CN103276590A - Method for preparing super-hydrophobic super-oleophylic cotton - Google Patents
Method for preparing super-hydrophobic super-oleophylic cotton Download PDFInfo
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- CN103276590A CN103276590A CN2013102164143A CN201310216414A CN103276590A CN 103276590 A CN103276590 A CN 103276590A CN 2013102164143 A CN2013102164143 A CN 2013102164143A CN 201310216414 A CN201310216414 A CN 201310216414A CN 103276590 A CN103276590 A CN 103276590A
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- cotton
- hydrophobic
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- oleophylic
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- 229920000742 Cotton Polymers 0.000 title claims abstract description 66
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title abstract description 21
- PYJJCSYBSYXGQQ-UHFFFAOYSA-N trichloro(octadecyl)silane Chemical compound CCCCCCCCCCCCCCCCCC[Si](Cl)(Cl)Cl PYJJCSYBSYXGQQ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000002360 preparation method Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000011010 flushing procedure Methods 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000012986 modification Methods 0.000 claims description 15
- 230000004048 modification Effects 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 4
- 229910052681 coesite Inorganic materials 0.000 abstract 2
- 229910052906 cristobalite Inorganic materials 0.000 abstract 2
- 239000000377 silicon dioxide Substances 0.000 abstract 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 2
- 229910052682 stishovite Inorganic materials 0.000 abstract 2
- 229910052905 tridymite Inorganic materials 0.000 abstract 2
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 238000009835 boiling Methods 0.000 abstract 1
- 238000010411 cooking Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- JBJWASZNUJCEKT-UHFFFAOYSA-M sodium;hydroxide;hydrate Chemical compound O.[OH-].[Na+] JBJWASZNUJCEKT-UHFFFAOYSA-M 0.000 abstract 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 11
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 8
- 239000000126 substance Substances 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 230000002209 hydrophobic effect Effects 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 2
- 239000012675 alcoholic extract Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000012178 vegetable wax Substances 0.000 description 2
- 239000002156 adsorbate Substances 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a method for preparing super-hydrophobic super-oleophylic cotton, and belongs to the field of functional materials, in order to solve the technical problems that an existing oil-water separation absorption object is high in preparation technique requirement, is high in cost and the like. The method provided by the invention comprises the following steps of: 1, preparing a SiO2 precursor solution; 2, preparing an OTS (octadecyltrichlorosilane) modified liquid; 3, immersing cotton in a NaOH water solution, capping, boiling, cooking on low heat, and cooling; 4, then immersing into the SiO2 precursor solution, flushing with absolute ethyl alcohol clearly, and drying at room temperature, thereby obtaining the super-hydrophobic/super-oleophylic cotton. Each gram of super-hydrophobic/super-oleophylic cotton material can absorb 10-40grams of organics, and can be recycled. The method provided by the invention is simple in technology, is low in cost, is short in cycle, is low in energy consumption, and does not need a complex special device.
Description
Technical field
The invention belongs to field of functional materials; Be specifically related to the preparation method of a kind of super-hydrophobic super oleophylic cotton.
Background technology
Recent years, owing to the leakage of oil, urbanization and excessively the water contamination phenomenon that causes of industrialization become more and more serious.At present, the waters that a lot of methods such as machinery extraction, situ combustion, chemical degradation etc. all are used to clear up and clean oil pollutes.Because oil adsorbent has better economic benefit and environmental benefit, use oil adsorbent to shift and absorb oil and be considered to a very effective method.Influence the infiltrating factor of the surface of solids and mainly contain two: the one, the coarse structure of the microcosmic of the surface of solids; The 2nd, the chemical composition of the surface of solids.Recent years, people are to the continuous research on the special wettability surface in the Nature, about preparation method and the technology on special wettability surface constantly occurs.Bionical super hydrophobic surface can be realized by following two kinds of methods: a kind of is that handy hydrophobic material makes up shaggy structure; Another kind is to modify with the low-surface-energy material at the coarse surface of solids.By these two kinds of methods, may obtain bionical super hydrophobic surface.Super hydrophobic surface mainly contains following feature: low (3) automatically cleaning that adheres in (1) anti-pollution (2).The research of water-oil separating material at present more and more receives researcher's concern, but method is loaded down with trivial details mostly, and raw material is comparatively expensive.
Summary of the invention
The present invention will solve the present adsorbate technology of preparing of carrying out water-oil separating and require high, the high technical problem of cost; And provide the preparation method of a kind of super-hydrophobic super oleophylic cotton.
For solving the problems of the technologies described above, the preparation method of the super-hydrophobic super oleophylic cotton of the present invention is undertaken by following step:
Step 1
,90mL absolute ethyl alcohol, 10mL ethyl orthosilicate and 10mL deionized water are mixed, add 5 ~ 10mL ammoniacal liquor again, magnetic agitation obtains SiO to evenly at ambient temperature then
2Precursor solution;
The purpose that step 1 adds deionized water is to accelerate SiO
2Generate SiO on the cotton fiber surface in the precursor solution step 4
2Speed, improve reaction efficiency.
Step 2,100mL absolute ethyl alcohol, 1mL ~ 2mL octadecyl trichlorosilane (OTS) and 0.1mL ~ 0.25mL deionized water are mixed, stirred at ambient temperature then 2 hours, obtain OTS modification liquid;
Step 2 has been used " deionized water ", is to form silanol in order to accelerate the OTS hydrolysis, is conducive to the percent hydrolysis of OTS simultaneously, when improving reaction efficiency, has also improved the productive rate of silanol hydroxyl in the modification liquid.
Step 3, cotton is soaked in mass percent concentration is in 2% ~ 5% the NaOH aqueous solution, adds a cover then to boil the little fire in back and boiled 5 ~ 10 minutes, and cotton is taken out, and is cooled to room temperature, then the water flushing rub simultaneously to the pH value of flushing liquor be 7.0, dry naturally;
Pretreated purpose is that one deck vegetable wax shape structure on cotton fiber surface is got rid of, and exposes more hydroxyl, impels SiO in the step 4
2The hydroxyl of particle surface better is combined with cotton fiber, strengthens SiO
2Adhesion with the cotton fiber surface.
Step 4, the cotton after step 3 is handled is soaked in the SiO of step 1 preparation
2In the precursor solution, soaked under the room temperature condition then 0.5 ~ 2 hour, dry at ambient temperature after rinsing well with absolute ethyl alcohol again;
By chemical method at cotton fiber superficial growth one deck nanometer SiO
2Form the coarse structure on cotton fiber surface, SiO
2Well combine by chemical bond with cotton fiber.
Step 5, the cotton that step 4 is obtained are soaked in the OTS modification liquid of step 2 preparation, modification is 2 ~ 5 hours under 60 ℃ of conditions, rinse (to remove not reacted OTS) well with absolute ethyl alcohol then, dry at ambient temperature again, obtain super-hydrophobic super oleophylic cotton.
The super-hydrophobic super oleophylic cotton of the inventive method preparation is used for realizing water-oil separating, and this method is carried out preliminary treatment to cotton earlier, and one deck vegetable wax shape structure on cotton fiber surface is got rid of, and exposes more hydroxyl, to impel SiO in the step 4
2The hydroxyl of particle surface better is combined with cotton fiber, strengthens SiO
2Adhesion with the cotton fiber surface; Again by chemical method at cotton fiber superficial growth one deck nanometer SiO
2Form the coarse structure on cotton fiber surface, wherein SiO
2Well combine by chemical bond with cotton fiber, and then utilize the OTS modifying and decorating, form alcoholic extract hydroxyl group after the OTS hydrolysis, with SiO
2The hydroxyl of nanoparticle surface comprehensively combines securely by dewatering, and makes SiO
2The hydrophobic grouping of densification on the surface grafting can reduce its surface, reaches the function of super-hydrophobic super oleophylic, has strengthened the effect of water-oil separating; Greater than 150o, gasoline then is 0o at its surperficial contact angle to water at its surperficial contact angle.
The invention has the advantages that:
1, method is simple, and raw material is easy to get, and cost is lower, and is with short production cycle, and the consumption energy consumption is little.
2, super-hydrophobic super oleophylic cotton can be used for water-oil separating, is widely used in fields such as environmental protection.Every gram super-hydrophobic/super-oleophilic cotton material can absorb organic matter 10 ~ 40 grams.
3, has not agio.
4, can be recycled.Mode by extruding and suction filtration is discharged the oil that super-hydrophobic super oleophylic cotton inhales, and the cotton of the super-hydrophobic/super-oleophilic of the oil of draining can reused.
5, the present invention need not complicated special equipment.
Description of drawings
Fig. 1 is the high power electromicroscopic photograph (SEM) of cotton; Fig. 2 is the high power electromicroscopic photograph (SEM) that adopts the cotton of the super-hydrophobic super oleophylic that obtains after the inventive method processing; Fig. 3 does not adopt the cotton of the inventive method processing to the contact angle schematic diagram of water; Fig. 4 adopts the cotton of the inventive method processing to the contact angle schematic diagram of water; Fig. 5 adopts the cotton of the inventive method processing to the contact angle schematic diagram of oil.
The specific embodiment
The various details specific embodiment, but content of the present invention is not confined to this.
The specific embodiment one: the preparation method of super-hydrophobic super oleophylic cotton is undertaken by following step in the present embodiment:
Step 1
,90mL absolute ethyl alcohol, 10mL ethyl orthosilicate and 10mL deionized water are mixed, add 5 ~ 10mL ammoniacal liquor again, magnetic agitation obtains SiO to evenly at ambient temperature then
2Precursor solution;
Step 2,100mL absolute ethyl alcohol, 1mL ~ 2mL octadecyl trichlorosilane, (OTS) and 0.1mL ~ 0.25mL deionized water is mixed, stirred at ambient temperature then 2 hours, obtain OTS modification liquid;
Step 3, cotton is soaked in mass percent concentration is in 2% ~ 5% the NaOH aqueous solution, add a cover then boil the little fire in back and boil 5 ~ 10 minutes after, cotton is taken out, the water flushing is rubbed simultaneously then, to the pH value of flushing liquor be 7.0, dry naturally;
Step 4, the cotton after step 3 is handled is soaked in the SiO of step 1 preparation
2In the precursor solution, soaked under the room temperature condition then 0.5 ~ 2 hour, dry at ambient temperature after rinsing well with absolute ethyl alcohol again;
Step 5, the cotton that step 4 is obtained are soaked in the OTS modification liquid of step 2 preparation, modification is 2 ~ 5 hours under 60 ℃ of conditions, rinse (to remove not reacted OTS) well with absolute ethyl alcohol then, dry at ambient temperature again, obtain super-hydrophobic super oleophylic cotton.
The specific embodiment two: what present embodiment and the specific embodiment one were different is: the described NaOH aqueous solution of step 3 is prepared by following step
:Take by weighing the NaOH solid of 2 ~ 5g, be dissolved in the deionized water of 100ml, be cooled to room temperature, stand-by.Other step is identical with the specific embodiment one with parameter.
The specific embodiment three: present embodiment and the specific embodiment one or two are: the described soak time of step 4 is 1 ~ 1.5 hour.Other step is identical with the specific embodiment one or two with parameter.
The specific embodiment four: what present embodiment was different with one of specific embodiment one to three is: the step 5 modification time is 3 ~ 4 hours.Other step is identical with one of specific embodiment one to three with parameter.
The specific embodiment five: the preparation method of super-hydrophobic super oleophylic cotton is undertaken by following step in the present embodiment:
Step 1
,90mL absolute ethyl alcohol, 10mL ethyl orthosilicate and 10mL deionized water are mixed, add 8mL ammoniacal liquor again, magnetic agitation obtains SiO to evenly at ambient temperature then
2Precursor solution;
Step 2,100mL absolute ethyl alcohol, 1.5mL octadecyl trichlorosilane, (OTS) and 0.20mL deionized water are mixed, stirred at ambient temperature then 2 hours, obtain OTS modification liquid;
Step 3, cotton is soaked in mass percent concentration is in 3% the NaOH aqueous solution, adds a cover then to boil the little fire in back and boiled 10 minutes, and cotton is taken out, and the water flushing is rubbed simultaneously then, to the pH value of flushing liquor be 7.0, dry naturally;
Step 4, the cotton after step 3 is handled is soaked in the SiO of step 1 preparation
2In the precursor solution, soaked 1 hour under the room temperature condition then, dry at ambient temperature after rinsing well with absolute ethyl alcohol again;
Step 5, the cotton that step 4 is obtained are soaked in the OTS modification liquid of step 2 preparation, modification is 3 hours under 60 ℃ of conditions, rinse (to remove not reacted OTS) well with absolute ethyl alcohol then, dry at ambient temperature again, obtain super-hydrophobic super oleophylic cotton.
The high power electromicroscopic photograph (as shown in Figure 2) of the super-hydrophobic super oleophylic cotton of present embodiment compares with the high power electromicroscopic photograph of the described cotton of Fig. 1, visible cotton fiber growth one deck coating, SiO
2The nano particle glomeration is arranged in the cotton fiber surface densely, forms alcoholic extract hydroxyl group after the OTS hydrolysis, with SiO
2The hydroxyl of nanoparticle surface comprehensively combines securely by dewatering, and makes SiO
2--the hydrophobic grouping of densification in the nanoparticle surface grafting.Contrast by Fig. 4 and Fig. 2 as can be known, the super-hydrophobic super oleophylic cotton that the present embodiment method obtains has the good hydrophobic performance, as shown in Figure 5, the super-hydrophobic super oleophylic cotton that the present embodiment method obtains has good oleophylic performance.
Claims (4)
1. the preparation method of a super-hydrophobic super oleophylic cotton is characterized in that the preparation method of a kind of super-hydrophobic super oleophylic cotton is undertaken by following step:
Step 1,90mL absolute ethyl alcohol, 1OmL ethyl orthosilicate and 1OmL deionized water are mixed, add 5～1OmL ammoniacal liquor again, magnetic agitation obtains SiO to evenly at ambient temperature then
2Precursor solution;
Step 2,1OOmL absolute ethyl alcohol, 1mL～2mL octadecyl trichlorosilane and 0.1mL～0.25mL deionized water are mixed, stirred at ambient temperature then 2 hours, obtain OTS modification liquid;
Step 3, cotton is soaked in the NaOH aqueous solution that mass percent concentration is 2%-5%, adds a cover then and boil the little fire in back and boiled 5～10 minutes, cotton is taken out, the water flushing is rubbed simultaneously then, to the pH value of flushing liquor be 7.0, dry naturally;
Step 4, the cotton after step 3 is handled is soaked in the SiO of step 1 preparation
2In the precursor solution, soaked under the room temperature condition then 0.5～2 hour, dry at ambient temperature after rinsing well with absolute ethyl alcohol again;
Step 5, the cotton that step 4 is obtained are soaked in the OTS modification liquid of step 2 preparation, and modification is 2～5 hours under 60 ℃ of conditions, rinse well with absolute ethyl alcohol then, and be dry at ambient temperature again, obtains super-hydrophobic super oleophylic cotton.
2. the preparation method of a kind of super-hydrophobic super oleophylic cotton according to claim 1, it is characterized in that the described NaOH aqueous solution of step 3 prepares by following step: the NaOH solid that takes by weighing 2～5g, be dissolved in the deionized water of 1OOmL, be cooled to room temperature, stand-by.
3. the preparation method of a kind of super-hydrophobic super oleophylic cotton according to claim 1 and 2 is characterized in that the described soak time of step 4 is 1～1.5 hour.
4. the preparation method of a kind of super-hydrophobic super oleophylic cotton according to claim 3 is characterized in that the step 5 modification time is 3～4 hours.
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| CN104176944A (en) * | 2014-09-05 | 2014-12-03 | 北京航空航天大学 | Method for modifying OTS self-assembled film on glass substrate |
| CN104801281A (en) * | 2015-04-07 | 2015-07-29 | 东北林业大学 | Preparation method for oil-water separation cotton |
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