that:
The size of described vesicular structure mesopore is 50nm-7um;
At oil absorption material described in air, to the contact angle of water, it is 150 °-160 °.
7. the application of arbitrary described oil absorption material in oil suction is processed in claim 4-6.
8. application claimed in claim 7, is characterized in that: described oil is normal hexane, sherwood oil, animal oil, vegetables oil, diesel oil, gasoline or kerosene.
In claim 4-6 arbitrary described oil absorption material in the processing of oily water separation, oily water or the application in water body purification.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103834054B (en) * | 2012-11-27 | 2018-05-11 | 东丽先端材料研究开发（中国）有限公司 | The preparation method of polylactic acid hollow microsphere |
| CN103157392B (en) * | 2013-03-22 | 2014-12-10 | 清华大学 | Biodegradable oil-water separation net film with super-hydrophobic and super-oleophylic properties and preparation method thereof. |
| CN104692482A (en) * | 2013-12-04 | 2015-06-10 | 黄然 | Water purifying matrix material prepared from polylactic acid |
| CN104846796B (en) * | 2014-12-10 | 2017-01-25 | 东华大学 | Nanofiber-foam-based continuous recovery device for floating oil on water surface and manufacturing method thereof |
| CN104987464A (en) * | 2015-07-06 | 2015-10-21 | 安徽成方新材料科技有限公司 | Macromolecule absorbent with modified high thermal stability based on nanosilicon dioxide polylactic acid and preparation method thereof |
| CN105837850B (en) * | 2016-03-11 | 2019-04-19 | 东华理工大学 | A kind of high tenacity and high transparency polylactic acid and preparation method thereof |
| CN106334543A (en) * | 2016-11-16 | 2017-01-18 | 东华大学 | Method for preparing three-dimensional porous oil absorption material |
| CN107082855A (en) * | 2017-06-01 | 2017-08-22 | 合肥创沃科技有限公司 | A kind of PLA is combined the preparation method of kapok fiber oil absorption material |
| CN110158316B (en) * | 2019-05-29 | 2021-02-26 | 南京大学 | Modified polylactic acid non-woven fabric for oil-water separation and preparation method and application thereof |
| CN112759906A (en) * | 2020-12-23 | 2021-05-07 | 青岛润兴塑料新材料有限公司 | Fully-biodegradable polylactic acid oil-absorbing foaming material for ocean |
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2012
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Non-Patent Citations (2)
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| Ch.Schugen，V.Maquent.Biodegradable and macroporous polylactide implants for cell transplantation：1 Prepartion of macroporous polylactide supports by solid-liquid phase separation.《Polymer》.1996,第37卷(第6期),第1029页，左栏第22-65行中"Foam preparation"节. |
| Ch.Schugen,V.Maquent.Biodegradable and macroporous polylactide implants for cell transplantation:1 Prepartion of macroporous polylactide supports by solid-liquid phase separation.《Polymer》.1996,第37卷(第6期),第1029页,左栏第22-65行中"Foam preparation"节. * |
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